摘要:

Journal of Analytical Atomic Spectrometry (Including Atomic Spectrometry Updates - Formerly ARAAS) JAAS Editorial Board* Chairman: L. C. Ebdon (Plymouth, UK) J. Brew (London, UK) M. S. Cresser (Aberdeen, UK) D. L. Miles (Wallingford, UK) B. L. Sharp (Aberdeen, UK) M. Thompson (London, UK) A. M. Ure (Aberdeen, UK) *The JAAS Editorial Board reports to the Analytical Editorial Board, Chairman J. D. R. Thomas (Cardiff, UK) JAAS Advisory Board F. C. Adams (Antwerp, Belgium) R. M. Barnes (Amherst, MA, USA) L. Bezur (Budapest, Hungary) R. F. Browner (Atlanta, GA, USA) S. Caroli (Rome, Italy) L. de Galan (Delft, The Netherlands) J. B. Dawson (Leeds, UK) K. Dittrich (Leipzig, GDR) W. Frech (UrneB, Sweden) K. Fuwa (Tokyo, Japan) A. L. Gray (Guildford, UK) S . Greenfield (Loughborough, UK) G.M. Hieftje (Bloomington, IN, USA) G. Horlick (Edmonton, Canada) B. V. L'vov (Leningrad, USSR) J. M. Mermet (Villeurbanne, France) Ni Zhe-ming (Beijing, China) N. Omenetto (lspra, Italy) E. PlSko (Bratislava, Czechoslovakia) R. E. Sturgeon (Ottawa, Canada) R. Van Grieken (Antwerp, Belgium) A. Walsh,.K. B. (Victoria, Australia) B. Welz (Uberlingen, FRG) T. S. West (Aberdeen, UK) Atomic Spectrometry Updates Editorial Board Chairman: "M. S. Cresser (Aberdeen, UK) R. M. Barnes (Amherst, MA, USA) N. W. Barnett (Plymouth, UK) *J. Brew (London, UK) *A. A. Brown (Cambridge, UK) J. C. Burridge (Aberdeen, UK) J. B. Dawson (Leeds, UK) J. R. Dean (Norwich, UK) *L. C. Ebdon (Plymouth, UK) H. J. Ellis (Ross-on-Wye, UK) J. Fijalkowski (Warsaw, Poland) D. J. Halls (Glasgow, UK) S.J. Haswell (London, UK) *D. A. Hickman (London, UK) G. M. Hieftje (Bloomington, IN, USA) S. J. Hill (Plymouth, UK) H. Hughes (Anglesey, UK) P. N. Keliher (Villanova, PA, USA) K. Kitagawa (Nagoya, Japan) *D. Littlejohn (Glasgow, UK) K. W. Jackson (Saskatoon, Canada) F. J. M. J. Maessen (Amsterdam, The Nether- *J. Marshall (Middlesbrough, UK) *D. L. Miles (Wallingford, UK) J. M. Mermet (Villeurbanne, France) E. Norval (Pretoria, South Africa) I. Novotny (Brno, Czechoslovakia) P. E. Paus (Oslo, Norway) P. R. Poole (Hamilton, New Zealand) T. C. Rains (Washington, DC, USA) J. M. Rooke (Leeds, UK) G. Rossi (lspra, Italy) I. RubeSka (Prague, Czechoslovakia) A. Sanz-Medel (Oviedo, Spain) *B. L. Sharp (Aberdeen, UK) W. Slavin (Norwalk, CT, USA) R. Stephens (Halifax, Canada) J.Stupar (Ljubljana, Yugoslavia) A. Taylor (Guildford, UK) M. Thompson (London, UM J. F. Tyson (Loughborough, UK) *A. M. Ure (Aberdeen, UK) B. Welz (Uberlingen, FRG) J. B. Willis (Victoria, Australia) lands) *Members of the ASU Executive Committee Editor, JAAS: Judith Brew The Royal Society of Chemistry, Burlington House, Piccadilly, London W1V OBN, UK. Telephone 01-734 9864. Telex No. 268001 US Associate Editor, JAAS: Dr. J. M. Harnly US Department of Agriculture, Beltsville Human Nutrition Research Center, BLDG 161, BARC-EAST, Beltsville, MD 20705, USA. Telephone 301 -344-2569 Advertisements: Advertisement Department, The Royal Society of Chemistry, Burlington House, Piccadilly, London WIV OBN. Telephone 01-437 8656. Telex No. 268001 Journal ofAnalytical Atomic Spectrometry fJAAS) (ISSN 0267-9477) is published eight times a year by The Royal Society of Chemistry, Burlington House, London WIVOBN, UK.All orders accompanied with payment should be sent directly t o The Royal Society of Chemistry, The Distribution Centre, Blackhorse Road, Letchworth, Herts. SG6 IHN, UK. 1987 Annual subscription rate UK f180.00, Rest of World f202.00, USA $356.00. Air freight and mailing in the USA by Publications Expediting Inc., 200 Meacham Avenue, Elmont, NY 11003. USA Postmaster: send address changes to Journal of Analytical Atomic Spectrometry (JAAS), Publications Expediting Inc., 200 Meacham Avenue, Elmont, NY 11003. Second class postage paid at Jamaica, NY 11431. All other despatches outside the UK by Bulk Airmail within Europe, Accelerated Surface Post outside Europe.PRINTED IN THE UK. 0 The Royal Society of Chemistry, 1987. All rights reserved. No part of this publication may be reproduced, stored in a retrieval system, or transmitted in any form, or by any means, electronic, mechanical, photographic, recording, or otherwise, without the prior permission of the publishers. Information for Authors Full details of how to submit material for publication in JAASare given in the Instructions to Authors in Issue 1. Separate copies are available on request. The Journal of Analytical Atomic Spectrometry (JAAS) is an international journal for the publi- cation of original research papers, short papers, communications and letters concerned with the development and analytical application of atomic spectrometric techniques. The journal is published eight times a year, includes com- prehensive reviews of specific topics of interest to practising atomic spectroscopists and incor- porates the literature reviews which were pre- viously published in Annual Reports on Analy- tical Atomic Spectroscopy (ARAAS).Manuscripts intended for publication must describe original work related to atomic spec- trometric analysis. Papers on all aspects of the subject will be accepted, including fundamental studies, novel instrument developments and practical analytical applications. As well as AAS, AES and AFS, papers will be welcomed on atomic mass spectrometry and X-ray fluoresc- ence/emission spectrometry. Papers describing the measurement of molecular species where these relate to the characterisation of sources normally used for the production of atoms, or are concerned, for example, with indirect methods of analysis, will also be acceptable for publication. Papers describing the development and applications of hybrid techniques (e.g., GC-coupled AAS and HPLC - ICP) will be parti- cularly welcome.Manuscripts on other subjects of direct interest to atomic spectroscopists, including sample preparation and dissolution and analyte preconcentration procedures, as well as the statistical interpretation and use of atomic spectrometric data will also be accept- able for publication. There is no page charge. The following types of papers will be con- sidered. Full papers, describing original work. Short papers: the criteria for originality are the same as for full papers, but short papers generally report less extensive investigations or are of limited breadth of subject matter.Communications, which must be on an urgent matter and be of obvious scientific i m porta nce. Co m m u n icat ions receive priority and are usually published within 2-3 months of receipt. They are intended for brief descriptions of work that has progressed to a stage at which it is likely to be valuable to workers faced with similar problems. Reviews, which must be a critical evaluation of the existing state of knowledge on a parti- cular facet of analytical atomic spectrometry. Every paper (except Communications) will be submitted to at least two referees, by whose advice the Editorial Board of JAAS will be guided as to its acceptance or rejection.Papers that are accepted must not be published else- where except by permission. Submission of a manuscript will be regarded as an undertaking that the same material is not being considered for publication by another journal. Manuscripts (three copies typed in double spac- ing) should be addressed to: Judith Brew, Editor, JAAS The Royal Society of Chemistry, Burlington House, Piccadilly, London WIV OBN, UK Dr. J. M. Harnly US Associate Editor, JAAS US Department of Agriculture, Beltsville Human Nutrition Research Center, BLDG 161, BARC-EAST, Beltsville, MD 20705, USA or All queries relating to the presentation and submission of papers, and any correspondence regarding accepted papers and proofs, should be directed to the Editor or US Editor (addresses as above).Members of the JAASEditorial Board (who may be contacted directly or via the Editorial Office) would welcome comments, suggestions and advice on general policy mat- ters concerning JAAS. Fifty reprints are supplied free of charge.Journal of Analytical Atomic Spectrometry (Including Atomic Spectrometry Updates - Formerly ARAAS) JAAS Editorial Board" Chairman: L. C. Ebdon (Plymouth, UK) J. Egan (London, UK) M. S. Cresser (Aberdeen, UK) D. L. Miles (Wallingford, UK) B. L. Sharp (Aberdeen, UK) M. Thompson (London, UK) A. M. Ure (Aberdeen, UK) *The JAAS Editorial Board reports to the Analytical Editorial Board, Chairman J. D. R. Thomas (Cardiff, UK) JAAS Advisory Board F. C. Adams (Antwerp, Belgium) R. M. Barnes (Amherst, MA, USA) L.Bezirr (Budapest, Hungary) R. F. Browner (Atlanta, GA, USA) S. Caroli (Rome, Italy) L. de Galan (Delft, The Netherlands) J. 6. Dawson (Leeds, UK) K. Dittrich (Leipzig, GDR) W. Frech (UmeA, Sweden) K. Fuwa ( Tokyo, Japan) A. L. Gray (Guildford, UK) S. Greenfield (Loughborough, UK) G. M. Hieftie (Bloomington, IN, USA) G. Horlick (Edmonton, Canada) 6. V. L'vov (Leningrad, USSR) J. M. Mermet (Villeurbanne, France) N i Zhe-ming (Beijing, China) N. Omenetto (lspra, Italy) E. PIGko (Bratislava, Czechoslovakia) R. E. Sturgeon (Ottawa, Canada) R. Van Grieken (Antwerp, Belgium) A. Walsh,.,K. B. (Victoria, Australia) B. Welz (Uberlingen, FRG) T. S. West (Aberdeen, UK) Atomic Spectrometry Updates Editorial Board Chairman: *M. S. Cresser (Aberdeen, UK) R. M.Barnes (Amherst, MA, USA) N. W. Barnett (Plymouth, UK) *J. Egan (London, UK) *A. A. Brown (Cambridge, UK) J. C. Burridge (Aberdeen, UK) J. B. Dawson (Leeds, UK) J. R. Dean (Norwich, UK) *L. C. Ebdon (Plymouth, UK) H. J. Ellis (Ross-on-Wye, UK) J. Fijalkowski (Warsaw, Poland) D. J . Halls (Glasgow, UK) S. J. Haswell (London, UK) *D. A. Hickman (London, UK) G. M. Hieftje (Bloomington, IN, USA) S. J. Hill (Plymouth, UK) H. Hughes (Anglesey, UK) P. N. Keliher (Villanova, PA, USA) K. Kitagawa (Nagoya, Japan) K. W. Jackson (Saskatoon, Canada) F. J. M. J. Maessen (Amsterdam, The Nether- *J. Marshall (Middlesbrough, UK) *D. L. Miles (Wallingford, UK) J. M. Mermet (Villeurbanne, France) E. Norval (Pretoria, South Africa) I . Novotny (Brno, Czechoslovakia) P. E. Paus (Oslo, Norway) P.R. Poole (Hamilton, New Zealand) T. C. Rains (Washington, DC, USA) J. M. Rooke (Leeds, UK) G. Rossi (lspra, Italy) I. RubeSka (Prague, Czechoslovakia) A. Sanz-Medel (Oviedo, Spain) *B. L. Sharp (Aberdeen, UK) W. Slavin (Norwalk, CT, USA) R. Stephens (Halifax, Canada) J. Stupar (Ljubljana, Yugoslavia) A. Taylor (Guildford, UK) M. Thompson (London, UK) J. F. Tyson (Loughborough, UK) *A. M. Ure.!Aberdeen, UK) B. Welz (Uberlingen, FRG) J. B. Willis (Victoria, Australia) *D. Littlejohn (Glasgow, UK) lands) *Members of the ASU Executive Committee Editor, JAAS: Judith Egan The Royal Society of Chemistry, Burlington House, Piccadilly, London W I V OBN, UK. Telephone 01-734 9864. Telex No. 268001 US Associate Editor, JAAS: Dr. J. M. Harnly US Department of Agriculture, Beltsville Human Nutrition Research Center, BLDG 161, BARC-EAST, Beltsville, MD 20705, USA.Telephone 301-344-2569 Advertisements: Advertisement Department, The Royal Society of Chemistry, Burlington House, Piccadilly, London W I V OBN. Telephone 01-437 8656. Telex No. 268001 Journal ofAnalytical Atomic Spectrometry (JAAS) (ISSN 0267-9477) is published eight times a year b y The Royal Society of Chemistry, Burlington House, London WIVOBN, UK. All orders accompanied with payment should be sent directly to The Royal Society of Chemistry, The Distribution Centre, Blackhorse Road, Letchworth, Herts. SG6 IHN, UK. 1987 Annual subscription rate UK f180.00, Rest of World f202.00, USA $356.00. Air freight and mailing in the USA b y Publications Expediting Inc., 200 Meacham Avenue, Elmont, NY 11003.USA Postmaster: send address changes t o Journal of Analytical Atomic Spectrometry fJAAS), Publications Expediting Inc., 200 Meacham Avenue, Elmont, NY 11003. Second class postage paid at Jamaica, NY 11431. All other despatches outside the UK by Bulk Airmail within Europe, Accelerated Surface Post outside Europe. PRINTED IN THE UK. 0 The Royal Society of Chemistry, 1987. All rights reserved. No part of this publication may be reproduced, stored in a retrieval system, or transmitted in any form, or by any means, electronic, mechanical, photographic, recording, or otherwise, without the prior permission of the publishers. Information for Authors Full details of how to submit material for publication in JAASare given in the Instructions to Authors in Issue 1.Separate copies are available on request. The Journal of Analytical Atomic Spectrometry (JAAS) is an international journal for the publi- cation of original research papers, short papers, communications and letters concerned with the development and analytical application of atomic spectrometric techniques. The journal is published eight times a year, includes com- prehensive reviews of specific topics of interest to practising atomic spectroscopists and incor- porates the literature reviews which were pre- viously published in Annual Reports on Analy- tical Atomic Spectroscopy (ARAAS). Manuscripts intended for publication must describe original work related to atomic spec- trometric analysis. Papers on all aspects of the subject will be accepted, including fundamental studies, novel instrument developments and practical analytical applications. As well as AAS, AES and AFS, papers will be welcomed on atomic mass spectrometry and X-ray fluoresc- ence/emission spectrometry.Papers describing the measurement of molecular species where these relate to the characterisation of sources normally used for the production of atoms, or are concerned, for example, with indirect methods of analysis, will also be acceptable for publication. Papers describing the development and applications of hybrid techniques (e.g., GC-coupled AAS and HPLC - ICP) will be parti- cularly welcome. Manuscripts on other subjects of direct interest to atomic spectroscopists, including sample preparation and dissolution and analyte preconcentration procedures, as well as the statistical interpretation and use of atomic spectrometric data will also be accept- able for publication.There is no page charge. The following types of papers will be con- sidered. Full papers, describing original work. Short papers: the criteria for originality are the same as for full papers, but short papers generally report less extensive investigations or are of limited breadth of subject matter. Communications, which must be on an urgent matter and be of obvious scientific importance. Communications receive priority and are usually published within 2-3 months of Veceipt. They are intended for brief descriptions of work that has progressed to a stage at which it is likely to be valuable to workers faced with similar problems. Reviews, which must be a critical evaluation of the existing state of knowledge on a parti- cular facet of analytical atomic spectrometry. Every paper (except Communications) will be submitted to at least two referees, by whose advice the Editorial Board of JAAS will be guided as to its acceptance or rejection. Papers that are accepted must not be published else- where except by permission. Submission of a manuscript will be regarded as an undertaking that the same material is not being considered for publication by another journal. Manuscripts (three copies typed in double spac- ing) should be addressed to: Judith Egan, Editor, JAAS The Royal Society of Chemistry, Burlington House, Piccadilly, London WIV OBN, UK Dr. J. M. Harnly US Associate Editor, JAAS US Department of Agriculture, Beltsville Human Nutrition Research Center, BLDG 161, BARC-EAST, Beltsville, MD 20705, USA or All queries relating to the presentation and submission of papers, and any correspondence regarding accepted papers and proofs, should be directed to the Editor or US Editor (addresses as above). Members of the JAASEditorial Board (who may be contacted directly or via the Editorial Office) would welcome comments, suggestions and advice on general policy mat- ters concerning JAAS. Fifty reprints are supplied free of charge.

ISSN:0267-9477    

DOI:10.1039/JA98702FX013

出版商:RSC    

年代:1987

数据来源: RSC

摘要:

JASPE2 2(4) 343-416,79R-l32R (1987) June 1987 Journal of Analytical Atomic Spectrometry Including Atomic Spectrometry Updates CONTENTS NEWS AND VIEWS 343 347 348 352 352 353 355 356 356 Historical Perspectives-D. Thorburn Burns Atomic Spectrometry Viewpoint-A. Grillo and P. Stockwell Conference Reports ASU Highlights-J. Marshall Book Reviews Conferences and Meetings Courses SAC Gold Medal Presentation Papers in Future Issues PAPERS 357 365 369 375 379 383 389 397 401 405 407 41 1 41 3 41 5 Peak-area Measurements in Electrothermal Atomisation Inductively Coupled Plasma Atomic Emission Spectrometry-Jose Alvarado, Paolo Cavalli, Nicolo Omenetto, Guglielmo Rossi, (the late) John M. Ottaway Spectral and Physical Interferences in a New, Flexible Inductively Coupled Plasma Mass Spectrometry Instrument-Daniel A.Wilson, George H. Vickers, Gary M. Hieftje Selection of Mode for the Measurement of Lead Isotope Ratios by Inductively Coupled Plasma Mass Spectrometry and its Application t o Milk Powder Analysis-John R. Dean, Les Ebdon, Robert Massey On-line Sequential Detection by Inductively Coupled Plasma Atomic Emission Spec- trometry of Trace Elements after Liquid Chromatography of Biological Fluids-Philip E. Gardiner, Peter Braetter, Bertold Gercken, Andreas Tomiak Fluoride Interference on the Boron Inductively Coupled Plasma Atomic Emission in Methanolic Solutions-Antonio Canals, Vicente Hernandis Use of a Thermospray Nebuliser as a Sample Introduction System for Inductively Coupled Plasma Atomic Emission Spectrometry-Koen A. Vermeiren, Philip D.P. Taylor, Richard Dams Evaluation of the Grid-type Nebuliser for Organic Solvent Introduction into the Inductively Coupled Plasma-Timothy Brotherton, Barbara Barnes, Nohora Vela, Joseph Caruso Direct Determination of Cadmium in Soil Slurries by Micro-sampling Cup Atomic Absorption Spectrometry-Garth Ryg h, Kenneth W. Jackson Optimisation of the Analytical Conditions for the Determination of Aluminium in Human Blood Plasma and Serum by Graphite Furnace Atomic Absorption Spec- trometry. Part 2. Assessment of the Analytical Method-Philip E. Gardiner, Markus Stoeppler SHORT PAPERS Development of Hollow-cathode Radiation Sources. Part 1. Study of the Effects of Cones Placed in the Cavity on the Emitted Light Intensity-Lajos Papp, Laszlo Racz Development of Hollow-cathode Radiation Sources.Part 2. Study of the Effect of a Cylinder Placed in the Cathode Cavity on the Emitted Light Intensity-Lajos Papp K and L Shell X-ray Relative Intensity Measurements-Chander Bhan, Anita Rani, S. N. Chaturvedi, N. Nath Atomic Absorption Spectrometric Method for the Determination of Phosphorus using the Bismuth - Phosphomolybdate Complex-Pramod K. Gupta, Ramadevi Ramchan- dran Indirect Determination of Adrenaline by Inductively Coupled Plasma Atomic Emission Spectrometry-Wuming Zhang, Zhengyin Yan, Yaping Liu ATOMIC SPECTROMETRY UPDATE 79R Instrumentation-John Marshall, Stephen J. Haswell, Stephen J. Hill 115R ReferencesJASPE2 2(4) 343-416,79R-l32R (1987) June 1987 Journal of Analytical Atomic Spectrometry Including Atomic Spectrometry Updates CONTENTS NEWS AND VIEWS 343 347 348 352 352 353 355 356 356 Historical Perspectives-D. Thorburn Burns Atomic Spectrometry Viewpoint-A.Grillo and P. Stockwell Conference Reports ASU Highlights-J. Marshall Book Reviews Conferences and Meetings Courses SAC Gold Medal Presentation Papers in Future Issues PAPERS 357 365 369 375 379 383 389 397 401 405 407 41 1 41 3 41 5 Peak-area Measurements in Electrothermal Atomisation Inductively Coupled Plasma Atomic Emission Spectrometry-Jose Alvarado, Paolo Cavalli, Nicolo Omenetto, Guglielmo Rossi, (the late) John M. Ottaway Spectral and Physical Interferences in a New, Flexible Inductively Coupled Plasma Mass Spectrometry Instrument-Daniel A. Wilson, George H. Vickers, Gary M. Hieftje Selection of Mode for the Measurement of Lead Isotope Ratios by Inductively Coupled Plasma Mass Spectrometry and its Application t o Milk Powder Analysis-John R.Dean, Les Ebdon, Robert Massey On-line Sequential Detection by Inductively Coupled Plasma Atomic Emission Spec- trometry of Trace Elements after Liquid Chromatography of Biological Fluids-Philip E. Gardiner, Peter Braetter, Bertold Gercken, Andreas Tomiak Fluoride Interference on the Boron Inductively Coupled Plasma Atomic Emission in Methanolic Solutions-Antonio Canals, Vicente Hernandis Use of a Thermospray Nebuliser as a Sample Introduction System for Inductively Coupled Plasma Atomic Emission Spectrometry-Koen A. Vermeiren, Philip D. P. Taylor, Richard Dams Evaluation of the Grid-type Nebuliser for Organic Solvent Introduction into the Inductively Coupled Plasma-Timothy Brotherton, Barbara Barnes, Nohora Vela, Joseph Caruso Direct Determination of Cadmium in Soil Slurries by Micro-sampling Cup Atomic Absorption Spectrometry-Garth Ryg h, Kenneth W.Jackson Optimisation of the Analytical Conditions for the Determination of Aluminium in Human Blood Plasma and Serum by Graphite Furnace Atomic Absorption Spec- trometry. Part 2. Assessment of the Analytical Method-Philip E. Gardiner, Markus Stoeppler SHORT PAPERS Development of Hollow-cathode Radiation Sources. Part 1. Study of the Effects of Cones Placed in the Cavity on the Emitted Light Intensity-Lajos Papp, Laszlo Racz Development of Hollow-cathode Radiation Sources. Part 2. Study of the Effect of a Cylinder Placed in the Cathode Cavity on the Emitted Light Intensity-Lajos Papp K and L Shell X-ray Relative Intensity Measurements-Chander Bhan, Anita Rani, S. N. Chaturvedi, N. Nath Atomic Absorption Spectrometric Method for the Determination of Phosphorus using the Bismuth - Phosphomolybdate Complex-Pramod K. Gupta, Ramadevi Ramchan- dran Indirect Determination of Adrenaline by Inductively Coupled Plasma Atomic Emission Spectrometry-Wuming Zhang, Zhengyin Yan, Yaping Liu ATOMIC SPECTROMETRY UPDATE 79R Instrumentation-John Marshall, Stephen J. Haswell, Stephen J. Hill 115R References

ISSN:0267-9477    

DOI:10.1039/JA98702BX015

出版商:RSC    

年代:1987

数据来源: RSC

摘要:

I andysed my c I I I ARL’s new 3410 ICP spectrometer brings ICP within your reach Now every laboratory involved in solutions elemental analysis can afford to employ the fast, sensitive ICP technique. The new affordable ARL 3410 ICP with MinitorchTM and IBM-PC-XT makes it all possible, and offer these advantages over other systems: lower instrument cost, with ARL’s MinitorchTM; ARL Applied Research Laboratories SA En Vallaire C~-1204 ECUBLENS / Switzerland Tel. (021) 34 97 Austria: (0222) 36 41 52 France: (1) 34 61 94 00 Germany: (021 1) 71 30 06 Spain: (1) 457 50 08 Sweden: (08) 730 o2 95 United Kingdom: (0582) 573 474/9 lower operating costs - lower power usage, lower argon flow give savings of up to 40% over conventional instruments; easier to operate - ARL’s ICP software is spe- cially written for the powerful IBM-PC-XT.The ARL 3410 offers the high performance and flex- ibility of ICP in the most cost-effective package. Can you afford to be without it? ARl APPLIED RESEARCH LABORATORIES Circle 001 for further informationI andysed my c I I I ARL’s new 3410 ICP spectrometer brings ICP within your reach Now every laboratory involved in solutions elemental analysis can afford to employ the fast, sensitive ICP technique. The new affordable ARL 3410 ICP with MinitorchTM and IBM-PC-XT makes it all possible, and offer these advantages over other systems: lower instrument cost, with ARL’s MinitorchTM; ARL Applied Research Laboratories SA En Vallaire C~-1204 ECUBLENS / Switzerland Tel. (021) 34 97 Austria: (0222) 36 41 52 France: (1) 34 61 94 00 Germany: (021 1) 71 30 06 Spain: (1) 457 50 08 Sweden: (08) 730 o2 95 United Kingdom: (0582) 573 474/9 lower operating costs - lower power usage, lower argon flow give savings of up to 40% over conventional instruments; easier to operate - ARL’s ICP software is spe- cially written for the powerful IBM-PC-XT. The ARL 3410 offers the high performance and flex- ibility of ICP in the most cost-effective package.Can you afford to be without it? ARl APPLIED RESEARCH LABORATORIES Circle 001 for further informationI andysed my c I I I ARL’s new 3410 ICP spectrometer brings ICP within your reach Now every laboratory involved in solutions elemental analysis can afford to employ the fast, sensitive ICP technique. The new affordable ARL 3410 ICP with MinitorchTM and IBM-PC-XT makes it all possible, and offer these advantages over other systems: lower instrument cost, with ARL’s MinitorchTM; ARL Applied Research Laboratories SA En Vallaire C~-1204 ECUBLENS / Switzerland Tel.(021) 34 97 Austria: (0222) 36 41 52 France: (1) 34 61 94 00 Germany: (021 1) 71 30 06 Spain: (1) 457 50 08 Sweden: (08) 730 o2 95 United Kingdom: (0582) 573 474/9 lower operating costs - lower power usage, lower argon flow give savings of up to 40% over conventional instruments; easier to operate - ARL’s ICP software is spe- cially written for the powerful IBM-PC-XT. The ARL 3410 offers the high performance and flex- ibility of ICP in the most cost-effective package. Can you afford to be without it? ARl APPLIED RESEARCH LABORATORIES Circle 001 for further informationI andysed my c I I I ARL’s new 3410 ICP spectrometer brings ICP within your reach Now every laboratory involved in solutions elemental analysis can afford to employ the fast, sensitive ICP technique.The new affordable ARL 3410 ICP with MinitorchTM and IBM-PC-XT makes it all possible, and offer these advantages over other systems: lower instrument cost, with ARL’s MinitorchTM; ARL Applied Research Laboratories SA En Vallaire C~-1204 ECUBLENS / Switzerland Tel. (021) 34 97 Austria: (0222) 36 41 52 France: (1) 34 61 94 00 Germany: (021 1) 71 30 06 Spain: (1) 457 50 08 Sweden: (08) 730 o2 95 United Kingdom: (0582) 573 474/9 lower operating costs - lower power usage, lower argon flow give savings of up to 40% over conventional instruments; easier to operate - ARL’s ICP software is spe- cially written for the powerful IBM-PC-XT. The ARL 3410 offers the high performance and flex- ibility of ICP in the most cost-effective package. Can you afford to be without it? ARl APPLIED RESEARCH LABORATORIES Circle 001 for further information

ISSN:0267-9477    

DOI:10.1039/JA98702FP021

出版商:RSC    

年代:1987

数据来源: RSC

摘要:

JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY APR'87 READER ENQUIRY SERVICE For further information about any of the productsfeatured in the advertisements in this issue, please write the appropriate number in one of the boxes below. Postage paid if posted in the British Isles but overseas readers must affix a stamD. r PLEASE USE BLOCK CAPITALS LEAVING A SPACE BETWEEN WORDS Valid 12 mon fhs _ _ -_ -1-1 I I T 1 i 1 1 1 I I I I 1 I 1 I I I I I I I I I 1 I I I T I 1 I I I I I i I 1 m--n11-m l l I l l l l 1 1 1 l l I 1 1 1 1 1 1 I l l i l i l l t l HI mm-TLLml I I 1 I I I 1 1 1 1 1 1 I I I 1 1 1 POSTCODE 1 I 1 1 I I I I I 1 I I I I I I I I I - I I I I J I 1 I 1 - i I I 1 I In 1 Ti I I ! 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Ireland or the Isle of Man BUSINESS REPLY SERVICE Licence No. WD 106 Reader Enquiry Service Journal of Analytical Atomic Spectrometry The Royal Society of Chemistry Burlington House, Piccadilly LONDON WIE 6WF England 2 I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I - I I I I I I I I I I 1 I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I 1 I I I I I I I I I I I I I I i I I I I I I I I I I ! 1I I I I I I I I I I I I I I I I I JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY JUNE'87 For further information about any of the products featured in the advertisements in this issue, please write the appropriate number in one of the boxes below.Postage paid if posted in the British isles but overseas readers must affix a stamD. 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Ireland or the isle of Man BUSINESS REPLY SERVICE Reader Enquiry Service Journal of Analytical Atomic Spectrometry The Royal Society of Chemistry Burlington House, Piccadilly LONDON WIE 6WF England I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I ! I I I I I I 1 I I I I I I I I I I I I I I I I I I I I I 1 I I I I I I Ivii PHOTOMULTIPLIERS, ACCESSORIES and SYSTEMS -the key to successful photodetection PHOTOM ULTl PLIERS 0 State of the art technology. 0 Diameters from 19 to 190 mm, including side window, hemispherical, UV and metal ceramic types.0 Gain up to I@ high sensitivity and low dark current. 0 Wide choice of spectral response. 0 Rugged tubes for hostile environments, such as space research and oil well logging. 0 Custom design and spectral calibration service. ACCESSORIES 0 HV power supplies, cooled and ambient housings, voltage dividers, amplifier discriminators, magnetic focusing assemblies, filter holders and shutters. SYSTEMS 0 Low cost photon counting units,withTTLand analogue outputs and microcomputer interface capability. 0 Complete, computerised photon detection systems for users of any level of experience. Sophisticated results quickly and accurately. THE MOST COMPREHENSIVE CAPABILITY IN PHOTODETECTION SERVING SCIENCE, INDUSTRY AND MEDICINE THORN EM1 Electron Tubes Limited Bury Street, Ruislip, Middlesex HA4 7TA, England.Tel: (08956) 30771. Circle 008 for further information Reprint of a review published in Chemical Society Reviews JOHN JEYES LECTURE The Environmental Chemistry of Radioactive Waste Disposal by John R. Duffield and David R. Williams Dept. of Applied Chemistry, UWIST Over the past forty years there has been a revolution in the way in which man fulfils his energy requirements. In this period we have moved from a predominantly fossil-fuel based power economy to one in which nuclear fission plays an increasingly significant role. This transition has placed new and potentially very serious stresses on the environment and associated ecosystems. This review considers the environmental chemistry problems that the disposal of radioactive waste has generated and how they might be tackled.Brief Contents: Introduction; The Threat to Man; Contamination Pathways; The Chemistry of Waste Containment; Groundwater; Aqueous Speciation of Radionuclides; Sorption; Risk 17pp f2.00 ($4.00) PAYMENT MUST ACCOMPANY ORDER (Cheques made pay- able to “The Royal Society of Chemistry”) Assessment; Models and Simulation Techniques; Calculation Procedures; Databases; Verification and Validation; Conclusions and a Strategy for the Future Orders should be sent to: K. J. Wilkinson, Books Department, The Royal Society of Chemistry, Burlington House, Piccadilly, London W1V OBN, UK. IN SPECTURAL SOURCES I- @ High quality High intensity High spectural purity High stability& long life Hollow cathode lamps at the lowest available prices! k Although a relatively new name in H.C.lamps, SIP Analytical Limited combines personnel each with over 25 year‘s manufacturing experience with purpose built, high capacity manufacturing plant, to produce a high quality, reliable product at significantly lower prices A comprehensive range of tubes t o fit all makes of instrument available ex-stock For further details contact:- S. 1. P. ANALYTICAL LTD Unit 1, All Saints Industrial Estate, All Saints Avenue, Margate, Kent CT9 50W Tel: (0843) 22 1295. Telex: 826932 Circle 010 for further information Circle 006 for further informationvii PHOTOMULTIPLIERS, ACCESSORIES and SYSTEMS -the key to successful photodetection PHOTOM ULTl PLIERS 0 State of the art technology.0 Diameters from 19 to 190 mm, including side window, hemispherical, UV and metal ceramic types. 0 Gain up to I@ high sensitivity and low dark current. 0 Wide choice of spectral response. 0 Rugged tubes for hostile environments, such as space research and oil well logging. 0 Custom design and spectral calibration service. ACCESSORIES 0 HV power supplies, cooled and ambient housings, voltage dividers, amplifier discriminators, magnetic focusing assemblies, filter holders and shutters. SYSTEMS 0 Low cost photon counting units,withTTLand analogue outputs and microcomputer interface capability. 0 Complete, computerised photon detection systems for users of any level of experience. Sophisticated results quickly and accurately. THE MOST COMPREHENSIVE CAPABILITY IN PHOTODETECTION SERVING SCIENCE, INDUSTRY AND MEDICINE THORN EM1 Electron Tubes Limited Bury Street, Ruislip, Middlesex HA4 7TA, England.Tel: (08956) 30771. Circle 008 for further information Reprint of a review published in Chemical Society Reviews JOHN JEYES LECTURE The Environmental Chemistry of Radioactive Waste Disposal by John R. Duffield and David R. Williams Dept. of Applied Chemistry, UWIST Over the past forty years there has been a revolution in the way in which man fulfils his energy requirements. In this period we have moved from a predominantly fossil-fuel based power economy to one in which nuclear fission plays an increasingly significant role. This transition has placed new and potentially very serious stresses on the environment and associated ecosystems.This review considers the environmental chemistry problems that the disposal of radioactive waste has generated and how they might be tackled. Brief Contents: Introduction; The Threat to Man; Contamination Pathways; The Chemistry of Waste Containment; Groundwater; Aqueous Speciation of Radionuclides; Sorption; Risk 17pp f2.00 ($4.00) PAYMENT MUST ACCOMPANY ORDER (Cheques made pay- able to “The Royal Society of Chemistry”) Assessment; Models and Simulation Techniques; Calculation Procedures; Databases; Verification and Validation; Conclusions and a Strategy for the Future Orders should be sent to: K. J. Wilkinson, Books Department, The Royal Society of Chemistry, Burlington House, Piccadilly, London W1V OBN, UK. IN SPECTURAL SOURCES I- @ High quality High intensity High spectural purity High stability& long life Hollow cathode lamps at the lowest available prices! k Although a relatively new name in H.C. lamps, SIP Analytical Limited combines personnel each with over 25 year‘s manufacturing experience with purpose built, high capacity manufacturing plant, to produce a high quality, reliable product at significantly lower prices A comprehensive range of tubes t o fit all makes of instrument available ex-stock For further details contact:- S. 1. P. ANALYTICAL LTD Unit 1, All Saints Industrial Estate, All Saints Avenue, Margate, Kent CT9 50W Tel: (0843) 22 1295. Telex: 826932 Circle 010 for further information Circle 006 for further information

ISSN:0267-9477    

DOI:10.1039/JA98702BP025

出版商:RSC    

年代:1987

数据来源: RSC

摘要:

JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, JUNE 1987, VOL. 2 79R ATOMIC SPECTROMETRY UPDATE-INSTRUMENTATION John Marshall* ICl Chemicals and Polymers Group, PO Box No. 90, Wilton, Middlesbrough, Cleveland TS6 8JE, UK Stephen J. Haswell Thames Polytechnic, Wellington Street, Woolwich, London SE 18 6PF, UK Stephen J. Hill Department of Environmental Sciences, Plymouth Polytechnic, Drake Circus, Plymouth PL4 8AA, UK Summary of Contents Light Sources 1.1. Lasers 1.2. Hollow Cathodes 1.3. Glow Discharges 1.4. Other Sources Optical Systems and Detectors 2.1. Optical Systems 2.2. Detectors Background Correction 3.1. Optical Systems 3.2. Computer Aided Systems Automatic Sample Introduction 4.1. Flow Injection 4.2. Chromatographic Sample Introduction 4.3. Other Techniques for Sample Introduction Instrumental Control and Data Processing 5.1.Instrumental Control 5.2. Data Processing 5.3. Calibration 5.4. Data Acquisition and Manipulation Complete Instruments 6.1. Emission 6.2. Absorption 6.3. Fluorescence 6.4. Mass Spectrometry Table 1. Evaluation of Analytical Instrumentation. Part Ill. Polychromators for Use in Emission Spectrometry with ICP Sources Commercial Instruments 7.1. Emission 7.2. Absorption 7.3. FI u o rescence 7.4. Mass Spectrometry Table 2. Commercially Available Instruments Table 3. Instrument Company Addresses This review describes developments in all aspects of atomic spectroscopic instrumentation reported in the Atomic Spectrometry Update References in JAAS, Volume 1 (86/71&86/2039) and Volume 2 (87/1-87/637). Thus it follows the review published last year (87/417).The full references, names and addresses of authors can be readily found from the Atomic Spectrometry Update References in the relevant issues of JAAS, however, as an additional service to readers an abbreviated form of each literature reference quoted (except for those to Conference Proceedings) is given at the end of the review. This innovation is in response to suggestions from readers, and other comments as to possible improvements in future reviews are always welcome. It is hoped that succeeding reviews in this series will be extended to include X-ray spectrometry although this current review is principally concerned with the instrumentation for AAS, AFS, AES and ICP-MS. * Review Topic Co-ordinator, to whom correspondence should be addressed.80R JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, JUNE 1987, VOL.2 1. LIGHT SOURCES 1.1. Lasers Although lasers have a number of advantages over conven- tional sources, i. e., higher intensity, monochromaticity, low beam divergence, the availability of short and ultrashort pulses for studies of transient phenomena and coherence (well defined phase) (87/54), their use is still largely confined to diagnostics and to laser ablation for sample introduction. However, laser-excited atomic fluorescence spectrometry (LAFS) using a carbon tube furnace as the atom cell continues to attract attention (86/C877, 86/C916, 86/C990, see also section 6.3). Typically a dye laser pumped by a nitrogen laser is used to excite the analyte, the fluorescence being observed by a photomultiplier tube at an angle of 90" from the laser beam.This arrangement has been used to excite the atomic fluorescence of Au, Ir, Pd, Pt and Ru in an air - C2Hz flame (86/1282) and detection limits at the ng ml-1 level with linear dynamic ranges of >4 orders of magnitude have been reported. Detection limits were improved using a large- aperture detection system and a frequency-doubled dye laser for excitation of non-resonance AF. Laser-excited molecular fluorescence spectrometry with electrothermal evaporation (LAMOFS-ETE) has been modified for the determination of non-metals combined with added metals. Vaporisation was achieved using a graphite tube atomiser resulting in the formation of stable diatomic molecules which were excited by laser light (87/C144).Apparatus for AFS with laser pulses of 1-2 ps has been described and its analytical possibilities compared with those of similar spectrometers delivering nanosecond pulses (86/1372). Nd-YAG and Cu vapour pumped dye lasers have also been evaluated (86/C915) with regard to detection limits, growth curve linearity, precision and noise sources and accuracy in the analysis of real samples. A theoretical derivation of the signal obtained with the technique of intermodulated AFS has been presented (86/ 1102). One laser beam, tuned at a selected atomic transition was divided into two beams which were then amplitude modulated at different frequencies and recombined in a flame containing the vapour of the element being investigated. The fluorescence signal at the sum of difference frequency was then measured.A method for laser-saturated fluorescence for measuring concentrations from a single shot has also been proposed (86/1662). The method utilised the wing effect of a non-uniform laser irradiance, and the measurement was independent of both the collisional transfer rate and variation in laser power. If the laser power is known the method could also be used for measurement of the collisional transfer rate at any pressure. Two dye lasers, simultaneously pumped by an excimer laser, have been simultaneously directed into the analytical zone of an ICP or air - C2Hz flame (86/C914, 86/C1245, 86/1791). This technique, variously called double-resonance fluorescence or two-step fluorescence produces highly excited ion levels which are efficiently populated in saturated condi- tions, the resulting fluorescence being spectrally isolated with a monochromator.Spectral interferences from matrix ele- ments have been investigated using this method (87/387). Laser microprobes have again been used, in this instance for an investigation of the spatial distribution of sodium dimers (86/1398). A giant-pulsed ruby laser Raman probe was used for space- and time-resolved oxygen concentration and temperature measurements in a pre-mixed laminar CH4 - air flame (86/1655). It was suggested that the technique could be used for controIIing the stoicheiometry of fuel-lean flames with various equivalence ratios. In addition, by appropriately selecting different narrow-band interference filters, a simul- taneous determination of vibrational and rotational temperat- ures was proposed.Trace gas detection by laser intracavity photothermal spectroscopy has also been reported and the results obtained compared with phase fluctuation optical heterodyne spectro- scopy and thermal beam deflection in terms of practicality and sensitivity (86/1663). 1.2. Hollow Cathodes There have been few developments in the use of hollow- cathode sources. The effect of the boosting discharge on the concentration of ground state metal atoms in a boosted output discharge lamp has been studied (86/1609). A ten-fold decrease in the number density was noted when the boosting discharge was operated. Removal of atoms from the ground state was relatively slow, indicating the involvement of a heavy-body process.It was considered that the aggregation of atoms to form clusters was the most important process, and cataphoresis did not appear to play a significant role. Larkins (87/107) has carried out work to determine the effects of higher powers and currents on the resonance lines emitted by a range of HCL and EDL sources. In general, the tendency to self-absorption and self-reversal was greater for the more volatile elements, although the strong self-reversal of the Pb 217.0-nm line from an HCL was an exception. Electrodeless discharge lamps for less volatile elements incor- porated as iodides, showed relatively little variation in line width except at the highest powers. Quasi-elastic light scattering measurements were carried out to observe cathodic particulate material ejected by a high voltage spark discharge from an aluminium cathode (86/C826).It was suggested from examination of the data collected that the formation of observed particulates was due to the condensation of cathodic material in the post-discharge environment. Dawson et al. (87/C150) have measured magnetically induced optical rota- tions (coherent forward scattering) in atomic vapours using an HCL in the pulse mode. The authors described a system for which a fully corrected signal, proportional to the sine of the angle of rotation of the plane of polarisation by the atomic vapour was obtained. Preliminary results indicated a peak height sensitivity of 500 pg per 1.2" rotation for Cu using the 324.8-nm line. Non-specific transmission losses due to back- ground absorption could also be detected by modulation of the degree of polarisation (87/432).The background from non- specific emission could be determined from the base-line intensity of the spectrum or by additional modulation tech- niques. The performance of HCLs have been compared with a GDL (86/1681) and microwave-excited EDLs (86/1355). The merits of a plane hollow cathode and heated-coated systems have been discussed (87/C193). The dependence of the intensity of selected neon lines on the discharge current was recorded over a wide range of parameters (pressure, length, diameter and different orientations of the positive column), and the voltage - current characteristics were also recorded. A miniature hollow cathode emission source has been developed (86/C853).This water-cooled device was designed so that the hollow cathode could be quickly removed and replaced, and was used for the determination of trace elements in biological samples. A demountable hollow cathode source for the determination of major constituents in metal samples was also reported (87/131). The use of hollow-cathode lamps as excitation sources for analytical atomic spectroscopy has been the subject of a review with 44 references (87/589). A hollow-cathode plume has been utilised as an atomic emission source. Studies on atomisation and excitation processes (86IC856) and various applications have been reported (86/C810, 86/C814). The hollow-cathode plumeJOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, JUNE operated in a reduced pressure (1-5 torr) Ar atmosphere at currents up to 200 mA and powers of <70 W.The plume emerged through a small orifice (1.5 mm) in a disc that formed the analytical sample. Sample atoms were ejected directly into the base of the plume where excitation occurs (8611821). 1.3. Glow Discharges Glow discharges have received considerable attention in recent years. The source is convenient for laser-excited atomic spectroscopic studies of atoms sputtered from cathodic materials (86/C913, 87/124). A pulsed dye laser excited optogalvanic detection system has been used to monitor the presence of a transient molecular intermediate (SiH) in a chemical vapour glow discharge (87/36). The technique was reported to offer direct electrical signal generation, no optical background noise, good sensitivity and application to non- emitting species present in chemical vapour discharge plas- mas.The glow discharge as an atomisation source for laser-resonance ionisation has been used to produce a steady-state atom population from metal and alloy samples (87/58). In addition, non-conducting materials mixed with graphite could be pressed into suitable pins or discs for glow discharge atomisation. Glow discharge sputtering of Ag - Cu alloy surfaces has been studied by AES (87/55). The change in the intensity ratio between Ag and Cu emission lines was monitored during the course of sputtering. A reduction in the over-all sputtering yields with sputter time, probably due to the coating of Cu atoms on to the Ag grains, was observed.A hollow cathode discharge method for the determination of phosphorus present in metal samples and solution residues has been reported (86/974), although spectral interferences arising from matrix elements proved a significant problem. The use of GDL-AES has also been reported for the analysis of complex alloyed steels (86/C1504) and routine foundry alloys (86/ C866); and GD-MS used for trace determinations in high- purity solids (86/C1253). Charge-transfer excitation in glow discharges has been studied, in particular the charge exchange reaction for Ar - Cu systems (87K1.52). The results suggested that the 8.23 eV Cu I1 level was selectively excited by charge exchange with a metastable Ar I1 state with E ca. 0.02 eV, thereby increasing the Cu+ population.The effect was observed with plane and hollow cathodes in a Grimm lamp, using various inert gases and a brass hollow cathode in most instances, as these gave a more stable discharge than plane cathodes. Emission lines and relative intensities of Ag, Al, Cu, Sn and Zn were investigated in the range 200-600 nm using a Grimm-type discharge (86/1100). The observations made suggest that the energy levels and the excitation energies of each foreign gas play significant roles in determining the ionisation and excitation of the analyte atoms. Equipment for the excitation of a GD, with 1987, VOL. 2 81R glow efficiencies up to 300 W, has also been described (861729). 1.4. Other Sources Various plasma systems have been used as light sources. A two-electrode direct current plasma was used as an excitation source for flame atomic fluorescence by aspirating high concentrations of a metal into the plasma (86/1007, see also section 6.3).The shapes of atomic emission calibration graphs in the plasma and atomic fluorescence graphs in the flame showed that under certain experimental conditions the plasma could be considered to be either a narrow spectral line source or a pseudo-continuum source, depending upon the position of the sample introduction tube. The same authors have also reported some applications for the above system (86/1888), although the two-electrode version of the DCP used limited the precision of the measurements to 10% RSD. Measure- ments of self-absorption and analyte entrainment efficiency in a DCP have been reported (861C860).An inductively coupled plasma has been used as a line source in ICP-AFS to reduce matrix effects and improve detection limits (86/C912, see also section 6.3). Spectral interferences resulting from direct line overlap as well as ICP background emission were minimal compared with ICP-AES because of the selectivity of the fluorescence technique when a narrow line source is employed. However, ionisation interfer- ences were more pronounced than in ICP-AES as a result of the relatively lower temperature and electron number density of the sample cell ICP employed. Apparatus for measuring Thomson scattering from an ICP by laser light scattering has been reported (86/1394,86/C1507), and the theory of how the scattered-light spectra are related to electron-density fluctua- tions was also briefly described (86/1897).The results of fundamental studies of the ICP have been reported by a number of authors (86/C847,86/C861,86/C1205), and charac- terisation of ICP nebuliser aerosols using near-forward angle Fraunhofer diffraction was described (87/27). Spectral and noise characteristics of a xenon microwave inducedplasma lamp have been studied (86/1944). They were found to be more stable but less intense when compared with commercial 150-W high-pressure xenon short-arc lamps. The intensity of the line spectra that was superimposed on the continuum was higher than with the short arc, although it was possible to decrease this and improve the signal to noise ratio, and increase the total emitted intensity by increasing the gas pressure and/or the microwave power.A study of AES/AFS using continuum-source excitation from a Xe-arc lamp has been reported (8611876). The system employed a quartz refractor plate which was sinusoidally modulated and the second harmonic used for detection. Continuum-source AAS was the subject of a short review (87/110) and its use for multi-element AAS was also reported (87/57). The use of a continuum spectral source for the isotopic analysis of Pb has been described (87/385). 2. OPTICAL SYSTEMS AND DETECTORS 2.1. Optical Systems Fourier transform spectroscopy (FTS) has been extensively documented in the literature (see also sections 5.4 and 6.1). Stubley and Horlick (86/978) have reported the use of a Michelson interferometer system for Fourier transform spectrochemical measurements from the UV to the infrared. Laser fringe referencing was used for sequence digitisation, and interferograms were signal averaged under white-light interferogram control.A compact and transportable Fourier transform spectrometer which operates to ca. 170 nm has been described by Thorne and Harris (86/C1190, see also sections 5 and 6). The system employed a Michelson interferometer with arms at 10" instead of the conventional 90°, and catseye retroreflectors instead of plane mirrors. The instrument provided a resolution of 1.5 x 10-4 nm at 230 nm. The use of F"S in evaluating ICP emission spectra has received considerable attention, and design features for such instruments have been reported (86Kl236). Stubley and Horlick (86/979) have reported an excellent spectral response for their interferometer from 193 to 650 nm, although82R JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, JUNE 1987, VOL.2 quantitatively it suffered from a “multiplex disadvantage” and dynamic range limitations, so that detection limits were poorer by at least an order of magnitude compared with those obtained with a commercial direct reader-based ICP instrument. A windowed slew-scanning FTS has been proposed by the same workers to improve the quantitative performance (86/980). This consisted of a slew-scanning monochromator with wide entrance and exit slits coupled to the Michelson interferometer. Wavelength identification and resolution and simultaneous multi-element measurement within a 4-nm spectral window were provided by the interferometer, while the monochromator provided a method of selecting different spectral windows.The results of studies (86/802, 86/C1240) on the signal to noise ratio characteristics of ICP-FTS systems have been reported and showed that the noise was not evenly distributed across the spectrum but was higher on or near spectral peaks (86/802, 86/C1240, see also section 6.1). There was some distribution of noise from strong spectral features into the base line resulting in matrix dependent detection limits. The limiting noises were background photon noise at low concentrations and source flicker noise at high concentations. There appeared to be little, if any, transition region of signal shot noise limiting character. A low-noise laminar flow torch has also been described for use with ICP-FTS (86/C1241).Improvements in spectral resolution using photodiode array Fourier transform spectrometry have been reported by applying a moire fringe heterodyne technique to a square path Sagnet-type interferometer with a 512-element photodiode array. The instrument was capable of 0.9-nm resolution at 546 nm (87/63). The use of an ICP-excited ICP resonance monochromator and fluorescence spectrometer has been suggested as an alternative to emission spectrometry in order to alleviate spectral interferences and avoid the expense of a high- resolution monochromator (86/1881, see also section 6.3). The sample was aspirated into a source ICP and the resulting emission was used to excite atomic and ionic fluorescence of a sample aspirated into a second ICP.By using the second plasma as a resonance monochromator in this way, linear dynamic ranges of up to 5 X l o 7 were obtained. The use of a resonance monochromator is also reported to increase the detection sensitivity of weak lines (in comparison with dispersive monochromators) by more than two orders of magnitude, and in AAS to decrease the mean-square error several times (87/358). Other spectrometer designs reported include the combination of a linear photodiode array detector and kchelle spectrometer with a unique dispersion - selection - recombination line selector (86/C804), a time-multiplexed spectrometer with a single photomultiplier detector (86/C805) and a sequential spectrometer that is both direct peaking and has its focus on the Rowland circle of a simultaneous spectrometer (86K932).Davis and Winefordner (86/C840) have reported a coherent forward scattering atomic spectrometer. The study utilised the Voigt effect, with two orthogonal Glan - Foucault polarisers to detect the magneto-optic rotation of polarised light produced by a transverse magnetic field. A xenon-arc lamp excited resonant transitions in a graphite furnace atomisation cell, and amplitude modulation with a lock-in amplifier allowed the detection of the coherent signal. A Heath monochromator was used to slew scan to the wavelength of interest. Direct optical probe sampling of radiation from an ICP has been used for analytical and diagnostic studies in the vacuum UV region (86/C823). The horizontally oriented ICP flowed around the tip of a water-cooled copper cone that supported a circular orifice.The sampling cone was mounted on the optical axis of a vacuum monochromator, and no lenses or optical windows were used in the optical path leading to the detector, although the path was purged by a He or Ar stream. Spectral line detection down to 80 nm was described. A computer controlled fibre optic modular ICP monochromator has been described (86/C1171 , 86/C1189) which operated in the spectral range 165-800 nm. The system used optical fibres as the relay optics in combination with a conventional optical relay system from the source to the entrance slit. An emission spectrometer with four spectral systems and several light guides has also been described for multi-element analysis (87/426).Of interest for reference, a number of publications have described elemental spectral data. An atlas of ICP-AES spectra of REEs has been described (86/C1184), as have details of the Ni spectrum between 250 and 300 nm (87/82) including relative intensities and spectral interferences for lines not reported in the M.I.T. Wavelength Tables. An extensive work has also been published (87132) detailing spectra and relative intensities of Ar, Br, C, C1, H, N, 0 and S lines in the red - near-infrared region for a “pure” argon ICP. The prominent spectral lines for 45 elements using an Ar - N2 ICP have also been reported (87/33). Boumans and Vrakking (86/C1164, 86/C1864, 86/C1865, see also section 6.1 and JAAS, 1986, 1, 67R) continued their assessment of spectral interferences in ICP-AES.This investigation includes a theoretical and experimental study of the effect of spectral band width on selectivity, limits of determination, limits of detection and detection power. The effect of spectral band width on the inaccuracy in net signals originating from wavelength positioning errors in a slew-scan spectrometer was discussed, together with an assessment of hydroxyl (OH) band interferences using the ratio of the limit of determination and the limit of detection as a rational criterion. 2.2. Detectors Further advances have been reported in detection technology related to optoelectronic imaging detectors and optical systems. A system employing a charge-injection device and a reduced image size kchelle spectrometer has been evaluated and found to offer sensitivity comparable to a PMT (86/ C1580).Two different imaging spectrometers which provide quantitative, spectrally resolved maps of the entire ICP simultaneously have been described (86/C1217). The elec- tronic slitless spectrograph used a de-magnified image of the source as the effective entrance slit. At the focal plane of the spectrograph a separate image of the plasma was produced for each analyte or plasma emission line. While this arrangement provided high light throughput there was an inherent trade-off between spectral and spatial resolution. The monochromatic imaging spectrometer employed optics to feed collimated light through the entrance slit of a Czerny - Turner mono- chromator. After passing through the monochromator, exter- nal optics reformed a monochromatic image of the source on the face of a two-dimensional detector, Two-dimensional transient images have also been studied using a silicon intensified target (SIT) vidicon detector (86/C15 12).Signals were processed by an optical multi-channel analyser and transferred to an IBM-PC microcomputer configured with a data acquisition board. Fast acquisition algorithms provide real-time data evaluation, and further data processing was available for detailed study of the source. The same group of workers have also used a SIT vidicon detector for tomographic reconstruction studies of an ICP (86K1514). Photoelectric sensors, such as a cadmium sulphide photo- conductive cell, have been used for several applications including the monitoring of low-temperature ashing (86/1047) and the measurement of flame temperature distributions by IR emission computed tomography (860401).A number of papers have described the use of photodiode array detectors. Spatial resolution enhancement with a linear photodiode array has been reported by McGeorge and Salin (8711 14). The technique utilised the photodiode geometry and the intensityJOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, JUNE 1987, VOL. 2 83R profile of the image to determine positions to sub-diode accuracy. A series of lines was used to calibrate the detector system and the resulting information then used to compensate for the non-linear change in dispersion across the spectral region falling on the photodiode array (86/970). Spatially resolved electron density measurements in Ar, Ar - Nz and Ar - O2 ICPs have been made (87/629).The electron density maps produced clearly showed the electron density values to be highly spatially dependent. A new spectrometer employing a self-scanning linear photodiode array camera as the detector has been described for operation between 185 and 415 nm (86K876, 86K1170). A similar development has been made by Blades et al. (86/C1972) who have reported a spectrometer with both photodiode array and PMT detection. The photodiode array was used for the detection of spectral information at wavelengths greater than 280 nm and the PMT for wavelengths less than 280 nm. The use of red and near-infrared photodiode arrays has been reported for the determination of Br, Cl, F, I and S (86/1834) and C, H, N and 0 (86/1048), in ICP emission spectra and for the determination of oxygen in organic solvents using an ICP (86/983).However, the limitations of photodiode array detectors for spectroscopic intensity measurements has been the subject of study by Winge et al. (87/31). Misregistry intensity errors, which occur when the spectral line is not in exact registry with the diode or diodes from which its intensity is being measured, were found to be as high as 25-30%. These errors were documented for a range of spectral band widths and for a single diode (pixel). A helium discharge afterglow has been described for use as a gas chromatographic detector (86/1870). The detector differed from those previously reported, such as the He glow or discharge detectors, in that the analyte stream was not introduced into the primary discharge, and thus extinction and contamination were avoided.Absolute limits of detection in the picogram range were reported. The same workers (86/C1151) later mounted this type of detector directly in front of the entrance slit of a vacuum spectrometer such that the afterglow was operated in a He atmosphere without air entrainment and with no intervening optics to absorb any optical radiation. Spectral data were obtained at wavelengths below 100 nm with this arrangement. Other advances reported for chromatographic detectors include a study of noise sources in MIP-GC detectors (86/C816) and a water cooled radiofrequency powered gas discharge tube developed to reduce peak tailing resulting from degradation of discharge tubes at high temperature (86/1046).A double centering insert laminar flow torch which kept the plasma away from the walls of the discharge tube was also reported (86/C858, see also section 6.1). This design facilitates flow-rates compatible with capillary gas chromatography. A Fourier transform red - near-infrared AE spectrometer has been used as a simultaneous multi-element detector using an MIP as an interface (86K1242). 3. BACKGROUND CORRECTION 3.1. Optical Systems Few new developments in optical systems for background correction in atomic spectroscopy have been reported. Zee- man-effect background correction has continued to attract attention (87/621). The dynamic range of analytical curves was reported to be extended ten times when intensity measure- ments are made at three different field strengths, rather than just at zero and maximum field strength.Dougherty et al. (86/C878) described some preliminary data for the application of Zeeman-effect background correction for laser excited atomic fluorescence spectrometry (LAFS) in a carbon fur- nace. Zeeman-effect background correction may be applied to AF in a similar way to that in AAS but using a different magnetic field configuration. An a.c. magnetic field with the laser light directed parallel to or, in the case of conventional sources perpendicular with, the magnetic field, could be employed. Over compensation using Zeeman-effect back- ground correction has been further assessed using a transverse a.c. Zeeman-effect corrector system with the magnet acting on the graphite atomisation cell (86/1787).Thirty elements and 53 spectral lines were investigated in the presence of relatively large amounts of Co, Mn or Ni. The study revealed three cases of background overcompensation (on Au at 267.6 nm, B at 249.7 nm and Hg at 253.7 nm), all being caused by overlap of a Co line adjacent to the analytical line. Over-correction in the determination of Cd at 326.1 nm, believed to be due to splitting of PO bands, and Pt on Fe at 271.9 nm have also been reported (87/634). Background over-correction errors as observed in ETA-AAS have been the subject of a review with 28 references (86/1909). Smith - Hieftje background correction has also received attention. The technique has been applied successfully for the determination of trace metals in gas turbine fuels by FAAS (86/C1557), and the direct determination of Cr in solid gallium arsenide semiconductor material by ETA-AAS (86/1650). As Smith - Hieftje background correction relies on the broaden- ing and self-reversal of emitted lines as the hollow-cathode lamp current is increased, the design and operation of such lamps is of obvious importance.This has been the subject of a study by Schleicher et al. (86/C839), who presented data on new HCL designs after investigating parameters such as filler gas, cathode and anode geometry. The optimisation of Smith - Hieftje background correction has also been studied by other workers (86/1914) using a cadmium hollow-cathode lamp. The results obtained were compared with Zeeman-effect back- ground compensation. The performance of the various background-correction techniques have been evaluated.Stray light in Zeeman and Smith - Hieftje may cause errors in background correction when the stray light is not completely absorbed by the sample matrix (86/C778, 87/132). Experimental results have shown that the stray radiation was located close to the resonance wavelength of the analyte. However, non-absorbable stray radiation as well as non-linear response of the electronics, led to a limiting absorbance of the gross AAS signal and to errors in the net absorbance in the presence of high-background absorbance. Zeeman and Smith - Hieftje background correction techniques have also been compared in terms of loss in sensitivity, ability to correct for rapidly changing backgrounds and various other differences between the systems such as the ability to correct for the presence of background matrix in the determination of Cr (86/C1565). However, such comparisons have proved difficult, as although the same sample, sample introduction technique, temperature programme and detection protocol were employed, less than optimum operating conditions were sometimes required for each instrument to make a direct comparison.The timing of the measurement of background and total absorbance on the accuracy of background correction has been further investigated (86/C1564). Minimising background correction errors was, however, found to be very difficult due to the problems of switching very rapidly between the two measurements with both the Zeeman-effect and Smith - Hieftje approaches.A number of other studies have also compared various background correction systems for specific applications, such as Zeeman-effect with deuterium-arc84R JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, JUNE 1987, VOL. 2 corrected ETA-AAS and continuum-source wavelength modulated AAS for the determination of Cu in urine (86/C920). Zeeman-effect and deuterium-arc background correction have also been compared for the determination of Se in environmental samples (86/C921), As and Se (86/C1594), Pb in whole blood (86/1757) and Co in urine (87/234). A method for evaluating the performance of the background corrector in ETA-AAS has been reported by Niemczyk and Yin (86/985). Instead of using a neutral density filter or wire gauge, the correction efficiency was evaluated under con- ditions that mimic those of an actual experiment. This work exploited the vaporisation as molecules of alkali and alkaline earth halides, thus causing a “background” absorbance that mimics the performance of the actual sample.Sodium iodide was chosen as the test molecule, and the experimental data obtained indicated that the system corrected the background to an absorbance of <0.01, as long as the peak background absorbance was less than ca. 0.6. For backgrounds derived from large amounts of sodium chloride a correction method based on passing the sample solution through a U-shaped tube packed with chelating resin has been suggested (87/395). Absorption measurements were made before and after passing through the resin, the technique being employed for the determination of 0.05-0.5 pg ml-1 of Cd in the presence of 3.5% sodium chloride.Other methods reported for reducing background absorption in furnace work include the use of aerosol deposition and delayed atomisation techniques (86/ ClOOO), and use of a furnace alignment jig (86/1704). Halls and Fell (87/47) have determined Cr in urine without interference by careful attention to the atomisation tempera- ture, and use of conventional deuterium-arc background correction. An extensive study of background in an ICP mass spectrum has been reported by Tan and Horlick (87/30, see also section 6.4). The background spectral features were measured for the nebulisation of water and for 5% solutions of HC1 and HzS04.Background spectra were presented for all of these solutions for the mass range 1-84 u, and extensive tables are presented for observed species and their isotopic combinations. Sample preparation methods to minimise polyatomic ion interferences in ICP-MS have been reported (86/C1104), and various procedures to simplify ICP mass spectra were described (86/C1114). The influence on ultratrace analysis of back- ground and matrix response has been described by Gray (87/66). Detection limits obtained under compromise operat- ing conditions are given for a range of elements in both single-ion and multi-element detection modes. 3.2. Computer Aided Systems The use of microcomputer controlled background correction has been the subject of a number of publications.A system for use in AAS and AES based on a high-resolution kchelle spectrometer has been reported (87/C147). Wavelength modulation was employed to perform automatic background correction on signals as high as 1.5 A, and a microcomputer was used to control data acquisition and perform data processing. In the ETA mode, the microcomputer program provided peak-height and peak-area data simultaneously and a procedure was used that allowed expansion of the linear calibration range by measurement of absorption in the wings of the AA profile (86/C780). Second derivative wavelength modulation has also been employed in AES and AFS (86/1876). The AE and AF signals were collected simul- taneously using sinusoidal wavelength modulation and phase sensitive detection of the second harmonic mode.The system, consisting of a continuum source, Ar-separated air - C2H2 flame and a wavelength-modulated monochromator, was used for the analysis of a copper alloy. A software-controlled system for automatic background correction in ICP-AES which employed the technique of refractor plate wavelength displacement was also reported (86/1653, 86/1892). A mathematical treatment of multiple point data that removed the background contribution to the data has been described (86/1006). This background subtraction method was applied to the determination of low amounts of U in phosphoric acid by ICP-AES in the presence of spectral interferences and facilitated a four-fold improvement of the detection limit. A chemometric technique for deconvoluting both the background and spectral interference contributions to the analyte line has also been demonstrated (86K1182).The procedure involved scanning of a spectral segment on either side of peak positions. Concomitant solutions were nebulised separately in order to characterise the spectrum of each interference. A method for extending the dynamic range for Zeeman ETA-AAS has been proposed (87/367). The calibration graph was made by slicing the absorbance time profile at a height Awl, which is higher than (1/20)Ao and lower than (1/2)Ao, where A. is the peak height and W, is the width resulting from the slicing procedure. The dynamic range could be extended more than ten times compared with the usual peak-height method. The application of multiple linear regression of wavelength scans for spectral interference correction in ICP has been reported (861C1185). A com- puterised spreadsheet was used for the matrix calculations.The deconvolution of atomic absorption spectra has been reported by Harnly and Holcombe (86IC886, 87/C145) to reduce significantly errors associated with traditional instrumental background correction techniques. These arise, particularly in ETA-AAS, from having to measure separately both the sample and reference signal. It was found that the first derivative of the background absorbance signal was proportional to the systematic errors and when taken for one reference could reduce the magnitude of the error by a factor of 20. As the background absorbance exhibited primarily a low frequency noise component, and the number of reference points taken affected the susceptibility of the computed absorbance to low frequency noise, taking a larger number of reference point values, will inevitably improve the correction.It was further demonstrated that by superimposing a plot of the second derivative over a pair of reference measurements and using a quadratic algorithm to give a non-linear interpola- tion the error could be reduced by a further factor of 20. Quantification could therefore be achieved by multiplying the derivative by an appropriate constant. This approach appears to offer an attractive chemometric method for improving background correction in ETA-AAS, the authors however give no indication of the analytical significance, in terms of real data, of this method.An interesting paper by Taylor and Schutger (87/25) reported a sophisticated “user friendly” computerprogram written in FORTRAN that intended to replace the human factor in signal interpretation of background correction interferences. Scan data collected from a high- resolution computer controlled monochromator were run through the program, which, as an expert system, performed the automatic correction required and thus obviated the necessity for operator decisions. A detailed description was given of how the program performed peak detection, peak smoothing, background and spectral correction routines. The data analysis and correction carried out with this program, were shown to be superior when compared with the classical three-point measurement technique.Once again a number of papers have appeared addressing the recurring problems of matrix effects and spectral interfer- ences in ICP-AES. The use of an internal standards method to correct for matrix interactions has been statistically evaluated by Sedcale et al. (87/73). Selecting a series of six elements as internal standards, these workers used the internal standard ratio method (ISRM) and an analysis of variance (ANOVA) for each analyte. The influence of various matrix components including KC1, CaC12, NaSi03, polymaleic acid (PMA) andJOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, JUNE diethylenetriaminepentaacetic acid (DTPA) in 2 M HC1 were investigated. Not surprisingly, the conclusions drawn from this study indicated that before an internal standard method can be used as a diagnostic marker for noise reduction, well defined response factors must be established for the entire range of matrix conditions encountered.In a similar way, both experimental factorial design and regression analysis have been used, to study the influence of hydrochloric acid and sulphuric acid matrices on analyte signals (86/725). The stabilisation of regression coefficients enabled a flow chart to be constructed which compensated for the background signal associated with mineral acids being transported to the ICP torch. It was clear however that neither of these approaches to signal correction were able to compensate for changes in matrices between samples. For applications therefore where matrix matching is relatively simple, for example in metallur- gical samples, techniques such as the generalised internal reference method (GRIM) (87/43) or simple ratio intensity comparisons (86/1698) are perfectly adequate.Such tech- niques, which in addition to requiring the compositional nature of the analyte matrix, commonly include a degree of computer manipulation of the emission data, can offer simple calibrations, good accuracy and precision in the order of 0.1-0.3% RSD. One emerging area where internal standards find an important use is in the coupled LC - ICP systems. Kosman et al. (86/C1155) evaluated two methods for perform- ing correction for long-term drift in LC - ICP determinations. The first approach was to add a reference element to each sample in equal concentrations, whilst the second was to dissolve an internal standard in the mobile phase. The results obtained from this study indicated that either of these internal standard methods were able to compensate for drift.The paper outlined the criteria necessary for the practical selection of an internal standard but caution was stressed in this matter as an incorrect choice will result in improper correction arising from gross differences in retention times or peak widths between the standards and the analytes. A critical review (871516) on the use and misuse of the internal standardisation technique considered the practical value of this methodology 1987, VOL. 2 85R for use with ICP-AES. The introduction of an interactive matrix matching procedure (IMM) reported by Ramsey and Thompson (87/C218) seems more amenable to variations in the sample matrix.Analytes present in for example a limestone matrix, are subject to wide variability in calcium concentrations, which correspond to broad-band spectral interferences from the calcium lines. The IMM procedure used a computer controlled, on-stream, variable diluter to adjust each sample to match a pre-determined matrix concen- tration, enabling standardisation of the calcium matrix. The only limitation of this technique is the possible dilution of analytes below their detection limits. The authors reported, however, substantial improvements in accuracy for a wide range of analytes using IMM. Lorker et al. (86/C755) described a chemometric technique of deconvoluting both the background and spectral interfer- ences from the spectral lines.The practical limitations of this method are however that a peak scan of each individual component of the spectrum is required, and thus the problem of having to have prior knowledge of the matrix composition still exists. In a series of papers by Ramsey and Thompson (86/C822, 86lC2036, 87/C155) a parameter related internal standard method (PRISM), was decribed. This approach was designed to compensate for differing analyte line intensities, associated with their individual matrices, thus overcoming the problem of matrix matching or having to use a standard additions method. Precisions using PRISM were reported to be of the order of 0.4% RSD for major constituents in geological samples. The authors suggested that this approach may eventually provide the basis for a more fundamental type of matrix correction in ICP-AES.The increasing use of chemometrics employing single or combined algorithms, running on powerful computing equip- ment have been demonstrated to facilitate improved back- ground correction procedures. Further developments in instrumental design, together with the growing area of mathematical correction, offer the opportunity for powerful background correction techniques in both AA and AE instrumentation. 4. AUTOMATIC SAMPLE INTRODUCTION The increasing number of publications related to automatic sample introduction over the last review year, have mainly been on flow injection (FI) and coupled chromatographic techniques. These two subjects will be considered individu- ally, but obvious links between the two methodologies will be apparent.In addition to these two important areas, other interesting and novel techniques have also been reported in the literature for automatic sample preparation and introduc- tion and these will be considered separately in the latter part of this section. Automatic sample introduction, in general, including the topics mentioned above together with many other aspects of sample introduction into ICP spectrometers, was the subject of a broad-based review by Barnes et al. (86/C1493). The reader will find references to more specific reviews in the relevant sections of this Update. 4.1. Flow Injection The use of FI as a sample introduction technique in atomic spectroscopy has stimulated over 40 publications in the last 12 months, including four detailed reviews (86/C1142, 86/1680, 87/362, 87/584) which included principles, apparatus, applica- tions and performances of FI compared with conventional procedures.A rather sophisticated computer-controlled system has been described by Martin et al. (86/C863), which enabled intelligent sample handling based on a Fiatron SHS-3000 FI instrument. This system automatically performed the analysis of undiluted samples, carrying out up to 200-fold dilution if necessary, selected the optimum calibration curve for each element and spiked the samples with standards thus enabling standard additions studies. The authors reported that the analysis of 76 samples of widely varying concentrations could be carried out totally automatically, with no operator intervention, using the system described coupled to a 36-channel ARL 3400 ICP spectrometer. More fundamental work on FI has focused on the kinetics of instrumental response (86/1867) and the interesting area of nebuluser efficiency and design (86/1607,86/1915).One group of workers (86/1607) published results that compare their direct injection nebuliser with a conventional pneumatic system for use with ICP-AES. They reported that the direct method offered clog-free operation and ng ml-1 limits of detection for a 30-~1 sample, thus achieving detection limits for some elements comparable to those obtained for elec- trothermal vaporisation ICP-AES. Hardy and Beecher (8hl 1915) demonstrated, however, that by careful control of sample flow-rate when using FI-AAS with a conventional86R JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, JUNE 1987, VOL.2 nebuliser system, nebulisation efficiencies may be improved by factors of 4-12. Despite this improvement in nebuliser efficiency, the signal to noise ratios for the FI-AAS peak- height and -area measurements approached, but never exceeded, the ratios for conventional nebulisation. Although many authors indicated the improvements in precision that are possible with FI and the ease with which calibration can be achieved, few concentrated specifically on these aspects (86/1445, 86/1459, 87/C185). Controlled disper- sion or concentration gradients have featured in two papers (86/1457, 87/C185), which illustrated the ease with which calibration could be achieved with FI, whilst removing the need for serial dilution.An improvement to the concentration gradient approach has been suggested by Zagatto et al., (8611445) who advocated the simultaneous injection of several plugs into the same carrier stream in order to obtain overlapped zones. Such an approach was reported to give better precision and improvements in the standard additions method over the conventional concentration gradient methods. In a further paper, Zagatto et al. (87/438) described a hydrodynamic injection system using a specialised injection duct for the analysis of low sample volumes (1-10 pl). The system, designed to operate with a single peristaltic pump was reported to reduce mechanical flexibility and diffusion effects, resulting in precisions of the order of 1% RSD.The application of the FI technique to continuous flow hydride generation represents a popular and growing applica- tion of this methodology. Whilst the majority of papers described AAS as the detection system, the use of direct current plasma atomic emission spectrometry (86/C884) and molecular emission cavity analysis (86/1633) have also been reported. These two papers identified the advantages of the continuous flow approach over the batch introduction system in terms of precision and levels of detection. Despite claiming improvements in detection power, the figures quoted by Buguera and Buguera (86/1633) of typically 0.1-10 pg ml-1 were still 100-fold higher than those obtained by AAS detection. The majority of FI manifolds described have been laboratory constructed and full instrumental details were usually given.One commercially available system from Varian Associates has been the subject of two papers (86/C784, 86/C951) which described its applicability to both AA and AE instrumentation. In these papers the performance and chemical reaction conditions were compared for both batch and continuous flow systems. In common with a number of other studies (86/C784, 86/C95 1 , 86/C953) interference eflects from transition metals were evaluated and the general conclusion reached that the continuous flow methods signifi- cantly reduce interferences. Whilst most of these methods relied on an in-line gas - liquid separator to remove the volatile hydrides from the reaction mixtures, Straka et al. (86/1780) described a dual phase gas diffusion technique for the removal of the hydrides which reportedly decreased interference effects even more effectively than conventional FI methods.The degree of sophistication of these systems ranged from a basic injection system (86/1633, 86/2029) to fully automatic sample introduction (86/C951, 86/C953, 86/1009, 86/C1581). One such computer-controlled system (86/C1581) employed an Apple computer operating in BASIC which controlled the hydride generator and autosampler, whilst carrying out data acquisition from the AAS instrument. Manual (86/2029, 87/448) and automatic (86/C953) sample injection methods, employed for the determination of Se by AAS provided precisions of 1 and 2.8% RSD, respectively. Good accuracy was confirmed by the use of CRMs.The most popular atom cell used in conjunction with FI - hydride generation systems was the heated quartz tube optically aligned in an AAS spectrometer. Heating of the tube was achieved by either an air - C2H2 flame (86/C784, 86/C951, 86/C1581) or electrically (8612029). However, Yao et al. (86/1009), by introducing the hydrides directly into the air flow of an air - C2H2 flame, surprisingly reported detection limits for As, Bi, Sb, Se, Sn and Te of the order of ten-fold less than those obtained by the heated quartz tube method. It seems probable that the interest in this area of automatic sample introduction will continue to develop with practitioners already now reporting fully auto- matic replicate determinations of more than 50 digested samples per hour (86/C953).Flow injection provides the opportunity to incorporate an in-line pre-concentration step. This approach has been applied to both AA (86/1316, 86/C1549) and AE (86/C1144, 86/1671, 86/2019, 87/339, 87/475) techniques and involved packing activated alumina (86K1144, 86/2019, 87/339), exchange (86/1316,86/C1549,86/1671) and chelating (87/475) resins into microcolumns. Whilst some improvement in the detection limits, typically five fold, and extensions to the dynamic working ranges were achieved (86/1671), it is the ability to pre-concentrate elements, many 100 fold, on, for example, Chelex 100 at a rate of 20-75-fold per minute which makes this technique attractive to users of ICP and FAAS systems. The enrichment achieved by this method was reported for various materials, including an iminodiacetate based chelating resin (87/475), Dowex A-1 (86/1316), HC-pellionex SCX (86/ C1549) and activated alumina in the basic form (86/C1144, 87/339), these materials being packed in columns of typically 1-2 mm i.d.and a few cm in length. Numerous elements have been determined using these materials, however sequential elution of selective groups of elements may be necessary with the activated alumina columns (86/2019). In many papers (86/C1144, 86/C1549, 86/1671, 86/2019), details were given of the important chemical and physical parameters for these systems together with the optimum conditions that were required. Some workers have claimed that this simple technique using a standard ICP or FAAS system, is compar- able in detection power to the more sophisticated techniques such as ETA-AAS and ICP-MS.Some novel and interesting variations to the FI method employing more traditional classical chemical approaches, easily adapted to the continuous flow philosophy, were reported. One such paper described a continuous precipitation method built into the FI manifolds (87/C192). The precipitate was formed by injecting an anion into a carrier flow containing a cation and collected on a conventional stainless-steel HPLC filter. Two flow configurations were then evaluated. The first, an indirect method, measured signal decreases in the carrier flow corresponding to the degree of the precipitation, whilst the second configuration required the dissolution of the precipitate by the introduction of an appropriate reagent.Whilst the authors expounded on the advantages of a FI system over batch procedures, it is clear from their paper that the methodologies proposed were experimentally difficult to use and problems may be encountered in obtaining acceptable analytical data. An in-line process using a microwave oven has been used for the mineralisation of samples (87/239). In this application, the authors reported that for the determination of Cu, Fe and Zn by AAS, no pre-treatment of blood samples was necessary and an RSD of <3% was achieved in all instances. Comparison of this novel FI method with conventional treatment and spectrophotometric detection gave close agreement for blood samples. The automation of traditional liquid - liquid extractions has been carried out using specially constructed FI manifolds (86/1023).In this work, the extraction of a Cd - DDTC complex into CC14 was performed and then detection was by ICP-AES. Optimisation of conditions , particularly for plasma stability, were discussed and a detection limit of 0.4 ng ml-1 of Cd was reported with a 1.5% RSD. Liquid - liquid extractions based on an ion-pair technique have been used by Silva et al. for the indirect determinations of nitrate and nitrite in meats (87/304) and the analysis of waste waters for anionic surfac- tants (87/457). In these applications, the nitrate and nitriteJOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, JUNE 1987, VOL. 2 87R were reacted with bis(2,9-dimethyl-1 ,lo-phenanthroline) - copper(I), whilst, similarly, a detergent - (1 ,lo-phenanthro- line) - copper(I1) ion pair was formed.Extraction into 4-methylpentan-2-one was then carried out with subsequent determinations of Cu being achieved by AAS. A selective oxidation step using cerium(1V) enabled differentiation to be made between the nitrate and nitrite species, which were detectable at pg ml-1 levels. The indirect determination of anions was also the theme of a paper by Haj-Hussein et al. (86/1382), where a system for determining cyanide down to 1 pg ml-1 was described. The introduction of cyanide into a FI system that contains an in-line column packed with CuS facilitated the determination of Cu, as cuprocyanide complexes, to be carried out using FAAS detection. Details of experimental conditions were given in this reference together with data on anionic interfer- ences.No indication was given, however, of the column life, but a precision of 2% RSD was quoted for a 23 pg ml-l cyanide standard, Signal enhancement of Fe associated with Ce and La has been exploited in a FI system for the indirect determination of Ce and La by air - C2H2 FAAS (86/1451). This paper , which described the optimum working conditions and chemical parameters required, reported the method to be 5000 times more sensitive than the direct technique of using a N20 - C2H2 flame. In addition, samples with a high salt content produced no apparent interferences, however, it was necessary to prepare samples in sulphate and/or nitrate solutions. This FI application offers the characteristic advan- tages of low sample volume (54 pl) and a high sampling frequency (150 h-1).Other papers of interest in the area of FI discussed the combination of detection systems. A UV detector operating at 254 nm being used for fulvic acids analysis was coupled in series to an AA spectrometer for trace element determina- tions using a FI technique (86/C1549), whilst an electrochem- ical detector coupled with AAS was used for the determina- tion of Ca and Mg in waters (87/312). In this report a tubular poly(viny1 chloride) membrane electrode was used for the potentiometric determination of Ca followed by a FAAS assay for Mg. The system incorporated an on-line dilution facility for Mg determinations. It is evident from the literature that FI is becoming an increasingly popular technique for automatic sample process- ing and introduction for atomic spectroscopy.As basic understanding of manifold design improves, simple and attractive procedures for sample pre-concentration and matrix modification become readily compatible with FI methodol- ogy. Above all, the level of precision, speed of analysis and the ability to automate fully the system makes FI a most attractive technique to the practising analyst, and one in which there will be many interesting developments in the future. 4.2. Chromatographic Sample Introduction There have been further reports of chromatographic inter- facing to both AA and AE instrumentation (see also JAAS, 1986, 1, 140R). The combination of these techniques has not occurred with sample introduction as the main aim, but has been stimulated by increasing interest in trace elemental speciation.The relevance of coupled chromatographic atomic spectroscopic techniques to elemental speciation studies has been the subject of three general reviews (86/C1147,86/1813, 87/C158) , covering the mechanisms and equipment required in a wide range of gas chromatographic and high-performance liquid chromatographic interfaces, for both AA and AE instrumentation, including post-column hydride generation. Numerous examples of the applications of these interfaces to food and environmental trace elemental studies were given. The coupling of gas chromatography (GC) to element specific detectors has been restricted to readily volatile or easily chemically volatised elements. The resulting gaseous form of the analyte from this type of chromatography makes interfacing a relatively simple procedure.This has formed the basis of an exhaustive review (87/90) which includes the various structures for plasma generation, sample introduction and the expected detection limits for a wide range of applications. Sources of noise in a MIP - GC coupled system have been investigated in terms of the factors which influence precision (86/C816). The experimental details for a range of operating conditions were given together with precision and signal to noise ratios obtained. The ability of the MIP to excite atoms such as Br, C, C1, F, H, N, 0 and S leads the technique into slightly different fields of application than those normally encountered in, for example, ICP-AES. This area of non- metal determination led to the development of an interesting interface between a GC - MIP coupled with a Fourier transform red - near-infrared atomic emission spectrometer (86/C1242).Uden et al. (86/C1148,87/C170) described the use of apyrolysis gas chromatography - helium microwave induced plasma system with both the low pressure Evenson and atmospheric pressure Beenakker cavities, for empirical for- mula determinations of hydrocarbons, chlorinated organics and organosilicon compounds. A direct application of this technique has been used for the identification of nitrogen and sulphur compounds associated with heavy crude oil fractions (86/C1149). More fundamental studies into deuterium reac- tions with numerous compounds and functional groups is one novel way of using the analytical advantage of the GC - MIP coupling.More conventional applications of this technique have included pesticide characterisation (86/C1150), analysis of biological material for dimethylselenide (87/450), and speciation studies of various organometallic compounds in air samples (87/C171). Although the MIP represents the most popular detector system for GC coupling, DCP (87/C563), ICP-AES (861C807, 87/88) and AAS (86/C927, 86/1629, 87/C158, 87/C159) have all been used by various workers for alkylmetal and halogenated compound studies. In addition, the separation by GC of pre-column formed elemental hydrides is described by Rigin (86/1928), who achieved the determination of numerous elements employing an interesting GC - AFS interface. The coupling of high-performance liquid chromatography (HPLC) to atomic spectroscopic techniques is finding numer- ous applications in the study of non-volatile elemental species.The main limitations reported for this type of interface were the losses in sensitivity that occur when real samples were fractionated on the separatory column and were then subjec- ted to the inefficient nebuliser systems and operating paramet- ers associated with AA and AE instruments. Two papers of particular interest (86/C892, 86/C1482) considered some of the fundamental aspects of HPLC - ICP couplings and described the limitations and possible improvements that can be made to operating parameters, torch design and aerosol generatiodtransport properties. A series of interesting papers concentrated specifically on the problems of nebuliser effi- ciency in HPLC - FAAS and HPLC - ICP interfaces.A simple yet effective coupling that utilised pulse nebulisation for a directly coupled HPLC - FAAS system has been described by Ebdon et al. (86/C2038, 87/C198), who achieved a further signal enhancement with this system by placing a slotted tube atom trap device in the optical axis of the instrument. The replacement of a conventional pneumatic nebuliser with the more efficient ultrasonic system appeared to give the adequate improvement in sensitivity necessary for the FAAS determi- nation of Mg and Zn species in a urine sample following HPLC separations (86/1755). Interestingly the authors reported no apparent memory problems with this system for this particular application. In the area of HPLC - ICP interfacing Jinno et al.(86/728) described a modified cross-flow nebuliser with no spray chamber enabling more efficient sample introduction whilst Koropchak and Winn (86/C883, 871599) evaluated two methods for increasing transport efficiency by firstly adapting88R JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, JUNE 1987, VOL. 2 a thermospray device and secondly employing a polymeric frit nebuliser system. The deployment of a direct injection nebu- h e r (86/C917) offering 100% efficiency has been described. However, in order to reduce solvent loading in the atom cell, low sample volumes (100-200 vl min-1) were required and so an HPLC eluent splitting device was necessary to give a constant low-volume sample delivery.The direct introduction of low-volume samples without the need to split the eluent has been achieved through the direct coupling of a microcolumn HPLC - ICP system (86/728). In this application some problems were encountered in obtaining a reproducible emission signal, this was alleviated to some extent by heating (at 60-80 "C) the lower section of the plasma torch, particu- larly when using an aqueous mobile phase. Continuing on the theme of 100% transport efficiencies, Faske and Browner (86/C843, 86lC1487) have advocated the use of a MAGIC interface based on a mono-disperse aerosol generation unit with controlled evaporation to reduce solvent loading in the plasma. The introduction into the interface system of a post-column continuous flow hydride generator (86/C2038 , 87/C198) or on-line cold-vapour generation (86/1645) is an attractive way of removing the problems associated with nebuliser inefficien- cies and can be achieved with comparable ease (see section 4.1).Removing the need for a nebuliser completely is the basis of a novel approach (87/C198) in which the HPLC eluent was collected on a series of platinum wire spirals, which were then introduced directly into the flame of an AAS instrument. In addition to by-passing the nebuliser system the interfacing of HPLC which is essentially a continuous flow technique, to a discrete batch sampling technique such as an electrothermal atomiser adds additional problems to the construction of a high performance liquid chromatograph - electrothermal atomiser - atomic absorption spectroscopic interface. The common approach to this problem has been to combine these techniques with a programmable fraction collector (86/1423, 87/299).However Nisama et al. (86/1751) described a varia- tion in this approach, using carbon cups to collect eluent fractions from the column and then inserting them directly into a modified electrothermal atomiser. This method of interfacing was also capable of a pre-concentration step, achieved by drying the carbon cups prior to their introduction into the atom cell. Despite numerous authors expounding on the problems of nebuliser inefficiencies , the direct connection of an HPLC column to the nebuliser uptake of both AA and AE instruments seems quite adequate for many applications. These include the speciation - separation and determination of S in surfactants (86/C1154), Cr species in water extracts (86/1768) , metallothioneins (86/1847) , As species in cultured cell suspensions (8743) and the separation of transition metals (86/C1574, 86/1579).4.3. Other Techniques for Sample Introduction The numerous devices for both liquid and solid sample introduction have formed the basis of two main reviews (86/1001 , 86/1987) which placed great emphasis on direct solid sample analysis by AE techniques. For solution analysis a system employing a series of computer controlled peristaltic pumps has been shown by the authors (86/C827) to be capable of carrying out routine manual manipulations such as the addition of matrix modifiers, dilution of samples and serial calibrations, In a similar programmable system (86/C1582), designed for the analysis of metallic impurities in refined oils, details of the automatic sampling system controlling both sample preparation and transport to the ICP-AES were given.Handling up to 30 individual samples per hour, the good accuracy and precision obtained with this equipment were reported to be due to: ( i ) the bidirectional communications with the sampling system; (ii) internal clock control and versatile sampling matrix; and (iii) the easy programmability and memory capacity of the system. Automatic wet chemical sample preparation including sample processing and robotic control in both batchwise and continuous flow systems, have been critically evaluated by Knapp (86/C1165). Methodology detailing a closed system for wet chemical decomposition of organic and inorganic materials, and sample pre-concentra- tion were presented, for use with ICP-AES instrumentation.A device known as Plasmasol for automatic treatment of solids by fusion or dissolution at high temperature using glassy carbon crucibles has been used in the analysis of iron ores (86/1005) and various commercially available flux mixtures (87142). Both these papers report the use of ICP-AES detection and stress the improved performance and good agreement achieved with certified values over the traditional manual methods. The growing interest in direct solid sample analysis has resulted in some interesting and novel developments. The probe design of Carroll et al. (87/C187), used in conjunction with a modified electrothermal atomiser, has been described and performance details of recent developments to this sample introduction system discussed.The concept of probe insertion into an ICP torch has interested one group of Canadian workers (86/C1136,87/600) , who have continued the develop- ment of an automatic insertion system based on graphite or metal carrying cups (see section 6.1). The system, capable of handling both liquids (10 pl) and solids (10 mg) has been used for the analysis of various materials including coal, oil, ash and numerous other solid materials. Detection limits as low as 0.1 ng ml-1 Cd were quoted for 10-pl aqueous samples with a 3% RSD value for liquid samples and 7% for powdered samples being reported. In addition to the probe insertion system the same workers presented preliminary results (86/C1136) for a new approach to laser vaporisation for direct sample introduc- tion.The use of lasers for the vaporisation of small amounts of solid materials was discussed by Dittrich (87/C144) (see section 6.3). The use of a fluidised-bed sampling system for the direct introduction of silica powders to an ICP was found to be suitable as a continuous flow system (87/624). In this application changes to hardware design and optimised experimental conditions were given for the determination of Cu, Si and Zn. Using a powder introduction ( 4 0 0 pm diameter) flow-rate of 20 mg min-1 the emission characteris- tics and linear working ranges for the three elements were found to be dependent on the applied r.f. power.In a further development of this methodology chelating materials (87/625) were analysed for elemental composition as a means of achieving sample pre-concentration. The authors of both these papers concluded that the fluidised-bed approach was found to be satisfactory provided particle size was carefully controlled. Gas sampling systems for ICP-AES were considered in a paper by Miller et al. (87/37) who described an interesting approach incorporating a fast-switching valve coupled to a He-driven actuator. A digital valve interface electronically initiated the He actuator pulses and allowed for variations in sampling frequencies. This system has been used for the determination of deuterium, H, N and Nz. The analysis of gaseous components with automatic sample introduction into MIPS have also been reported for N2 (86/1835) and 0 2 studies (86/1837).Both these systems incorporated cold-trap steps prior to sample introduction into the element specific detec- tor. Sample introduction and pre-treatment are the concern of many analysts, and improvements in extraction efficiencies and automation will remain important parameters in analyses. Whilst there is little doubt that direct solid sample analysis will become increasingly important as a technique, the growing areas of computing and robotics will undoubtedly ensure continued interest in automatic sample introduction for atomic spectroscopic instrumentation.JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, JUNE 1987, VOL. 2 5. INSTRUMENTAL CONTROL AND DATA PROCESSING 89R In this section, papers concerned with the growing influence of microcomputers and microelectronics on atomic spectroscopic instrumentation and data processing are reviewed.Total or partial instrumental control, developments in data processing and signal manipulation will be discussed subsequently. 5.1. Instrumental Control The automatic control of instrumentation, other than for sample introduction and background correction, ranges from that of individual components to total system management. The increasing use of computers in the design of atomic spectrometers has stimulated considerable interest in the literature with various authors reviewing the concepts of computer interfacing (86/C1173, 86/C1567,86/2007,87/22). In addition to reviewing the basic philosophy, these papers also outlined the protocols and design considerations relevant to computer controlled instrumentation.In a more practical vein, Tabani and Kratochvil (86/1310) described the design strategy for an IBM-PC controlled atomic absorption system. Computer control of the spectrometer data acquisition and sample introduction facilities, relied on software designed to combine the language of compiled BASIC with the specific application to achieve full operational control. A good example of how an older design AA spectrometer can be updated by the addition of a microcomputer, to realise the capabilities of a modern integrated software instrument, was illustrated in a paper by Grant and Keesee (86/C909). The software written in BASIC (LABSOFT) ran on an Apple I1 microcomputer, interfaced through an ISAAC (Cyborg Corp.) 91A data acquisition device to a Perkin-Elmer 380 AA, HGA-400 furnace and AS-40 autosampler.The software enabled real-time data computation through a machine language sub-routine which performed a fault detection step prior to calibration. During the run, the computer made intelligent decisions on: changes in sensitivity and precision, identified outliers with a Q-test, detected base-line drift, and observed shifts in peak time, indicative of changes in the graphite surface. This system which appears to go further than just realising the capabilities of a modern Perkin-Elmer AA spectrometer (86lC1567) will no doubt be of interest not only to Perkin-Elmer, but to AA users in general. A commercially available sequential ICP has been described which incorpor- ates automated parameter control (86/C817).The modified software not only operates, collects and processes the data, but also offers many new features. These include the optimisation of operating parameters including background correction during the analysis of each analyte, a mathematical smoothing routine to improve precisions and a new real-time internal standardisation technique to compensate for both short- and long-term noise. An alternative approach to that of total automated computer control is described in a second paper (86/C933). Based on microelectronics this system appears to offer most of the facilities of its software driven counterpart and does suggest a move away from interactive software instrumentation.Soltero [Clin. Chem. (Winston- Salem, N . C.), 1985, 31, 10941 described a microprocessor interface which enables automatic operation and calibration of a totally automatic flame photometer to be achieved. The program operating in BASIC, has enabled the system to be used in a full automatic mode for the determination of Ka, Li and Na in serum, urine and plasma samples. The atom cell represents one of the individual components of spectroscopic instruments that has once again been the focus for direct computer controlled interfacing. Temperature control of electrothermal atomisers has been the subject of two papers, describing interfaced power and feedback systems. The first (86/C1531) reported on a new thermo-electrically cooled IR sensor which enabled more accurate temperature control (see section 7), whilst the second by Bass et al.(87/257), described a triac-based circuit which controlled power delivery to the furnace with a precision of 0.4% RSD. The a.c. voltage control was interfaced via a 6522 adaptor to the parallel output port of a microcomputer which used an up-counter routine to vary the amount of power being delivered to the load. The application of this technique to ETA was described fully in this paper. A simple electronic device for automatically regulating gas flow-rates in induc- tively coupled plasmas was outlined in a paper by Borsur and Labarraque (87128). The device coupled to the nebulisation and sheathing gas systems, regulated optimum flow-rates, stabilising plasma conditions.This system analysing 200 samples per day was reported to give a precision of better than 5% RSD for a 34 element programme. This review year has seen developments in the area of instrumental control which appear to be moving towards truly expert systems. The phase of “chips with everything” is now thankfully diminishing and it is refreshing to observe move- ments towards more meaningful computer enhanced control for atomic spectroscopic instrumentation. 5.2. Data Processing The mathematical manipulation of instrumental signals, other than for background correction (see section 3) are considered here. The three distinct areas of optimisation, calibration and data transformation, will for the purpose of this review be examined separately, however, where overlap between these areas occurs due reference will be made.Simplex optimisation has once again been popular with many analysts, and whilst the modified Simplex of Nelder and Mead is still widely used (86/C891, 86/1834, 87/C212), improvements to this technique have been the subject of a series of interesting papers. Comparison of a new super- modified Simplex with both the basic algorithm of Nelder and Mead and the existing super-modified Simplex, has been described by Parker et al. (86/1728). This new version, used for the optimisation of an ICP-AES, was reported to offer significant increases in speed and accuracy when compared with its predecessors. An improvement to the modified Simplex algorithm was also proposed in a paper by Belcham- ber et al. (87427). Operating in BASIC on an Apple I1 microcomputer , the composite-modified Simplex (CMS) was shown to compensate for high matrix acetic acid levels (up to 70%) in ICP-AES analyses for several elements.Adding to, rather than altering the modified Simplex algorithm, in order to improve performance, has been the approach taken by a group of Chinese workers (86/1354). Using a combined partial factorial design - modified Simplex optimisation procedure the authors, operating an Ar - H2 plasma, reported improved detection limits for Br, Cd, Cr, Fe, Ni and V for the optimal, multi-element compromise conditions of Ca. Utilising features of both Simplex optimisation and multi- linear regression fit, Smith et al. (86/C838) outlined the advantages of an alternative surface response algorithm Optiplex.The authors claim that the ability of Optiplex to retain all the data from every experiment, unlike Simplex which discards the poorest response, represents the most significant advantage of the technique as Optiplex remains global in its data base and therefore suffers less risk of finding a false optimum. Optiplex does however require 2N + 1 experiments for the initial set of vertices, unlike Simplex which only requires N + 1. Thus for a large number of parameters (N) Optiplex may require a considerable degree of experimental work. The authors demonstrated however that once the initial Optiplex has been established optimum conditions are achieved quicker than with Simplex. The speed90R JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, JUNE 1987, VOL.2 argument with these two techniques does seem a little like “swings and roundabouts” and perhaps of more relevance to the analyst is, which algorithm achieves an unambiguous optimum and can identify the significant parameters. Despite avoiding these points the authors do give specific AA and AE examples of Optiplex optimisation (86/C838). In two papers the Fletcher - Powell directed search or “hill climbing” algorithm was used for the optimisation of ICP operating conditions (86/C1176, 87/C548). This exhaustive search method, through graphic displays, allows the analyst to visualise which element or groups of elements are susceptible to specific parameter changes, at each step towards the optimum. Such an approach enables each element or group of elements to be determined under optimum conditions within a multi-element analysis.Examples are given of how this automated optimisation procedure can reduce the time and skill required in method development. In practical terms an automated optimisation of the ICP parameters r.f. power, nebuliser argon flow and viewing height can be performed at one analytical wavelength in about 10 min. No indication is given of the total analytical time one might expect for, for example, the determination of a mixture containing ten analytes, however the technique described represents a most interesting and advanced optimisation procedure. 5.3. Calibration Calibration procedures, have, over recent years, moved away from the traditional manual methods of the “eye” and towards microcomputers, running at times some very sophisticated software.The importance of an appropriate calibration procedure enabling accurate results to be obtained, has been the theme of two reviews on the general concept of calibration in atomic spectroscopy (86/1008,87/C184). It is now common- place to find modern instrumentation incorporating a micro- computer to carry out the calibration process, and such systems have been generally based on the least-squares fitting algorithms. A more recent development by manufacturers has been to adapt different mathematical functions for their “on-board” computers in order to smooth and improve calibration routines, however this approach can lead to far from perfect curve fitting (87/C541). Bysouth and Tyson (86/1654, 86/1889) examined a number of these commercially available curve fitting algorithms, comparing them with each other and with both linear interpolations and manual graph- ical plots.This evaluation of calibration methods carried out for FAAS, concluded that, in general, the algorithms selected produced curve fitting errors well below 5%, the exceptions being the simple parabola, linear interpolation and manual methods. For the commercial systems tested the authors did stress that goodness of fit is dependent on the degree of curvature and number of data points. These concluding remarks suggest that the user should at least look at the calibration curve produced by the computer. Examining more closely the accuracy of calibration procedures, Ripley and Thompson (87/C139) described a new weighted regression method for estimating the bias or systematic error in sample measurements.This approach enabled compensations to be made for variations in analyte concentration and the matrix effects of the individual samples. The principles and analytical significance of the standard additions method, in calibration procedures, has formed the subject of a detailed review (87/368). In an attempt to overcome the limitations associated with linear extrapolation, the main criticism of this technique, Liu and Li (87/5) described a method of non-linear standard additions. The paper outlined how three equations were selected as a mathematical computer based model that can determine a non-linear extrapolation. From experimental data obtained by FAAS for various elements, the authors reported that both the percentage error and the coefficient of variance of this method were less than 5%.Extending the calibration concentration range beyond the normal linear working curves obtained in AAS, has once again been an area of interest. One such approach (87/389) measured peak widths, rather than the more commonly measured peak height or peak area, through the interfacing of a FI-AA spectrometer system to a microcomputer. Using this configuration the operating software can extend the calibra- tion range over typically three orders of magnitude, for elements such as Cr, Mg and Ni. O’Haver and Kindervater (86/C1568, 86/1820) developing on earlier work in this area, described a computer model which evaluated all of the following parameters, the inherent shape and width of spectral lines, the background intensity (lo), instrumental broadening due to finite resolution and stray light.The computed value from this model produces the “intrinsic absorbance,” that is, the absorbance at the line centre, free from instrumental broadening and stray light. The intrinsic absorbance when plotted against solution concentration gave a linear calibration over at least five orders of magnitude. Two studies in the area of AE have concentrated on novel approaches to calibration. A computer program written in MICROSOFT 6800 BASIC has been developed (861C874) for use in spectrographic (photographic emulsion) quantitative calcu- lations. Using a two-step calibrated neutral density filter, a preliminary curve was constructed from which the gamma curve can be derived.The percentage transmission values were then converted to Seidel values and using linear regression, a straight line calibration was achieved. Calibra- tion with the gamma curve required a second degree quadratic fit algorithm for quantitative measurements. The program was designed €or a methodology using an internal standard which permitted background correction to be achieved with this technique. Blades et al. (86/C942,86/1384,86/1471) continued investigations of the multivariate space calibration procedure. Using a 1024-element photodiode array, data collected from an ICP-AES was compressed to 38 points with an effective low spectral resolution of 0.4 nm. Qualitative analysis was accomplished using pattern recognition and factor analysis, with quantitative analysis being achieved through the con- struction of multidimensional working curves in hyperspace.The hyperspace co-ordinate system was transformed to give an axis corresponding directly to elemental concentrations, allowing direct simultaneous calibration and determinations of elemental composition. These papers reported full details of the technique and gave practical examples, which include effects on line intensities, detector dynamic range and matrix effects. This approach to ICP-AES calibration, which appears at present to be limited to the authors laboratory, makes interesting reading. 5.4. Data Acquisition and Manipulation Data management in the developing field of computerisation represents a significant growth area in both data acquisition and manipulation techniques.In the literature one can regularly observe reports of new and sophisticated computer programs enabling enhancements in all aspects of atomic spectroscopy. However, in a rather sobering paper Katzen- berger (86/C1187), examined the role of the computer in instrumental applications and identified the enormous finan- cial and practical problems in software development. The author outlined the many pitfalls of this aspect of instrumental design and recommended that a well established operating system with a large software data base should be used where possible. Additionally, in an attempt to achieve cost effective- ness, software development can be minimised by transferring more resources to the design of hardware.A practical example of how this can be achieved was demonstrated by a new program written for the instrumental control of a sequentialJOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, JUNE 1987, VOL. 2 91R ICP-AES system. Particular attention was focused on the tools used to increase programmer productivity and in making the software more robust. Modifications improving the existing data handling facilities of commercial instruments by adding furtherprocessingpower to the instrumental system has been reported by various authors. Of the systems described, a Digital Equipment PDP-11, minicomputer running under the real-time operating system RSX-IIM appears to be a very popular machine for this type of interfacing. For example, Parlow et al.(87/422) described how two Perkin-Elmer 5000 AA instruments equipped with furnaces can be coupled to the PDP-11 minicomputer through the serial CAMAC I/O port. This configuration enables simultaneous independent processing of transient atomisation signals from both spectrometers. In addition io data acquisition routines the software contains sub-programs for graphic representation and detailed evalua- tion of signals. Based on the same computer, independent authors described similar software developments for both AA (86/C1517) and AE (87/467) equipment. The refinement of data handling in terms of both speed and signal treatment, will of course continue to be reported by manufacturers updating processing facilities. Shrader et al. (86K1572) described the latest developments in AA systems whilst Dungs et al.(86/1818) outlined new software packages available for a data station. The power for data transfer available through computerised data acquisition is most relevant in the area of multi-element emission techniques. The recent introduction of ICP-MS instrumentation has stimulated a number of reports on data handling facilities specific to this type of equipment. Peak- jumping routines for rapid data acquisition in ICP-MS have been the subject of two conference papers (86/C1179, 861C1485). A comparison of peak hopping and multi-channel scaling modes of data acquisition for isotope ratio determina- tions by ICP-MS (86/C1485), identified that peak hopping was in fact not only a quicker technique but gave a better measure of precision when limited by counting statistics.The optimised peak hopping technique was reported to give a typical precision for isotope ratio determinations in the order of 0.1% RSD for elemental concentrations of 1 p,g ml-1 or more. In this paper, which gave full experimental details, the statistical evaluation of Ag and Sr quoted precisions in this instance of 0.06 and 0.08% RSDs, respectively. An equivalent system was described by Hutton et al. (86/C1179). Instrumen- tal details were outlined of this fast data acquisition procedure together with a brief consideration of sample introduction techniques. Data for silver isotope analysis was given with a precision of t 0.2% RSD quoted for these determinations. Moving away from the subject of data acquisition, various workers have been concerned more with the manipulation of data in order to increase the amount of information obtainable from spectroscopic events.Horlick and co-workers in a series of papers (86/978, 86/981, 86/1272), described a simple cross-correlation technique for processing interferograms generated by a UV - visible Fourier transform spectrometer (mS) coupled to an ICP-AES. The Michelson interferometer used laser fringe referencing to sequence the digitisation and interferograms were processed on a PDP-11 microcomputer interfaced with a 6502 based microprocessor controlled system which, had at its heart a multiplier - accumulator chip. The interferograms which resulted from the emission of samples in the ICP, could be automatically interrogated for the presence or absence of up to 70 elements, and automatic qualitative analysis was possible.Other facilities available included identification of spectral interferences and complete measure- ment of spectral background. Application of the cross-correla- tion method achieved basically by “software slew scanning’’ provided the user with a unique technique to study and select the spectral information about an analyte. It is of course not practical to obtain such information with the current direct reading and slew-scanning dispersion spectrometers. This system, described in detail in the references, has been used for studies on Cu, Pb, Sn and Zn. The power of computers in data manipulation is perhaps most evident when used for model or simulation experiments. Work by Blades and Burton (86/C1177, 86/C1515), on computer simulation of ICP spectra opens up the possibility of providing general purpose, software based, spectral line tables which can be tailored to a particular ICP instrument.The program, used to study the ICP analyte emission spectra, inputs data from tabulated wavelengths, transition probabili- ties (gA values), excitation and ionisation temperatures, Doppler and Stark broadening line widths, excitation ener- gies, spectrometer slit function, dispersion and optical transfer functions. The object of combining this enormous amount of data represents an attempt to compensate for the relative elemental emission intensities dependent on individual physical properties, such as temperature and electron density in the plasma, which are not currently allowed for in spectral line tables.The authors claim that such a program will offer a substantial improvement in alerting users to potential spectral interferences. The final paper in this section reports a rather unorthodox use of computerised pattern recognition techniques. Burns et al. (86/717) described how the ICP-AES determinations of the elemental composition of boll weevils can be processed by a pattern recognition routine to monitor migratory trends of this organism. This final example of the use of computers will perhaps remind us how instrumental automation and data manipulation have disseminated into all aspects of analytical atomic spectroscopy. 6. COMPLETE INSTRUMENTS 6.1. Emission The advent of plasma spectrometry, in all its various forms, has undoubtedly had a profound effect on the way in which elemental analysis is now carried out.In some respects, the technology can now be considered mature, as evidenced by an increasing number of reviews devoted to plasma instrumenta- tion (86/1305, 86/1697, 86/1861, 87/518). The major article by Keliher and co-workers is an invaluable reference source, covering developments in emission spectrometry over the last two years (8611961). The introduction of “second generation” ICP spectrometer systems which are computer controlled, highly automated and much more compact has resulted in the widespread acceptance of the technique within the analytical community (86/1438). There have been attempts in the past year to place these developments within the framework of historical perspective in order to identify the most likely directions for future research work (86/C896, 86/C1122, 86/C2034).Ebdon et al. (86/1962), in an authoritative review, addressed the versatility of the ICP in the fields of emission, fluorescence and mass spectrometry. This article also pro- vided a particularly useful state of the art discussion of sample introduction and the application of the ICP as a chromato- graphic detector. de Galan (87/23, 87/1351) in critically reviewing progress in optical spectrometry, identified a92R JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, JUNE 1987, VOL. 2 number of weak points in ICP-AES which must be remedied if the technique is to be developed further to meet future analytical challenges.The evolution of instrumentation able to cope with the limitations imposed by spectral interferences, and the requirement for improved sample introduction systems for the ICP, were amongst the topics considered. The selection of inductively coupled plasma equipment for an analytical laboratory is a matter of some complexity, given the wide range of commercial instruments now available. One way of tackling this problem is to establish criteria for evaluating instruments (86/727). In this clear and concise introduction to the technique, the concepts of detection limits background equivalent concentrations, precision, stray light and spectral resolution were discussed in relation to establish- ing the performance characteristics of ICP-AES equipment. A critical survey has been made of commercially available ICP, MIP and DCP equipment in conjunction with sequential and simultaneous emission spectrometers, and in fluorescence and mass spectrometric detection (86/1842).Guidance in respect of likely future trends in instrumefitation and selection of the most suitable instrument for a given application was also provided. The third report of the Instrumental Criteria Sub-committee of the Analytical Methods Committee which considered the evaluation of polychromators for use in emission spectrometry with ICP sources has now been published (86/1980). The guide is reproduced as Table 1. The notes on scoring to facilitate comparison are the same as for the first two reports on atomic absorption instruments (see ARAAS, 1984, 14, 67).In a series of important papers, Boumans and Vrakking (86/C1164, 86/1864, 86/1865) have continued to investigate analytical performance figures of merit in ICP-AES, using an kchelle spectrometer operated under “high” (4-5 pm) and “medium” (1 1-16 pm) resolution conditions. The differences in reported detection limits for different experimental set-ups were discussed in terms of source parameters, spectral resolution and the noise characteristics of each system. It was found that both the spectral band width and the physical line width influence the resolving power of the spectrometer, and this effect can be accounted for by ratioing the measured values of the effective line widths. The ratio of SBRs were reported to vary inversely with the ratio of the effective line widths of the spectrometer.A comparison was made of detection limits published in the literature for a 27.12-MHz ICP using a medium resolution spectrometer and those obtained by the authors (86/1864) using a 50-MHz ICP and a 1.5-m echelle spectrometer with pre-disperser, for approxi- mately 100 prominent ICP lines between 280 and 325 nm. These values were broken down in terms of the ratio of SBRs in the sources, the modification of these ratios by the spectrometers and the ratios of the background RSDs. It was concluded that this procedure provided a rational explanation for differences observed in reported detection limits using different optical systems. The instrument was used to investi- gate the potential spectral interferences by hydroxyl bands on prominent lines emitted by the ICP (86/1864).The criterion used for assessing the degree of interference was the ratio of the limit of determination, CD, and the limit of detection CL (see also JAAS, 1986, 1, 65R). Twenty-five lines were found to experience significant interferences ( CD/CL > 10) out of more than 100 lines examined. It was considered that in the case of line overlap, the limit of determination should be preferred as the criterion for optimisation of ICP parameters (86/C1164, 86/1864). The general philosophy of how to approach the problem of spectral interferences using available instrumentation was the subject of a major review by Boumans (871588). Aspects of data handling and the concept of selectivity were discussed. The choice between simultaneous and sequential spec- trometers for ICP-AES often depends on the relative impor- tance of analytical speed and flexibility.Using a poly- chromator based system, restrictions in wavelength selection and the necessity of employing compromise plasma conditions can lead to losses in sensitivity in the measurement of some elements. A system has been described in which a 15-channel polychromator (wavelength range 200-500 nm), a two-chan- nel polychromator (wavelength range 500-800 nm) utilising glass-fibre collection optics and a UV optimised N2 purged monochromator (wavelength range 170-400 nm) with two automatically interchangeable photomultipliers were used as combined detectors for a 3.5-kW ICP (86/C1201). Internal standardisation was used to compensate for short- and long-term fluctuations and a precision of 0.5% average was reported.The separate two-channel polychromator was opti- mised with respect to viewing height for the determination of Na and K, and detection limits between 10 and 50 pg 1-1 were quoted. The UV monochromator was applied to trace analysis, and in the determination of P and S. It was claimed that a ten-fold improvement in detection limits was obtained. The instrument system was used for elemental analysis of environmental samples in respect of the operation of coal- fired power stations. In a similar approach, two direct reading spectrometers were used to view a single ICP source, providing a total of 124 signal channels (86/C988). The system could operate in “parallel” or “slave” modes and was designed for automated, unattended operation.Applications to the analyses of soils, steels and alloys were discussed. A combined sequential - simultaneous ICP spectrometer system was described in which the same optical path was used for both types of measurement, i.e., the sequential spec- trometer was installed inside the simultaneous spectrometer (86/C932). Thus the sequential spectrometer offered a direct peaking facility, and focused on the Rowland circle of the simultaneous spectrometer. The analytical features of the instrument and its software implementation were also dis- cussed. In a different approach to multi-element analysis, the design of a time division multiplexed spectrometer using a single photomultiplier as detector was described (86/C805).The instrument provided a high degree of wavelength accuracy, random access to the UV - visible spectrum and a rapid analysis capability. Detection limits in the parts per billion range for Ca, Li, Na and Sr using an air-acetylene flame as the excitation source were reported. Several papers described the advantages of spectrometers incorporating photodiode arrays for multi-element emission spectrometry. The operation and performance characteristics of an automatic arc spectrometer, fitted with a linear charge coupled photodiode array detector were described (86/1701). The instrument was applied to qualitative and semi-quantita- tive analysis of alloys and metals. The combined recording and data processing time was <5 min and errors were reported to be within 10%.The enhancement of wavelength accuracy using a linear photodiode array as a detector in ICP-AES has also been the subject of investigation (86/970). One of the advantages of the use of a photodiode array is that it allows the simultaneous measurement of analyte line and background intensities. This feature was demonstrated in ICP-AES using the SPS-10 spectrometer which incorporated a 1024-channel self-scanning linear photodiode array camera as the detector (86/C561, 86/C876, 86/C1170). The optical design consisted of a low- resolution polychromator and used a masked Rowland circle to identify analytical regions of interest for a band pass of 1 nm in the wavelength range 185415 nm. The dispersed radiation was recombined using a second grating and collimated on to an echelle grating.The resultant high dispersion spectrum was focused on to the array detector. It was reported that the system could be used to analyse 10-20 elements simultaneously employing the masking technique, and the potential for the measurement of transient signals was also indicated.JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, JUNE 1987, VOL. 2 93R Table 1. EVALUATION OF ANALYTICAL INSTRUMENTATION. PART 111. POLYCHROMATORS FOR USE IN EMISSION SPECTROMETRY WITH ICP SOURCES* Notes on the Use of this Document Column 1. The feature of interest. Column 2. What the feature is, and how it can be evaluated. Column 3. The Sub-committee has indicated the relative importance of each feature and expects users to decide on a weighting factor according to their own needs.Column 4. Here the Sub-committee has given reasons for its opinion as to the importance of each feature. Column 5 onwards. It is suggested that scores are given for each feature of each instrument and that these scores are modified by weighting factor and sub-totals obtained. The addition of the sub-totals will give the final score for each instrument. Notes on scoring 1. (PS) Proportional scoring. It will be assumed, unless otherwise stated, that the scoring of features will be by proportion, e.g., Worst10 to Bestl100. 2. (WF) Weighting factor. This will depend on individual require- ments. An indication of the Sub-Committee’s opinion of the relative importance of each feature will be indicated by the abbreviations VI (very important), I (important) and NVI (not very important).A scale is chosen for the weighting factor which allows the user to discriminate according to needs, e.g., x l to x3, or x l to x10. The factor could amount to total exclusion of the instrument. 3. (ST) Sub-total. This is obtained by multiplying PS by WF. INSTRUMENTAL CRITERIA SUB-COMMITTEE INSTRUMENT EVALUATION FORM Type of Instrument: Polychromator for Use in Emission Spectrometry with ICP Source. Manufacturer: Model No: Score Definition andlor test procedures and guidance for assessment Feature Importance Reason ~~ ~ 1. Resolving power in the wavelength region of interest ~ _ _ _ _ _ ~ Maximum score for highest values of AtAA. AA is the smallest difference between two wavelengths that can be distinguished as two spectral lines (normally separation at half height), Maximum score for the highest value of AxIAA.Ax is the distance between two spectral lines differing in wavelength by AL VI In emission spectroscopy it is essential to be able to measure a line of interest in a complex spectrum. PS WF ST PS WF ST I 2. Linear dispersion The linear dispersion will govern the number and proximity of exit slit/detector assemblies which can be mounted in the focal plane. 3. Wavelength range ( a ) The instrument must cover the spectral range which encompasses the lines of interest to the user. (b) Score additionally for an extended range. VI NVI Whilst it is obviously necessary for the user to be able to select the principal lines of interest, it is advantageous to be able to select other lines of occasional interest.PS WF ST PS WF ST 4. Number of channels Maximum score for the highest number that can be supplied by the manufacturer as standard. The greater the number of channels the greater the versatility of the spectrometer, enabling the measurement of the widest range of lines. This permits measurements at both atom and ion lines and the selection of other suitable lines to minimise interferences. I 5 . Ease of changing channellline corn binations Score maximum for the easiest and most economical method of changing channel/line combinations. I It is convenient to be able quickly and economically to change the suite of lines to meet changing requirements. PS WF ST * Taken from a Report of the Analytical Methods Committee, Analytical Proceedings, 1986, 23, 109 (Analytical Methods Committee, Analytical Division, Royal Society of Chemistry, Burlington House, Piccadilly, London W1V OBN, UK).94R JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, JUNE 1987, VOL.2 mportance Table 1. EVALUATION OF ANALYTICAL INSTRUMENTATION-continued Feature 6. Number of lines available for use 7. Effect of varying light levels 8. Stray light 9. Light gathering power Definition and/or test procedures and guidance for assessment Maximum score for the highest number of relevant lines available on the instrument. Using a suitable source, e.g., a hollow-cathode lamp run at high current or an electrodeless discharge lamp, measure the signal resulting from this high intensity source. Insert a flag filter to reduce the intensity by a factor of 10000 and repeat the measurement.This experiment should be repeated rapidly 20 times and the standard deviation and mean at each level calculated. Various sources should be used to cover the wavelength range of interest. There should be no statistically significant difference between the initial and final reading. [Analysis of co-variance (ANOCOV) table.] Score accordingly. A He - Ne laser should be used. The signal at 632.8 nm should be substantial, so that a large amount of light enters the spectrometer. Measurements of this signal at minimum gain should be obtained, together with measurements at 631.8 and 633.8 nm made at high gain. Score maximum for the minimum ratio of readings at the other wavelengths to those obtained at 632.8 nm. Other channels, particularly at short wavelengths, should be interrogated using high gain.This is the minimum amount of energy that can be detected at a suitable selection of wavelengths covering the instrument's range. Use a calibrated tungsten lamp at the normal source position of the spectrometer, focused by the spectrometer lens on the slit. An iris diaphragm, suitably positioned, will determine the useful solid angle, S, subtended by the source. If the area of the slit is A and the magnification I VI VI I Reason 'he least desirable feature of mission spectroscopy is pectral interference. The reater the number of lines to hoose from, the greater the hance of avoiding such iterference. n routine use the lhotomultiplier tubes of the lolychromator will be ubjected to rapidly changing .ght levels and this must not ffect the response of the PMT o a given level if quantitative neasurements are to be eliable.4s well as light loss, stray ight produces unwanted and rariable background readings. The light gathering power of he polychromator will affect he sensitivity of the nstrument (see Appendix). - ;core PS WF ST PS WF ST PS WF ST PS WF STJOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, JUNE 1987, VOL. 2 Table 1. EVALUATION OF ANALYTICAL INSTRUMENTATION-continued Feature 10. Short-term stability 11. Long-term stabiliq 12. Temperature stability Definition and/or test procedures and guidance for assessment af this image, M , the energy passing into the spectrometer is BAS AA A4 where B is the spectral radiance af the source (watts steradian-1 cm-2) and A1 the spectral band width.The diaphragm should be closed until a very small net signal is obtained, the result being expressed as counts W-1. Score maximum €or the highest value for this €unction. Using a stabilised light source, such as a hollow-cathode lamp or low pressure mercury lamp, produce a series of readings at one per minute for 30 min. This should be repeated using suitable attenuation to cover the dynamic range of the instrument. The system should be allowed to stabilise between each set of measurements. Score maximum for the lowest standard deviations. Drift should be essentially absent over the period of the measurements. Using conditions similar to those for the middle of the dynamic range used in test 10, produce a set of readings at a rate of two per hour for 24 h, or if this is impracticable, over 2 consecutive working days.Score maximum for lowest standard deviation and minimum drift. Maximum score for the widest range of ambient temperatures 3ver which the stabilities as jetermined above can be Zuaranteed by the supplier/ nanufacturer . ~~ mportance VI VI VI Reason If the polychromator is not stable, within acceptable limits: €or short periods it will not be possible to obtain useful quantitative results. If the instrument is to be used in conjunction with an automation sample changer, long-term stability is essential. Long-term use of stored calibration functions also calls for long-term stability. The shorter the temperature range over which the kstrument will function at full :fficiency, the more complex md expensive will be the .equired laboratory emperature control system.Score - PS WF ST PS WF ST 95R96R JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, JUNE 1987, VOL. 2 Table 1. EVALUATION OF ANALYTICAL INSTRUMENTATION-continued Feature 13. Slit geometry and selection 14. Grating 15. Focal length 16. Computer compatibility ( a ) Sophistication ( b ) output (i) High-quality graphics (ii) High-speed printer (iii) Report for- matting ( i v ) Plotter Definition and/or test procedures and guidance for assessment Jertical rather than horizontal lits are more compatible with he plasma source geometry. h v e d slits are claimed to be referable to straight slits. 'reference should be given to nstruments with a selection of mtrance and exit slits.~~~ The properties that are affected )y such considerations as ruled )r holographic gratings, blaze ingle, etc., are light gathering lower and stray light, and hese have been dealt with inder the appropriate ieadings. The properties that are most iffected by focal length, such as lispersion, stability, and light gathering power, have been dealt with under the ippropriate headings. Score maximum for the greatest extent to which the instrument is under computer Zontrol. Further score for ease and provision of high level language programme access. Score according to availability of each of these accessories and their degree of sophistication. nportance I I Will vary with user circum- stances Reason The region of maximum signal o background in a plasma )ource is a small vertical region vhich is readily matched by rertical slits, minimising critical idjustment of the source.The mage of the entrance slits at It the Rowland circle is curved md theoretically light losses ire minimised by compensating 'or this by using curved slits. 9 choice of slit widths ind heights is beneficial in ,electing conditions to naximise signal to noise and )ackground ratios and ninimise interferences. This :hoice may be made by the nanufacturers. ~~ A compact, easily operable system, which has speed and high capacity, greatly assists the operator to obtain accurate results quickly; it also facilitates such items as inter-element corrections, background corrections and calibrations. (i) Method development is often facilitated by visualisation of spectral profiles.provision of hard copy. conjunction with management systems. graphics output for investigation of interferences and for systems and methods evaluation. (ii) Quality Control requires (iii) Very useful in ( i v ) Complements - 'core - PS WF ST PS WF ST - PS WF ST PS WF ST -JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, JUNE 1987, VOL. 2 Table 1. EVALUATION OF ANALYTICAL INSTRUMENTATION-continued Feature 17. Background correction (inter-element) correction) 18. Qualitative information 19. Dynamic range and mode of integration 20. Speed of analysis Definition and/or test procedures and guidance for assessment Background correction is the compensation for extraneous radiation in the intensity of spectral lines, such as continuum overlap and stray light.Score maximum for systems which employ moveable entrance slits or refractor plates in addition to fixed slit routines. Identification of elements other than those for which there are channels on the polychromator. Score maximum for systems having an in-built scanning monochromator or equivalent device. Maximum score should be given for digital integration, however, in the absence of such a system score highly for capacitative integration using high-quality polystyrene feed-back capacitors. “Cascade” methods of capacitative integration are not recommended. This is mainly determined by the “washout” time of the nebuliserhpray chamber employed. This can be evaluated by measuring the time for the signal for 1000 p.p.m. of manganese, or other suitable element, to decay to a level at which it has no statistically significant effect upon the precision or accuracy of the measurement of a 1 p.p.m.solution. This mportancc VI I VI I Reason It is possible to store blank intensities in the computer for each channel and to subtract these from the sample intensities. Although this procedure is rapid and easy to use, illconditioning can occur, resulting in error when a general elevation of background occurs. Therefore, it is more accurate to use off- peak methods. This latter method is slower but more reliable than the former. The ability to analyse elements (spectral lines) not programmed in the polychromator is desirable. The provision of an n + 1 channel permits an intensity read-out from regions of the spectrum not covered by the fixed channels. Automatic scanning over user-selected spectral regions for qualitative analysis can be undertaken.For the stable signal produced by the ICP, digital integration following A-D conversion is the most accurate method. However, for multi-channel instruments this approach is not currently used because of the excessive cost of the integrating A-D convertors. It is thought that current methods of signal detection and integration will always have a linear dynamic range, which will exceed the requirements imposed by the nature of the ICP source (which, in practice, does not exceed 5 orders of magnitude). Instruments for routine use may require a high sample throughput for economic reasons. It is important that any such required rate can be met by the instruments under consideration. - score PS WF ST - PS WF ST PS WF ST - PS WF ST 97R98R JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, JUNE 1987, VOL.2 Table 1. EVALUATION OF ANALYTICAL INSTRUMENTATION-continued Feature 21. Over-all performance 22. Amenities (a) BencWfloor space/weight (floor loading) ( b ) Services ( i ) Environmental control (ii) Electrical (c) Servicing and spares (4 Applications support (e) Availability of major accessories and updates (f) Training facilities and documentation 23. Value for money Points perf Definition and/or test procedures and guidance for assessment 3arameter must be used with :aution as the use of a different iebuliser/spray chamber may ;ignificantly change the messment . [t is appreciated that most users will only perform part Df the exercise due to limitations of time Self-explanatory, Score maximum for minimum requirements for environmental control (room temperature and humidity) necessary to enable the instrument to operate within its specification.Score maximum for compatibility with existing electrical supply, both with regard to loading and stability. Enquire in detail as to local arrangements and score accordingly. Enquire as to availability of applications support in field(s) of interest and score accordingly. Enquire about manufacturers’ policy on updating software and compatibility of present and future accessories, score accordingly. Enquire as to local arrangements for operator training and available documentation and score accordingly. Sum of the previous sub-totals divided by the purchase price of the instrument.Subject to proportional scoring and weighting factor as for previous features. Include ST in grand total. :mportance VI Varies with users circum- stances . VI Varies with users circum- stances. VI I I I I Reason Evaluation of the over-all system is essential to ensure that performance of individual components is not degraded when they are intergrated into a complete system. The instrument must be laboratory compatible or else expensive alterations will be required. Additional installation costs may be considerable, if close control of environmental factors is required. Additional power requirements may significantly increase installation costs. Cost of spares, servicing and downtime may severely alter over-all running costs.Time and facilities for method development may add significant costs, especially if training facilities are scant. Future analytical requirements. Availability of efficient programme and good documentation can greatly reduce commissioning time for a new instrument. Simple instruments are often good value for money, whereas those with many refinements are often costly. Score PS WF ST PS WF ST PS WF ST PS WF ST PS WF ST PS WF ST PS WF ST PS WF ST him of totals sub- PS WF ST %and total -JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, JUNE 1987, VOL. 2 99R Perhaps the most significant feature of research work reported during the year under review has been the sustained emergence of inductively coupled plasma Fourier transform spectrometry (FTS). The number of papers in this area is undoubtedly increasing and the introduction of commercial instruments should see further exploitation of this new technique.Traditionally, Fourier transform spectrometers have found application in the IR region of the spectrum, and this feature has been used to good effect in the determination of C, H, N, 0, F, C1, Br, I and S in GC - MIP studies (86/C1242, 860988). The problems of extending the range of FTS into the UV region where the most favourable atomic emission lines are found, have largely been those of meeting extremely demanding optical and mechanical tolerances. A new FTS system (86/C1190) specifically designed to cover this wavelength region has been designed with arms at 10" rather than the conventional 90" and with catseye retroreflectors replacing the plane mirrors.One catseye was scanned over the range k 10 cm from zero path difference, to produce an interferogram which was detected by a solar blind PMT. The tilt invariance of the retroreflector was reported to ease the requirements of the guidance system for the scan. The interferogram was sampled at equal spatial intervals, as determined by sub-divisions of the fringes from a laser and these single points were used as data for the Fourier transform, The theoretical resolution of the system of 1.5 X 10-4 nm at 230 nm was reported to have been achieved in practice. The high resolution offered by the instrument was found to be valuable in the examination of line rich spectra. The characteristics of ICP-FTS have been discussed by Faires (86/1239,87/C151) and reviewed by Miyazaki (87/510). Although the technique provides advantages over conven- tional ICP-AES in terms of resolution, and simultaneous measurement over the entire wavelength range, a number of problems remain to be solved.The foremost of these is a multiplex disadvantage which results from source noise distribution throughout the spectrum in the F'T process (86/1792). Detection limits may be degraded as a consequence of noise from strong emission lines of a matrix. Examples were quoted for the determination of Ni, in which the presence of 1000 p.p.m. of calcium degraded the detection limit by a factor of 122 compared with a factor of five for a similar concentra- tion of aluminium as a matrix element. Methods such as optical filtering, limiting the band pass, using post FTS dispersion and multiple detectors, or employing low noise torches and nebulisers were suggested in order to overcome these difficulties.Stubley and Horlick (86/978, 86/979) have described an FTS-ICP system which covered a wavelength range of 193-650 nm. Detection limits were found to be at least ten times poorer than those obtained with a commercial direct reading instrument. This performance was attributed to dynamic range limitations and multiplex disadvantage. This has led to investigation of the signal to noise ratio characteris- tics of FTS systems. The distribution of noise across a spectrum and its variation as a function of analyte and matrix was evaluated for hollow-cathode lamps and the ICP (861 C802, 86/C1240).It was concluded that the noise was not distributed evenly across the spectrum but was associated with and was greater near to spectral peaks appearing as side bands. Furthermore, the presence of strong emission lines gave rise to increased base-line noise, and it was predicted that detection limits would be matrix dependent using this type of detection system. In an attempt to overcome these difficulties, a windowed FT spectrometer was designed in which a slow scanning monochromator operating with a 4-nm band pass was coupled to the Michelson interferometer (86/980). It was shown that this system reduced the dynamic range and SNR limitations of F'TS. Detection limits were reported which were largely comparable with those obtained using a commercially available ICP instrument.An alternative configuration, in which the interference fringes from the interferometer could be focused on to the exit slit of a direct reader was described. This would provide a narrow band interferogram at each detector. The application of a Bomen DA3 Fourier transform spectrometer to ICP-AES in the UV region was described (86/C1510). The incorporation of an aluminium coated quartz beam splitter was claimed to offer improvements in efficiency in the UV region of the spectrum. Electro-optical circuitry provided real time dynamic alignment of the interferometer with acceptable tolerances at UV wavelengths. Analytical applications of the system included analysis of an aluminium based alloy. Developments in source design are reported in detail in the ASU review on Atomisation and Excitation (see JAAS, 1986, 1, 122R).However, the main advances in respect of instrumentation are summarised here. The weakest aspect of plasma instrumentation is undoubtedly sample introduction. Although there is still considerable research effort devoted to the development (86/C889,86/C1123,86/C1529,86/1627) and comparison (86/C888, 86/2015) of pneumatic nebuliser based systems. These are obvious limitations imposed by the relatively poor efficiency of these devices. It is interesting to note the renewed interest in the use of ultrasonic nebulisers in this respect (86/C1126, 86/C1527, 87/C552). However there are now a large number of papers appearing concerning the use of alternative sample introduction techniques.In a significant review article, Matusiewicz (87/416) discussed the historical development of thermal vaporisation as a means of sample introduction in ICP-AES. All the main variants, such as direct sample insertion, electrothermal vaporisation, r. f . arc, high voltage spark, and laser ablation were considered. In a wide ranging comparison of literature detection limits between thermal vaporisation methods and conventional ICP- AES, it was concluded that improvements of between one and two orders of magnitude could be obtained by adopting the former technique. However, this sensitivity advantage is not retained in comparison with ETA-AAS. As the conventional ICP produces a steady-state signal, the response time require- ments of the spectrometer are not particularly demanding.In the measurement of rapid pulses such as derived from electrothermal vaporisation , design modifications are neces- sary to achieve optimum performance, in order to maintain multi-element capability (86/C895, 86/C1134, 86/C1490). In this system, a rotating refractor plate was used in conjunction with a direct reading spectrometer, to correct for spectral background interference. Two signal integrators were employed, one to estimate spectral line intensities at a rate of 20 measurements per second. Time gating of the data collection system in ETV-ICP has been utilised to discriminate against interference in simultaneous multi-element analysis (86/1274,86/1779). A signal versus time profile was generated for each polychromator channel in order to time resolve analyte and interferent responses.A hardware - software system specifically designed for transient signal measurement has been described (86/C865). The application to ETV-ICP in the analysis of semi-conductor materials was discussed. There have been a number of reports illustrating the use of commercially available AAS electrothermal atomisers in conjunction with DCP (86/1918), MIP (87/120) and ICP (86/C14907 86/C1578, 87/552) sources. However, the tech- nique is likely to benefit most by the adoption of a vaporiser designed to meet the requirements of AES measurement. There are some indications that this is beginning to occur commercially, and this should allow a more widespread evaluation in routine analytical situations. One of the main alternative methods to nebulisation now advocated is a technique in which the sample is directly inserted into the plasma on a support.Salin and co-workers (86/C930, 86K931, 86/C1138) have described a pneumatically driven direct sample insertion device (DSID) for ICP-AES. The system employed both graphite electrodes and wire loop sample supports. Detection limits were reported to be in the p.p.b.lOOR JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, JUNE 1987, VOL. 2 range for many elements. Similar mechanical and pneumatic direct sample insertion systems have been described which could be used in the analysis of solid (10 mg) or liquid (10 pl) materials (8611779, 8611992). Reproducibility of 7% was reported as a consequence of temperature limitations. It was also commented that spectrometer development would be required to obtain optimum performance on a multi-element basis.This applies equally to most of the other discrete sample introduction techniques currently in fashion. The use of electrical sparks to vaporise sample for introduction into the ICP has received further attention (86/C879, 86/C1491, 861C1533). Instruments were designed to sample molten metals in situ by sparking the sample via an inserted probe. The resultant particulate material was swept into the ICP by the argon flow. There has been continued investigation of laser ablation as a method of solid sampling into the ICP (86/C808,86/C841,86/1464). Once again, the development of intelligent instrumentation has considerably helped in improv- ing the speed and precision of analysis (86/C808).However, better reproducibility will be required in order to establish the method. Modulation of the sample introduction procedure has been shown to provide improvements in signal to noise ratios and detection limits in AES (86/1991). A pressure pulse was applied to the nebuliser chamber by means of a motor driven piston operated under controlled and variable frequency (8-20 Hz). The modulated analyte emission signal was measured using a conventional monochromator and photo- multiplier with a lock-in amplifier as a frequency selective detector. Although this system was evaluated for FES, the extension of the technique to ICP-AES was considered. Although the ICP has been commercially available for more than a decade, there is still some way to go in establishing an optimum configuration, and there has been a continual stream of design modifications to suit specific applications.The frequency of operation of the inductively coupled plasma is still under investigation, and is indoubtedly of interest to many users. The majority of commercial systems are operated at 27 or 40 MHz as these are “allowed” frequencies, but the characteristics of plasmas operated at higher frequencies are not well established. Webb and Denton (87/116) have compared the analytical performance of ICPs operating at 27 and 148 MHz. It was found that both analyte and continuum background intensities decreased at higher frequencies due to a lowering of temperature, and importantly, that SBRs were also lower. However, the ease of sample introduction was found to be improved at higher frequency.Michaud-Poussel and Mermet (86/2016) in an extremely valuable paper studied the influence of generator frequency and plasma gas inlet area on torch design. Generators at 27, 40, 56, 64 and 102 MHz were compared in order to design a lower-power low-flow plasma. It was found that at higher frequencies, torch dimensions had a less critical effect on plasma stability. The power requirements and Ar consumption were found to be significantly less at higher frequency. For example, the power range at 64 MHz was reported as 800-1000 W compared with 400-600 W for the 102-MHz system. In order to maintain a toroidal shaped plasma, a minimum gas flow of 3 1 min-l was required, irrespective of operational frequency or torch design.At higher frequencies, it was found possible to use low gas flow-rates even with very large torches (i.d. > 25 mm, 86/C1211) thus obviating the need for miniaturisation of the ICP as exemplified elsewhere (86/C818, 86/C890, 86/C1191, 86/1732). These observations were supported by independent studies of a 40-MHz plasma operated at 600 W and 6 1 min-l argon flow (86/C1508) and investigations of the characteristics of a laminar flow torch for ICP-AES and ICP-FTS. The latter could sustain a discharge on 400 W applied power at reduced gas flow-rates (86/1241, 86/1350, 87/C153, 87/C175, 87/521). This torch was also shown to reduce source noise which is an important consideration in FTS. de Galan (87/590) has reviewed the design requirements of high-performance low- power, low-flow ICPs whilst continuing to pursue the develop- ment of air-cooled torches operating at 1 1 min-1 total argon flow (8611605).Complementary to the studies of low argon consumption ICP instruments, investigations of the use of alternative discharge gases have been carried out. Recent advances in the design of air ICPs have been the subject of a review article (87/514). There is some evidence to show that molecular gas ICPs should be more efficient at decomposing samples than conventional Ar ICPs (861C1174). An on-line air ICP spectrometer has been described (86/C1573), which was intended for continuous monitoring in a production or process control environment. Air was supplied to the unit via a compressor, and the system therefore had a very low associated operating cost.The determination of three ele- ments in a brine stream was used to illustrate the performance of the system. In an evaluation of mixed gas ICPs, it was reported that the emission characteristics of an Ar ICP could be altered considerably by introducing the foreign gas into the source. The results appeared to indicate that superior perfor- mance, in terms of sensitivity, stability and freedom from certain interference effects may be obtained when the conventional Ar ICP is converted into a 10‘30 mixed gas plasma. In principle, the He ICP should be a more efficient excitation source than the Ar ICP. Several studies have been made of the characteristics of an annular He ICP (86/C806, 861C1213, 86/C1575, 86/1606, 871464).Results were obtained which indicate that detection limits for aqueous C1 and Br are improved by more than one order of magnitude in comparison with those of conventional Ar ICPs. Such a system could be operated at 8 1 min-1 He consumption using a low-flow torch and an applied power of 1000 W. Only minor modifications were required to convert a commercial ICP system for this purpose. A reduced pressure He ICP was also described which operated at a power of <300 W (86/1963). The system was investigated as a potential GC detector for Br and C1. Reviews have been published on instrumentation for microwave plasma spectrometry (86/1860) and the principles of the microwave hollow-cathode source (86/1307). The power transfer characteristics of microwave plasmas have been examined in several studies (86/C815, 86/C1539, 861 C1601).It was claimed that capacitative coupling of micro- wave power greatly increases the efficiency of plasma genera- tion. Thus extremely low-power Ar, He or N2 plasmas could be generated which were just as effective as conventional MIPS operating on an input power at least an order of magnitude greater. The low thermal capacity of the MIP has earned it a reputation for being unable to tolerate even small amounts of sample matrix. In an alternative approach, surface electromagnetic waves were used to sustain a microwave plasma in a device called a surfatron (86/C1166, 86K1593, 86/C1596). It was reported that this He plasma has an annular shape which gives rise to maximum analyte emission in the central channel in an analogous manner to an ICP.Signifi- cantly, the stability of the discharge was considerably improved in comparison with systems employing the Beenak- ker cavity, and it was found possible to nebulise solutions at flow-rates of 500 ml min-1 at relatively low power levels (100-150 W). The surfatron was applied as a GC detector for Br, C1 and S and its performance compared with that of established systems (86/C1593). The MIP is well established as a gas chromatographic detector (see section 4) and there have been attempts to improve torch design for applications in this area (86/C1598,86/1917). A low flow, plasma centering torch with laminar flow characteristics has been described which was evaluated using a computer controlled background correcting polychromator system.Detection limits of between 8 and 60 pg s-1 were reported for C, H, Br, C1 and F which were a substantial improvement in performance in comparison with the tangential flow torch. Relative standard deviations obtained on a 3 hour and 3 day basis were 2 and 6%,JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, JUNE 1987, VOL. 2 101R respectively. The centred plasmas could be sustained with flow-rates as low as 5 ml min-1. There has been relatively little development of instrumenta- tion for DCP-AES in the year under review. The most significant progress has been made in the re-design of the source to improve sample entrainment. The idea behind this approach is to produce a more ICP “like” plasma whilst utilising the much less expensive d.c.power supply. A conical three electrode d.c. plasma has been devised which was intended to provide similar efficiency of sample decomposi- tion as obtained in the ICP (86/C1168). The new configuration had an aerosol introduction tube (i.d. 1 mm) positioned beneath the plasma to improve sample penetration. Detection limits reported for the new system compared favourably with the commercial DCP, and the linear dynamic range was found to be extended by 1-2 orders of concentration. A sample entraining multi-electrode DCP was described which provided detection limits approaching those of an ICP (86/C1214). Three pairs of electrodes formed three vertical columns of d.c. arc which merged to surround completely the sample stream which was introduced along the vertical axis.The atom to ion intensity ratios obtained for Mg suggested that the sample experienced considerably increased temperatures, which would be expected to provide better performance in terms of dissociation and reduction in interference effects. There has been little progress in the field of electrothermal atomisation atomic emission spectrometry (ETA-AES) except in the applications area (86/1627,86/1796,87/492). A low-cost spectrometer system has been described which utilised a 174-mm focal length Ebert monochromator, modified for wavelength modulation background correction (86/1892). A Perkin-Elmer, HGA-72 atomiser, equipped with a graphite probe sampling accessory, was used in conjunction with the spectrometer to obtain detection limits in the low parts per billion range.Although the reported sensitivity was approxi- mately an order of magnitude poorer than an earlier system based on an Cchelle spectrometer with similar technology, the relative cost of the instrument could make it a more attractive option for many analyses. In the related technique of furnace atomic non-thermal excitation (FANES), several papers were devoted to studying the fundamental characteristics of the atomiser - excitation source (86/C781,87/C148,87/425) and to analytical applications (86/1642, 87/623). The commercial introduction of the FANES source is likely to stimulate further investigations of the analytical characteristics of this intriguing “discharge within a furnace.” 6.2. Absorption The state of the art instrument for AAS has reached a degree of refinement which is difficult to improve significantly upon without a fundamental reappraisal of the concepts on which the technique is based.Progress is therefore made rather slowly, in a gradual process of consolidation, rather than via any major “breakthrough” advances. Indeed, there may be very little commercial motivation to revise radically the principles of operation of what have proven to be, in the majority of analytical situations, highly successful instrument designs. Perhaps the most obvious example of the problem is illustrated by the technique of continuum-source atomic absorption spectrometry (CS-AAS) which provides a means of background corrected simultaneous multi-element analysis using flame or furnace atomisers. A number of reviews have been published in the past year which have documented the current status of the technique (86/1908, 86/2005, 87/57, 87/110).It is pertinent to note that the wavelength modulation background correction system employed in CS-AAS can also be used with equal efficiency in AES (86/1908, see also JAAS, 1986,1,15lR). The practical application of continuum-source ETA-AAS has been demonstrated in the multi-element analysis of slurries (86/C904, 86/C926, 86/C1975), in the determination of trace elements in blood (86/C779) and in the determination of trace elements in reference materials by a N20 - air - C2H2 flame (86/1087). The design of the computer based data acquisition and signal processing system offers considerable scope for the investigation of fundamental processes in AAS and in diagnostic studies (86/C1546).It is evident that the next stage in the development of this technique must be in a commercial implementation and it remains to be seen which manufacturer will take the first step. An interesting report described the application of AAS to isotope abundance determinations (86/C1586). Absorbances were measured for 63Cu and 65Cu using monoisotopic light sources and a variety of atom cells (air - C2H2 flame, ICP and a transient atomiser) by monitoring hyperfine structure. The Zeeman effect was also employed but was found to lessen the ability to distinguish between isotopes, presumably because of a reduction in resolution. It was predicted that it should be possible to distinguish f 0.5% absolute isotope abundances for Cu in the air - C2H2 flame using this technique.Few papers dealt with improvements in instrumentation for FAAS. A water cooled surface burner for AAS was described which incorporated a 10-cm slot through which the fuel, either C2H2 or H2, nebuliser gas and sample aerosol flowed (86/C1563). A row of drilled holes on either side allowed the flow of oxidant (02) to the burner surface where the diffusion flame was formed. The design of the burner prevented the possibility of flashbacks. As a consequence of the high temperature of the flame produced, detection limits were improved by up to an order of magnitude for marginally refractory elements such as Ca and Cr. A comparison has been made between single- and double-beam measurements in Part 6 of a study of FAAS (86/1783). Differences in precision between the two configurations were investigated for the Jenoptik AAS 5 spectrometer which could be operated in either mode under similar experimental conditions.It was reported that better precision in the single-beam mode was obtained under conditions of high amplification. A modified pneumatic nebuliser for FAAS was described which was claimed to improve liquid transport characteristics (86/C836). This was achieved by altering the position of the nebuliser capillary in the venturi throat to maximise suction. The uptake rate of the nebuliser was significantly less affected by hydrostatic pressure resulting from sample liquid levels. The dissolved solids handling capability of the nebuliser was claimed to be improved. In an interesting paper, the use of thermospray sample introduction, more familiar in LC - MS, was discussed in relation to ICP-AES (86/C1526).The system employed an electrically heated capillary tube which provided a controlled vaporisation of aqueous sample solution at flow-rates up to 2 ml min-1. A range of aerosol characteristics from droplets to dry particulates could be produced by adjusting the temperat- ure control. This device offers some of the favourable characteristics of electrothermal vaporisation in terms of improved efficiency, and nebulisation in terms of continuous sample throughput, and it is likely that further studies in this area will be undertaken. The primary focus of research effort in AAS is undoubtedly on the design of high-efficiency electrothermal atornisers. Some methods, such as platform atomisation, have now been accepted into routine methodology, primarily because of the simplicity of the approach (86/1471). Constant-temperature atomisers although no longer novel, now appear to be undergoing a second phase of development, in which refine- ments are being made to original concepts.The second surface atomisation technique has undergone a number of changes since its initial introduction (86/C905? 86/2027? 87/117). Analyte was evaporated from the tube surface on to a gas cooled tantalum plug inserted through a hole machined in the102R JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, JUNE 1987, VOL. 2 atomiser wall. After the atomiser reached a stable set temperature, the coolant was shut off allowing the analyte to be re-released. In the latest design, a contoured tube was introduced to avoid non-uniform heating caused by removal of graphite to accommodate the plug.The secondary surface was removed to allow autosampling and this has an additional benefit of improving residence time by eliminating the sampling hole. Higher coolant flows could be utilised with the new design, and independent choice of coolant and sheath gas was possible. The method was used to separate partially volatile analytes from a matrix by employing a “reverse ashing” procedure. The more general aim of reducing interferences was achieved on a scale comparable with other constant-temperature type atomisers. A spatially isothermal atomher was described in which the graphite cuvette was side-heated with integrated contacts. The entire cuvette and associated contacts were manufactured from a single graphite piece to avoid difficulties in electrical connections.For non-volatile elements, lower atomisation temperatures could be used to achieve similar sensitivities to those of Massman type furnaces. Fewer problems were reported with signal tailing, condensation and memory effects. The system was used in conjunction with a platform to provide higher vapour phase temperatures than those achievable using a Massman atomiser fitted with a platform. Consequently, the perfor- mance in respect of spectral and chemical interference effects was reported to be improved. Ottaway and co-workers (86/775, 87/318) made extensive investigations of probe atomisation for ETA-AAS.Contributions included studies of front- and end-entry configurations (86/1357, 86/1647), tube probes (871616) and probe materials (86/1647, 87/318) for an SP-9 furnace. The main benefits of these updated approaches appeared to be to improve performance in terms of reduction of chemical and physical interference effects, whilst maintain- ing the sensitivity of conventional ETA-AAS. An additional advantage of the technique was that the probe could be developed as an accessory for most commercial atomisers. Probe atomisation has been used in a novel application for the direct determination of toxic metals in air particulates (86/C928,86/C1978). In this technique, a detachable graphite probe was installed in an air filtration unit and atmospheric particulates were collected on its “head.” The probe was then inserted into a modified electrothermal atomiser, and the sample was atomised at constant temperature.The method had the advantage of avoiding contamination, was free from interferences and was extremely simple and rapid. Details of ETA-AAS instruments dedicated to atmospheric sampling using electrostatic accumulation (86/2017) and impaction (87/493) have now been published. In an important new development, the graphitefurnace has been used in conjunction with hydride forming elements. Dittrich and co-workers (86/1639, 86/1640, 87/434) investi- gated interferences in both liquid and gaseous phases in hydride generation. The chemical interferences in the liquid phase were eliminated by the use of matrix modifiers.However, to remove gas phase interferences, a new graphite paper atomiser with a 10-cm path length was developed, which could be resistively heated to temperatures of 2700 “C. It was found that in the presence of interferences resulting from hydride forming matrices, the graphite paper atomiser pro- vided improvements in sensitivity of X 10 to X 1000 compared with the conventional quartz tube device. This was attributed to the dissociation of diatomic molecules at the higher temperature of the graphite atomiser. In a similar approach, Sturgeon et aE. (86/720, 86/C786, 86/C902, 87/433) described the trapping of generated hydrides on the surface of an activated graphite tube, and their detection by subsequent atomisation. This provided an interference-free method for the determination of As, Sb and Se in sea water. Absolute detection limits of 30 pg for As and 70 pg for Se were reported, with respective working range precisions of 2-3 and 5-10%.6.3. Fluorescence In contrast to AAS, atomic fluorescence spectrometry (AFS) is a technique which has never really come of age. There has been remarkably little commercial exploitation of AFS, in spite of the high sensitivity and spectral selectivity inherent in the method. The lack of sufficiently intense and stable light sources during the early period of development of the technique perhaps contributed to its somewhat diminished role in mainstream analytical atomic spectroscopy. The advent of tuneable laser sources has undoubtedly revitalised the subject, and it is significant that the majority of new instrumental developments reported incorporate laser excita- tion.A variety of atom sources have been exploited in laser-excited atomic fluorescence spectrometry (LAFS). The characteristics of a LAFS system incorporating a glow discharge atomisation source have been described (86/1392, 86/C1495, 87/124, 87/512). Analytes, in either solid or liquid form, were sputtered from copper or graphite surfaces by means of a d.c. discharge operated at 550 V, 25-50 mA and 5-8 torr. A nitrogen laser was employed to pump a pulsed, frequency-doubled dye laser which was used as the excitation source. Detection limits, by non-resonance AFS, for In, deposited in 1O-pl droplets on graphite and copper electrodes, were reported to be 8 X 10-9 and 11 X 10-9 g, respectively (87/124).However, it was observed that diatomic species were produced in addition to analyte atoms, and the spectra of Cuz, Pb2 and CuO were identified in the sputtered vapour (86/1392, 87/572). It would appear from this study that matrix effects on the efficiency of atom production and spectral interference by molecules produced by the discharge process significantly limit the potential of the technique. Electrothermal atomisers provide extremely high sensitivity in AAS, but whilst an AFS equivalent might be desirable, a workable system is more difficult to devise because of optical considerations. The most convenient approach is to observe fluorescence above the atomiser, in the manner described by Bolshov et al. (87/126, 87/260). This procedure minimises the contribution of continuum radiation from the atomiser, but may give rise to interferences because of temperature gradient effects.However, in a recent development, the cup atomiser was modified to operate under vacuum conditions (871126). Although this had an adverse effect on detection limits, by as much as two orders of magnitude, it was claimed that matrix interferences were decreased as a result of the collisionless expansion of the atomised sample components. The solid sampling capability of the system was demonstrated by the interference free determination of Cu in tin, vegetation samples and quartz glass. Michel and co-workers (86/C877, 86/C990) have pursued the development of a LAFS system based on the more conventional tubular furnace design. It is encouraging to see this move towards more appropriate furnace technology, since this is likely to circumvent the re-discovery of atomiser design problems first encountered in AAS and AFS in the early 1970s.It was reported that detection limits obtained with this instrument were within a factor of 5-10 of the best literature values for LAFS. A comparison of rod and tubular atomisers for LAFS has now been published, which revealed substantially improved detec- tion limits and reduced interferences using graphite tubes of the HGA-500 type (87/523). The use of various graphite tube coatings to improve the atomisation efficiency for refractory elements has also been reported (861C916). The requirement for background correction is particularly important in ETA measurement, because of the intense radiation generated by the source, and in practical analysis, scattering effects produced by transient species.Zeeman-effect background correction, whilst mainly employed in AAS, is equally applicable in AFS measurement. In a discussion of the most suitable Zeeman configuration for laser-enhanced atomic fluorescence spectrometry in conjunction with ETA, it was concluded that an a.c. magnetic field should be employed,JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, JUNE 1987, VOL. 2 103R with laser radiation directed parallel to the field (86/C876, 86/C990). The related topic of coherent forward scattering (CFS) is likely to receive increasing attention as the use of lasers as light sources becomes more common (see also ARAAS, 1984, 14, 66).Essentially, polarised light is passed through an atomic vapour, typically generated by an electrothermal atomiser, which is located in a magnetic field in an analogous manner to that in Zeeman-effect background correction systems. The plane of polarisation of the transmitted beam is rotated with respect to the incident beam and can be detected by a second polariser. An important feature of CFS is that the signal is proportional to the intensity of the incident radiation, and consequently the application of laser sources should give rise to improvements in detection limits. A system was described comprising continuous wave and nitrogen-pumped dye lasers as sources, and a graphite furnace based upon a CRA-90 tube design, directly controlled by an IBM PC (86/C1479, 86/ C1544).The magnetic field was generated by means of an electromagnet constructed from transformer plates and ano- dised aluminium foil. It was claimed that this system could provide detection limits superior to those of ETA-AAS for many metals. A facility was also available on the instrument to correct for broad-band background absorption. In a related approach based on the Voigt effect, laser light, either an argon ion or a pulsed tunable dye laser, was passed through a polariser set at a 45" angle to the transverse magnetic field (86/C1558). A Varian A-60 electromagnet was used to produce a 1.4-T field at a polegap of 18 mm, and was compatible with an air - C2H2 flame or furnace atomisation. A second polariser was used to detect the rotated light and a monochromator and PMT were used to isolate the appro- priate atomic line.It was noted that because the CFS signal produced is coherent, the detector could be placed some distance from the atomiser, significantly reducing background emission contributions. Fluorescence systems incorporating plasma sources remain a focus of research activity, and although the majority of the work has been devoted to the ICP, instruments incorporating DCP and MIP sources have also been described. Atomic fluorescence spectrometry offers plasma spectroscopists diag- nostics facilities for mechanistic studies, in addition to providing an analytical alternative to AES measurement. Enhancement effects produced by easily ionised elements have been studied in a LAFS system consisting of a pulsed eximer laser, a DCP and an echelle spectrometer (87/89).It was found that fluorescence enhancement effects observed in the analytical zone of the plasma, close to the core, disap- peared if saturating laser power was employed, indicating that interferences were caused by rate effects rather than resulting from changes in atom population density. The analytical performance of this system was characterised for a three-electrode DCP (86/1866). Detection limits for Ba, Ca, Fe, Na and V were reported in the range 3-72 mg ml-1, but were inferior to comparable LAFS figures of merit obtained using flames and ICPs. The magnitude of the plasma background and scattering effects were shown to be the main factors which limited detection. A high efficiency nitrogen MIP operated on 50-W microwave power has been charac- terised as a LAFS source (86/C1501, see also section 6.1).A hot filament sampler and a Hieftje micro-arc system were compared as pre-atomisation devices for the MIP. Preliminary investigations of analytical performance concentrated on the measurement of Na for which a detection limit of 20 pg was reported. Publication of this work is awaited with interest, as these workers indicated that the MIP should provide superior detection capabilities in comparison with ICP or flame-based LAFS instruments. Several reports have appeared in the year under review documenting the continued use of ICPs as atom reservoirs in LAFS. In one of the more important studies, Omenetto et al. (86/1791) have now published details of a technique known as laser induced double resonance ionic fluorescence, using an ICP.Two tunable pulsed dye lasers, pumped by an excimer laser, were directed into the analytical zone of an ICP, allowing the simultaneous excitation of ions to select high lying levels. This two-step or double resonance excitation was found to be extremely sensitive with detection limits for alkaline earth elements reported at the sub-yg 1-1 level, highly selective spectrally (86/C1245), and free from scattering effects. The measurement of ionic fluorescence by the double resonance technique was more useful in the ICP than was atomic fluorescence in a flame because the second ionisation potential of the ions was usually larger than the excited energy level, and the phenomenon of depletion of energy levels due to ionisation was not observed.Using a more conventional experimental arrangement, a study was made of LAFS for the determination of precious metals and refractory elements (86/1875). An excimer pumped pulsed dye laser with fre- quency doubled ouput was used as the excitation source and an Ar ICP was employed as an atom - ion reservoir. Detection limits reported were in the range 1.3-58 mg ml-1 for Ag, Au, Hf, Ir, Mo, Nb, Pd, Pr, Ru, Ta and Zr and were found to be similar to those achieved in ICP-AES. For most of these elements, a linear dynamic range of about four orders of magnitude of concentration was achieved. Winefordner (86/ C1497) discussed the range of possibilities for AFS measure- ment using a variety of atom reservoirs including the ICP.Although LAFS provides spectral selectivity and high sensi- tivy it is relatively expensive and provides single-element rather than multi-element operation. The use of two ICPs, one as a radiation source and the other as an atom cell has been advocated by two groups (see also ARAAS, 1984, 14,20). Greenfield (86/C1244,87/286,87/460) has described the features of the ASIA (atomiser, source, ICPs in AFS) system which employed a 5-kW ICP as the source and a low-power Ar ICP as the atomiser, using modulation to provide phase sensitive detection of the AFS signal. The high-power plasma utilised a large torch which was more suitable for the aspiration of solutions of high analyte concentration. There is also an advantage to be gained in AFS measurement from the greater spectral radiance of the 5-kW ICP.Detection limits were reported to be superior to those obtained in ICP-AES except in the case of refractory elements (86/1603). The formation of refractory oxides in the ICP tail flame is a problem in AFS measurement, since the optimum viewing height in the plasma is considerably higher than for ICP-AES. This problem has been overcome by the addition of a small amount of propane to the plasma (86/1603,87/C540). Several examples of the use of non-resonance fluorescence to overcome spectral interference problems found in ICP-AES were described (87/C135,87/C178). Although this system is at present operated with two ICP systems, it should be possible, in principle, to run both plasmas from the same generator. In an alternative approach, the sample was introduced to a low-power Ar ICP, and its emission measured using a second Ar ICP, as a resonance monochromator (86/1881).This measurement system, intended for the analysis of major components, provided linear dynamic ranges of up to 5 x 107 but with reduced sensitivity. The system could also be used as a fluorescence spectrometer by aspirating the sample in the second plasma, and in this case, detection limits were found to be similar to ICP-AES for non-refractory elements. A DCP has been used in a similar fashion as an excitation source for FAFS (86/1007, 864888). It was found by examination of the shape of analytical growth curves that the DCP, under certain experimental conditions governed by the relative position of the sample introduction tube could be regarded as a narrow spectral line source or as a pseudo-continuum source.Limits of detection were reported to be in the range 1-30 mg ml-1 except for As and Pb which were 25 and 5 yg ml-1, respectively, presumably due to the relatively poor excitation104R JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, JUNE 1987, VOL. 2 conditions at UV wavelengths. The system was applied to the determination of Co, Cr, Cu and Mn in steel samples, and Cu, Fe, Mn and Zn in NBS reference materials (86/1888). Several studies were described in which xenon-arc continuum sources were employed for excitation purposes in AFS. These included a detection system for GC - MIP (86/C1502), a study of spectral interferences in FAFS (86/1415) and a wavelength modulated detection system for AFS in a metastable N2 plasma (87/C556).Details of a previously described combined atomic emission - atomic fluorescence spectrometer (see ARAAS, 1984, 14, 74) have also been published (86/1356, 86/1876). There have been few new developments in instrumentation for hydride generation atomic fluorescence spectrometry. An electrically heated silica tube atom cell was described for the determination of Se by AFS (86/1429). A detection limit of 1.4 mg in 10 ml of aqueous solution was reported, with linear calibration up to 600 ng. Relative standard deviations of 4.348% were obtained within the working range of the technique. Two non-dispersive AFS hydride generation procedures were developed for the determination of Pb (86/1793, 871482).6.4. Mass Spectrometry Although inductively coupled plasma mass spectrometry (ICP- MS) is by no means as yet a commonly encountered technique in laboratories concerned with elemental analysis, there is undoubtedly enormous interest in its potential, particularly amongst ICP-AES users. Reviews of the current state of the art are therefore particularly welcome in this context (86/1380, 86/C1477, 86/C1478, 86/1608). Many studies published in the year under review attempted to assess the “real” analytical performance capabilities of ICP-MS instruments “in the field” (86/1670, 87/26, 87/67, 87/68, 87/321). Most of these reports testified to the extremely high sensitivity that could be achieved using the technique. However, a number of prob- lems were identified in the application of ICP-MS instruments to determinations in complex matrices.These included spectral interferences, ionisation effects and limitations on the selection of acid media for the preparation of solutions and on the maximum dissolved solids content of samplts. Horlick and co-workers (86/C789,86/C821,87/106) investi- gated the effect of operating parameters on analyte signals observed in ICP-MS using a Sciex Elan instrument. It was found that the most influential instrumental parameters were aerosol flow-rate and power settings, as might be anticipated from ICP-AES studies. The influence of sampling depth, a parameter which is significantly different in the two commer- cial systems, was found to be small in the range 17-25 mm above the load coil.In a related study by the same group (86/C1499,86/C1970,87/29,87/30) extremely detailed investi- gations of ICP-MS spectra were reported. It was commented that serious spectral interference effects could arise as a result of the presence of oxide, hydroxide and doubly charged analyte species (86/C1970, 87/29) or from the inappropriate selection of acids in the analytical procedure adopted (86/ C1499, 87/30). It was also reported that the presence of a matrix at a level of 1000 pg ml-1 could give rise to the suppression of the signal of a trace analyte component by as much as 80%. This effect was reduced to about 10% by adjustment of instrumental parameters, but with a consequent loss in sensitivity (86/C1499). The matrix effect appeared to have a mass dependence in addition to being associated with ionisation potential.Inter-element interference effects of this type, which are not observed in ICP-AES are being reported with greater frequency (86/C1121,86/C1210, 8611381, 87/26). The effect of concomitant elements may give rise to significant enhancement or suppression of analyte signals, but the origin of these interferences is not well understood. It would appear, however, that such effects are not restricted to a particular instrument design. A new ICP-MS instrument has been designed in which the ICP was orientated in a vertical position on an xyz translation stage (86/C796, 86/C1105). It was possible to observe optically both the plasma, or an alternative source, and the one-torr intermediate region of the vacuum system.This allowed the study of the formation of interferent ions, e.g., doubly charged ions and oxide ions, either in the plasma or during transport to the mass spectrometer. The instrument could be used in the MS mode to detect both positive and negative ions. Analogue or digital detection was possible, which resulted in an increase in the linear dynamic range of the instrument. The system could be operated under a rapid scanning measurement mode or using rapid computer controlled peak switching for the detection of a limited number of species. The instrument was also used for the measurement of isotope ratios (86/C1486) and to study the influence of generator frequency on ICP-MS detection. Further studies have been made of the combination of a 100-MHz ICP generator and a quadrupole MS (86K1120, see also JAAS, 1986, 1, 67R).The effect of dimensions and pressure in the first vacuum stage of the instrument were discussed. The influence of the operating parameters and characteristics of the discharge using a low-power , low-flow torch system were described with reference to analytical performance and spectral complexity. The nature of the interface between the ICP and the mass spectrometer is undoubtedly the most critical design aspect of the instrument. Douglas and French (87/70) have reported that centre grounding of the load coil effectively eliminated a sccondary discharge between the ICP and the sampler. The levels of doubly charged ions observed using this new configuration were reported to be greatly reduced.No ions from the orifice or skimmer materials were observed in the spectra obtained, and sampler lifetimes were found to be improved. The construction and performance of a supersonic nozzle for ICP-MS and that of an off-axis detector arrange- ment for photon background suppression were described (86/1378). The search for improved means of sample introduc- tion for ICP-MS closely parallels that in ICP-AES (see section 6.1). However, as a rapid scanning technique, with relatively fast data acquisition facilities already in place, ICP-MS is perhaps better placed to take advantage of the development of sample introduction systems which produce a transient response (see also JAAS, 1986, 1, 67R). Developments in laser ablation (86/C797, 86/C1118, 86/C1133, 86/C1480), electrothermal vaporisation (86/C797, 86/C1133, 86/C1193, 87/C199) and arc sampling (86/C1141, 87/60) were reported.Laser ablation has also been applied in glow discharge mass spectrometry (86/C893). The laser was used initially as a direct atomisation source with no discharge, using the MS to detect analyte ions. However, subsequently the laser was employed to ablate material from an electrically neutral sample into an adjacent glow discharge. This was found to be preferable to direct laser ablation within the glow discharge which gave rise to noise spikes which interferred with the data acquisition system. The characteristics of a double focusing MS in combination with a glow discharge for trace elemental analysis has been described (87/C189). It was claimed that the use of a dual Daly - Faraday detector system covering a range of ten decades of concentration allowed for the determination of major component composition and part per billion level trace analytes in the same analysis.There have been further reports of the development of an MIP-MS system (86K1106, 86/ C1535, see also JAAS, 1986, 1, 67R).JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, JUNE 1987, VOL. 2 7. COMMERCIAL INSTRUMENTS 105R A list of commercial instruments, available at the time of writing (January 1987) is provided in Table 2. Details were supplied by manufacturers or their UK or European agents. The most significant developments are described below. Instrumentation introduced at the 1987 Pittsburgh Conference is also described in the text.7.1. Emission Commercial developments in emission spectrometry during the review period concerned the instrument companies almost as much as their products. Allied Analytical Systems have now become Thermo Jarrell Ash (Thermo Electron Ltd. in the UK). The company have introduced the ICAP 61, a 61 channel airhacuum simultaneous ICP system, which is con- trolled by an IBM PC/AT. A combination version of the instrument, incorporating a computer controlled monochro- mator for sequential analysis is also available. The in-built r.f. generator features auto-tuning, a facility common to the Plasma 300 instrument introduced last year (see JAAS, 1986, 1,67R). The benefits of the new auto-tuning system incorpor- ated into the Plasma 300 r.f. generator have been discussed with respect to the analysis of organic solutions (861C1559, 87/C551).ARL have introduced the 3410 sequential ICP system which features a mini-torch for low-power, low-flow operation. The plasma runs at power levels of 0.6-0.7 kW and is reported to consume 40% less Ar than when using a standard torch system, at a consequent cost advantage. Analytical charac- teristics of the 3410 instrument, which offers a 1-m Czerny - Turner monochromator controlled by an IBM PC/XT, are reported to be comparable to conventional systems (86/C818, 86/C890,86/C1191). ARL now includes the Spectraspan series of DCP instruments (ex Beckman) in its range of emission spectrometers. P. S. Analytical will market the instrument and associated accessories in the UK. In a significant development, Philips Analytical have introduced the PU 7450, a sequential bench top ICP instru- ment.An kchelle grating spectrometer is employed in the system to provide high resolving power. The PU 7450 is a modified version of the Leeman Labs Plasmaspec instrument, and bears the Philips name, following an agreement between the companies. The instrument is being marketed as a low-cost ICP system which can determine up to 20 elements in a single programmed run. The capability exists to store up to three programs using the basic instrument, but it can also be used in conjunction with a Philips Analytical Data Station if addi- tional program storage is required. Leeman Labs have also updated their software for the Plasmaspec by employing an IBM PC to run the Dataspec I1 Package developed by Ward Scientific. Philips have now deleted their PV 8210 and PV 8250 range of emission spectrometers, following the introduc- tion of the PV 8030 and PV 8020 series last year (see JAAS, 1986, 1,67R).At the 1987 Pittsburgh Conference, Perkin-Elmer intro- duced the Plasma 40, low-cost benchtop ICP instrument. The system incorporates a sequential monochromator (0.19 nm resolution) controlled by an IBM PC which also performs functions such as automatic background correction, data handling and report generation. The free running r.f. genera- tor runs at 40 MHz and this is a further indication of the general trend towards higher operating frequencies. An interesting feature of the source unit is that the load coil is argon cooled, eliminating the need for an external water Perkm-Elmer continue to promote their Plasma I1 ICP spectrometer (86/C804, 86/C817, 86/C933, 86/C1169, 86/ C1176).The company have acknowledged the trend towards improved resolution in ICP-AES by introducing the ICP 6500 supply .. XR instrument. This system is basically an enhanced version of the ICP 6500 which has been on the market some time. The new instrument utilises a 4200 grooves mm-1 holographic grating over the 160-460 nm range. The company have also produced a new autosampler for ICP or flame work. Features include removable interchangeable sample trays, which can accommodate different sizes of sample vessel, random access programming capability and solvent and acid resistant Sam- pling components. Jobin-Yvon offer essentially the same spectrometer range (86/C1188, 86/C934) but perhaps significantly, the operating frequency of their ICP systems is now 40.68 MHz, reflecting recent research trends.The series of plasma spectrometers available from Baird also operate at this frequency. The PSX incorporates a 0.75-m sequential monochromator whilst the PSQ is a low-cost simultaneous system offering 30 channels per analysis. Both instruments have low-power, low-flow torch units available and employ IBM PCs for signal process- ing. Workers from the company have described the charac- teristics of an on-line air plasma emission spectrometer, the APS-100 (86lC1174, 86/C1573). The system, designed for continuous monitoring applications, was constructed under exclusive licence from the Dow Chemical Company (86/ (3161).The use of compressor supplied air, rather than Ar, to sustain the plasma is obviously a major cost benefit of the system. PRA have announced improvements to their Plasmarray ICP instrument. The detection system has been updated to incorporate state-of-the-art photodiode array technology, and it is claimed that detection limits obtained with this sytem are now significantly better than standard literature values for conventional ICP instrumentation. The linear dynamic range is 5-6 orders of magnitude of concentration using the Plasmarray system. Chelsea Instruments formally introduced their FT500 spec- trometer at this year’s Pittsburgh Exhibition. The dual output Michelson interferometer has a spectral range from the near IR to 175 nm with a resolution of 2 x 106 at 200 nm.The spectrometer may be used as a high-resolution detector for ICP-AES, and potentially for continuum-source AAS. Spectro have up-graded their ICP power supply to a rating of 2.5 kW and their combination spectrometer is available with a range of reciprocal dispersions (86/C1171 , 86/C1189). Labtest Equipment Company continue to promote their 40-MHz low-power, low-flow ICP system (86/C1508). Several companies have changed their addresses or UK or European agents. An updated list is provided in Table 3. 7.2. Absorption Thermo Jarrell Ash (formerly Allied Analytical Systems) have updated their Video AA series with enhanced software in order to provide central control of their new furnace and autosampler. The CTF 188 atomiser incorporates a delayed atomisation cuvette, not dissimilar to that utilised some years ago for ETA-AES, which it is claimed, reduces interference effects (86/C922, 86/C924, 86/1920).The system has 112 pre-programmed factory supplied furnace methods, and up to 200 operator defined methods can be stored in non-volatile memory. Air ashing and solid sampling facilities are available. The system is compatible with aerosol deposition sample introduction. The ISC-60 autosampler consists of a micro- processor, a programmable random access sample changer and a removable sample tray and can be used with either flame or furnace autosamplers. The full system has the ADS-200 data station based on the IBM PC/XT to provide data management. At the Pittsburgh Conference the PS-75 auto- matic sample preparation system and ISC-75 Intelligent Sample Changer were introduced as accessories for the VideoJOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, JUNE 1987, VOL.2 106R E series of AA Spectrometers. The system provides automatic sample dilution, matrix modification, standard addition and standard preparation for both flame and furnace atomisers. Varian have deleted their AA 1275 and AA 1475 spec- trometers and have introduced the SpectrAA 10 (single- beam) and SpectrAA 20 (double-beam) spectrometers (86/ C1540). The introduction of Varian’s new SpectrAA Zeeman Series at the 1987 Pittsburgh Conference represents a signifi- cant addition to the company’s AA product range. The system employs a pulsing frequency of 60 Hz providing 120 measure- ments per second and a polynomial interpolation routine applied to multiple data points to compute accurately the background magnitude.An extensive software package including graphics error detection, data storage archiving and report generation facilities is available. The company have also pursued developments in automatic hydride generation (861C906, 86/C951) and nebuliser design (86/C836, see also J A A S , 1986, 1, 68R). Analyte Corporation have introduced a sequential multi- element AA spectrometer which enables the determination of up to 20 elements in 100 s. However, there are few details available at present in respect of instrument performance, or the nature of the background correction facilities. The company also offer a novel ambient temperature ETA operating at 0.01 atm, which utilises an argon etching process for atom generation.Primarily designed for solid sample analysis, the system is claimed to provide detection limits for most elements in the low p.p.m. range with RSDs typically of Perkin-Elmer have announced the introduction of two new AA spectrometers. The Model 5100 is a fully automated double-beam system in which functions such as wavelength, spectrometer slit, lamp position and current, gas flows and autosampler mode, can be directly controlled from hard disc software via a multi-tasking Perkin-Elmer Series 7000 com- puter. The instrument is capable of determining up to ten elements in a single method using flame, graphite furnace or hydride generation atom cells. A separate version of the instrument, the Zeeman 5100, is available, if Zeeman-effect background correction is required for graphite furnace appli- cations.A comprehensive software package is supplied with the instrument, and provision is made for routine analysis and method development modes of operation. The Perkin-Elmer 1100 spectrometer is, by comparison, a low-cost single-beam instrument with a built in VSU and soft-key based microp- rocessor control. Conditions may be selected manually by the operator, or automatically if default values stored in the instrument for each element are selected. Provision is made for storage of up to 48 user developed methods. The spectrometer is compatible with flame, furnace and hydride measurement. The AS-80, a flame or ICP autosampler, is described in section 7.1.The company have devoted research effort to evaluating tube materials, in particular pyrolytically coated polycrystalline electrographite (86/C766, 86/C887, 86/C1547, 87/130, 87/391). Baird have introduced the PULSAR ETA-AAS system. 0.3%. The instrument features capacitative discharge heating of the atomiser under computer control. Furnace parameters are set automatically by accessing analytical methods stored on disk. The computer is also used to control the associated 80-position autosampler and for signal handling and results processing and display purposes. The furnace can be used with a graphite platform and in situ pyrolytic graphite coating of the cuvette is possible. GBC are now using Techmation as their UK agent. The company have deleted the SB900 single-beam spec- trometer, the GF 900 graphite furnace and associated auto- sampler.The replacement graphite furnace, the System 2000, features a ten-step temperature programme facility, with ramp and hold parameters on each step. A dedicated furnace autosampler, the PAL 2000, allows standard additions, matrix modification, multiple injection and variable volume sample introduction. The FS 1000 also introduced, is a flame autosampler which accommodates up to 60 samples and ten standards. Shimadzu have added two new autosamplers to their range. The ASC 60F autosampler takes up to 50 samples for sequential flame analysis. Aspiration, delay times and number of replicates are all user selectable. The ASC 60G is a furnace autosampler with an interchangeable carousel for up to 50 samples of up to 2-ml volume.Injection volume and wash cycles in both sample and solvent are user selectable. Pye Unicam retain the same range of AA instruments. Further studies of the characteristics of the company’s totally pyrolytic graphite cuvettes have been reported (86/C765, 86/822, 86/C923, 87/419). 7.3. Fluorescence The Baird Corporation ICP-AFS system remains the most obvious commercial exploitation of the AF technique. Appli- cations to the determination of metals in organic solutions (86/C1560) and of toxic metals on industrial hygiene air filters have been described (86/C830). 7.4. Mass Spectrometry There has been growing interest in ICP-MS as a technique for multi-element analysis, for a number of years. The two principal manufacturers, VG Isotopes (86/C1179, 87/C136, 87/C188) and Sciex (86/C1117, 86/C1133, 86/C1484) have continued to promote their respective instruments.The main development in the commercial area has seen the formation of Perkin-Elmer - Sciex Instruments. Perkin-Elmer has assumed marketing responsibility for the Elan instrument, whilst Sciex will continue to progress technical advances in ICP-MS. The co-operation is likely to stimulate interest of competing manufacturers of ICP-AES equipment. VG Isotopes have also been active in demonstrating the advantages of GD-MS in the trace analysis of metals (87/C189). An electrothermal atomisation sample introduction system for ICP-MS is now commercially available from P. S. Analytical (86/C797, 86lC1193).JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, JUNE 1987, VOL.2 107R Table 2. COMMERCIALLY AVAILABLE INSTRUMENTS A. Emission Spectrometers Reciprocal dispersion/ Wavelength Supplier * Model nm mm-1 (a) The following instruments continue to be offered by manufacturers?- Applied Research Laboratories . . . . 3360 3520 Baird Corporation Hilger Analytical Jobin-Yvon . . Kontron . . . . Lab tes t Equipment Philips Analytical 3460 3560 3580 3600 . Spectromet 1000 Spectrovac 1000 Spectromobile MS3 FAS 2 . E 1000 Polyvac E 980 Series Polyvac . JY32E JY 48E . FANES 310 V25 2100 V82 . PV8030 PV 8035 PV 8050 PV 8055 PV 8065 PV 8370 ThermoJarrellAsh . . . . 8000series 8500 series 7000 series 1100 series Siemans AG . . . . . . Spectromet 100OA Spectromet 1 OOOV Spectromet 1 OOOHV Spectro . . .. . . . . Spectrotest Spectrotest Jr Spectrolab Vacuum Air Spectroil SpexIndustries . . . . 1404 1877 VEB Carl Zeiss Jena . . PG 52 0.04 0.46 0.60 or 0.30 0.69 or 0.35 0.03 or 0.46 or 0.31 As 3520 As 3520 As 3520 0.84 0.6 or 0.3 0.6 or 0.3 0.55 0.6 or 0.3 0.29or 1.15 0.55 or 0.74 0.56 0.39 0.5 0.56 0.46 0.34 or 0.68 0.42 or 1.68 0.46 0.69 0.46 0.46 0.46 0.46 - - - - 0.78 0.36 0.36 0.50 0.50 0.50 0.50 or 0.67 0.50 0.27 1.4 0.74 or 0.37 rangejnm 170-406 170-526 170-609 170-812 As 3520 As 3520 As 3520 240-450 210-590 190-295 190-440 210-590 156-880 173-767 and 766.4 174-670 170-830 170-830 200-520 190-900 170-428 170-1040 185-680 177-4 10 177-615 165-852 165-852 165-552 170-410 160-800 160-800 160-800 160-800 220-750 150-450 110-450 220-530 210-500 165-230 210-800 210-800 175-1 040 1 85- 1 000 200-2800 ~ ~~ Focal length/m 0.5 1.0 As 3520 As 3520 As 3520 0.5 1.0 1 .o 0.75 1.0 1.5 0.75 0.5 1 .o 0.75 1.5 1.0 1 .o 0.75 1 .o 1 .o 1 .o 1 .o 1 .o 1 .o 0.75 0.75 0.75 0.75 1 .o 1.0 1 .o 0.75 0.50 0.75 0.75 0.75 0.85 0.60 2.07 Type of source Foundry analyser Low-voltage spark, d.c.arc, GDL Spark As 3520 As 3520 Low-voltage spark Arc or spark; rotating disc; modular As Spectromet 1000 Spark Rotrode Various, including high repetition condensed arc, ICP, GDL, d.c. arc As E 1000 Spark, ICP, d.c. arc, GDL Spark, ICP, d.c. arc, GDL Graphite furnace incorporating low- pressure discharge “Transource” (high voltage triggered discharge), low voltage triggered d.c. arc “Transource” “Transource” Universal source Monoalternance 50 Hz/ 5-500 Hz spark with high-energy conditions, intermittent d.c.arc As PV 8030 Monoalternance 5-500 Hz high-repetition spark, intermittent d.c. arc As PV 8050 50 MHz ICP, arc or spark GDL ECS spark ECS spark ECWS spark, d.c. arc, SSEA, ICP As 7000 series Floating anode, spark, arc As for lOOOA As for 1OOOA D.c. arc, portable D.c. arc, portable Spark Spark D.c. arc Various Various Arc or spark108R JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, JUNE 1987, VOL. 2 Table 2. COMMERCIALLY AVAILABLE INSTRUMENTS-continued B. Plasma Spectrometers Generators Supplier* Model Reciprocal dispersion/ nm mm-1 ( a ) The following instruments are new entries and are described in section 7- Laboratories . . . . 3410 0.42 Applied Research Perkin-Elmer . . . . ICP6500XR UV 0.40 VIS 0.80 Philips Analytical .. PU 7450 0.083 or 0.27 Thermo Jarrell Ash . . ICAP 61 - (b) The following instruments continue to be ofSered by manufacturers$- Applied Research Laboratories . . . . 3510 3520 3560 3580 Spectraspan IV Spectraspan V Spectraspan VI BairdCorporation . . PSX PSQ PST AFS E 1000 Polyvac JY 38 PI JY 38 SHR JY 38 VHR JY 48 JY 70 Hilger Analytical . . E 984 Polyvac Jobin-Yvon . . . . JY32P (combination of any JY 38 + JY 32) JY 38 Plus Kontron . . . . . . Plasmakonl5 Labtam . . . . . . 8410 Plasmakon 135 Labtest . . . . . . Plasmatest75 Leeman Labs . , . . Plasma Spec Perkin-Elmer . . . . ICP6500 Plasma I1 Philips Analytical . . PV 8060 PV 8065 Sciex . . . . . . Elan Sopra . . . . . . DPS1500 Spectro Analytical . . Spectroflame and ICP 5500B SpexIndustries .. . . 1870 1702 1704 1269 Thermo Jarrell Ash . . Plasma 300 I CAP -900 ICAP-1100 VGIsotopes . . . . PlasmaQuad 0.65 or 0.32 0.93 or 0.46 or 0.31 0.93 or 0.46 or 0.31 0.93 or 0.46 or 0.31 0.06-0.27 As IV As IV 0.37 or 0.74 0.41-1.24 0.22-0.66 - 0.55-0.74 0.27-1.15 0.56 0.4 0.4 (1st order) 0.28 (1st order) 0.39 - (0 * 4) (0.56) 0.4 (0.2 in second order) 0.6 0.6 or 0.5 0.74 or 0.37 (second order) 0.62 0.083 (200 nm) 0.27 (800 nm) UV 0.65, visible 1.3 0.229 or 0.527 0.46 0.46 Focal length/m 1 .o 0.4 0.7 0.75 1.0 1 .o 1 .o 1 .o 0.75 As IV As IV 0.75 0.75 1.0 0.75 1.5 0.5 1.0 1 .o 1.0 1.0 1.0 - 1.0 0.6 0.6 or 0.75 0.75 0.75 - - 0.4 2 x l m 1 1 Quadrupole mass spectrometer 0.08 (300 nm) 1.5 0.25 0.33 0.50 0.67 1.6 1.1 0.8 0.65 0.5 0.4 0.4 0.75 0.5 0.75 1.0 1.26 0.33 0.75 0.75 Quadrupole mass spectrometer output power/kW 0.6-0.7 2.0 2.5 2.5 0.90-1.5 0.90-2.0 0.90-2.0 0.90-2.0 - - - 1.0 1.0 1.5 1.0 2.5 2.5 2.3 2.3 2.3 2.3 2.3 2.3 2.3 1.5 1.5 or 3.5 2.0 2 2.5 2.0 1.8 2.0 2.0 2.5 2.0 2.5 - - - - 2.5 2.5 2.5 1.5 Operating frequency1 MHz 27.12 27.12 27.12 27.12 27.12 27.12 27.12 27.12 d.c.d.c. d.C. 40.68 40.68 40.68 40.68 27.12 27.12 40.68 40.68 40.68 40.68 40.68 40.68 40.68 27.12 27.12 27.12 40 27.12 27.12 27.12 50, spark 50, spark 27.12 50 27.12 27.12 27.12 27.12 27.12 27.12 27.12 27.12 27.12JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, JUNE 1987, VOL. 2 109R Table 2. COMMERCIALLY AVAILABLE INSTRUMENTS-continued C. Atomic Absorption Spectrometers Model (single/ Resolution/ double beam) nm Background correction type Data output Supplier* (a) The following instruments are new entries and are described in section 7- RS 232C RS 232C 2 way, IEEE RS 232C 2 way, IEEE Centronics (IEEE, RS 232C optional) Centronics (IEEE, RS 232C optional) Perkin-Elmer .. . . . . . . . . 1100 (single) 5100 (double) 0.2 0.07 D2 lamp D2 lamp or W lamp Zeeman effect 0.07 Varian Techtron . . . . . . . . . . Zeeman 5100 (double) SpectrAAlO (single) 0.2 D2 lamp SpectrAA20 (double) 0.2 D2 lamp ( 6 ) The following instruments continue to be offered by manufacturers§- Baird Corporation . . . . . . . . Alpha 1 (single) 0.1 Alpha 2 (single) 0.1 Bit parallel Alpha computer BCD (TTL levels) systems Alpha 3 (single) Alpha 4 (single) GBC 901 (single) GBC 902 (double) GBC 903 (single) Hitachi 2-6000 (double beam) 2-7000 (double beam) 2-8000 (double beam) 2280 (single) 2380 (double) 3030B (double) Zeeman 3030 (double) SP9 (single) 0.1 0.1 0.1 0.1 0.2 D2HCL D2HCL D2 lamp D2 lamp D2 lamp IEEE - 488 RS 232C RS 232C GBC Scientific Nissei Sangyo 0.09 Zeeman effect Zeeman effect 0.09 0.09 0.2 0.2 0.07 0.2 0.2 Zeeman effect D2 lamp D2 lamp D2 lamp Zeeman effect D2 lamp RS 232C RS 232C RS 232C, 2 way RS 232C, 2 way SP9 computer/ PU 9007 AA PU 9090 RS 232C Data Station, RS 232C, 2 way Perkin-Elmer .PyeUnicam . . . PU 9000 (single/double) 0.2 D2 lamp Scintrex . . . . . . . . . . . . AAZ-2 (effectively double beam) 2.2 Shimadzu . . . . . . . . . . . . AA-670 (single) 0.02 S- 11 E (single) 0.04 S-12 E (single) 0.04 Thermo Jarrell Ash . . . . . . . . Video 11 E (single) 0.04 Digital or analog IEEE RS 232C RS 232C RS 232C Zeeman effect D2 lamp Smith - Hieftje Smith - Hieftje Smith - Hieftje + D2arc Smith - Hieftje + D2 arc Smith - Hieftje + D2arc + A - B channel D2 lamp Video 12 E (double) 0.04 RS 232C RS 232C Video 22 E (2 channel double) 0.04 Varian Techtron .. . . . . . . . . SpectrAA 30 (double) 0.1 Centronics (IEEE, RS 232C optional) SpectrAA 40 (double) 0.1 VEB Carl Zeiss Jena - - . . . . . . . . AA SIN (single) AAS 3 (double and single) D2 lamp D2 lamp UVtvisible 100 mV analog &lo V analog D. Electrothermal Atomisers and Autosamplers Supplier* Model Type Control unit (a) The following instruments are new entries and are described in section 7- Baird Corporation . . . . . . Pulsar A 140 Graphite furnace Capacitive discharge. Computer controlled heating; maximum temperature 3500 "C; platform atomisation 80 samples Furnace autosampler Computer controlled robot arm;110R JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, JUNE 1987, VOL.2 Table 2, COMMERCIALLY AVAILABLE INSTRUMENTS-continued D. Electrothermal Atomisers and Autosamplers Supplier* Model Type GBC Scientific . . , . . . . . System 1000 Graphite furnace FSlOOO Flame autosampler Perkin-Elmer . . . . . AS80 Shimadzu . . . . . . . . . . ASC 60F ASC 60G ThermoJarrellAsh . . . . . . CTF188 Flame or ICP autosampler Flame autosampler Furnace autosampler Graphite furnace Autosampler ( b ) The following instruments continue to be offered by manufacturersy- BairdCorporation . . . . . . A170 Graphite rod Perkin-Elmer . . . . . . . . XGA-300 Graphite furnace HGA-400 HGA-500 HGA-600 AS-40 AS-50 AS-60 Graphite furnace Graphite furnace Graphite furnace Furnace autosampler Flame or ICP autosampler HGA autosampler Control unit 10-step temperature programme with ramp and hold on each step; controlled heating to 2000 "C s-1; storage of 10 methods; programmable gas selection automatic recalibration; multiple readings; programmable rinse; standard additions 3 sample trays; 35 positions for 50-ml sample tray; options for 125- or 500-ml vessels Interchangeable carousel for up to 50 samples, of up to 20-ml volume; user selection of aspiration and delay times and number of replicates Interchangeable carousel for up to 50 samples of up to 2-ml capacity analysed sequentially or in up to 9 groups; selection of injection volume and wash cycles Temperature feedback/control from 7@3000 "C; methods storage for 329 programmes; 9-stage programme + clean; air ashing on first pyrolysis stage spectrometer; aerosol deposition sampling for flame or furnace Up to 10 standards; 60 samples; Random access sampling; IEEE control; Microprocessor controlled via Programmable, dry, ash (2 stages) atomise, maximum temperature 3500 "C to 8 steps of controlled heating.Control functions programmed via keyboard: temperature, time, ramp, hold, gas flow; maximum power heating As HGA-300 but with spectrometer control functions and digital displays of temperature, time and programme status; heating rate of 2000 "C s-1 between any two temperatures controlled heating; six programmes can be stored and recalled using magnetic cards HGA-500 from spectrometer or computer standards; methods of addition, matrix modification programmable functions, carousels containing 50 sample tubes (15 ml) All autosampler functions are controlled directly from the spectrometer or external computer; operates with the HGA-600 furnace Microprocessor unit provides up As HGA-400 but with 9 steps of IEEE controlled version of Automatic insertion of up to 35 Microprocessor controlled unit;JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, JUNE 1987, VOL.2 111R Table 2. COMMERCIALLY AVAILABLE INSTRUMENTS-continued Type Control unit Supplier* Model Pye Unicam . . . . . . . . Shim adzu Video furnace Graphite furnace SP-9 furnace Graphite furnace SP-9 furnace autosampler Autosampler . . . . . GFA4A ThermoJarrellAsh .. . . . . 755 FASTAC I1 VarianTechtron . . . . . . GTA-95 PSC-55 GTA-96 PSC-56 Graphite furnace Graphite furnace Flame or furnace autosampler Graphite furnace Autosampler Flame autosampler Graphite furnace Autosampler Microprocessor control of 6 phases and temperatures to 3000 "C; voltage or temperature control; 18 ramp rates, 9 linear, 2-2000 "C s-1 and 9 exponential; non-volatile storage of 10 programmes. TPC and solid sampling cuvettes optional 3000 "C; voltage or temperature control; 9 ramp rates 2-2000 "C s-1; digital parameter selection and display. TPC and solid sampling cuvettes optional Automatic sampler takes 35 samples and 2 wash positions; identifies blanks, samples and standards; selection of number of replicates and volume for each sample. Automatic matrix modification and standard additions Programmable, dry, ash, atomise; maximum temperature 3000 "C; temperature monitor with control loop; 9 ramp steps available; can store up to 9 programmes Programmable 6 stages, ramp or step heating, auto-clean, display of actual temperature in "C; temperature feedback system timers for sample deposition; remote triggering circuitry for autozeroing and auto- calibrating the spectrometer Programmable temperature range 20-3000 "C; up to 20 temperature steps; programmable heating rate to 2000 "C s-1; heat injection from 40 to 150 "C Blank, 5 standards, 45 samples and chemical modifier; programmable from 2 to 70 p1 samples; 4 solutions can be dispensed together Microprocessor controlled auto- sampler with 5 standard and 67 sample positions; keyboard programme entry furnace for compatibility with SpectrAA range autosampler for compatibility with SpectrAA range 4 phases each programmable to Aerosol deposition; digital Updated version of GTA-95 Updated version of PSC-55 * Company addresses are given in Table 3.t Fuller descriptions of this equipment can be found in JAAS, 1986, 1, 69R. $ Fuller descriptions of this equipment can be found in JAAS, 1986, 1, 70R. 9; Fuller descriptions of this equipment can be found in JAAS, 1986, 1, 71R. 7 Fuller descriptions of this equipment can be found in JAAS, 1986, 1, 71R.112R JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, JUNE 1987, VOL. 2 Table 3. INSTRUMENT COMPANY ADDRESSES Company ARL Applied Research En Vallaire, 1024 Ecublens, Switzerland Laboratories SA Company SCIEX, 55 Glencameron Road, Thornhill, Ontario L3T IP2, Canada UWEuropean Agent Perkin-Elmer Ltd., Post Office Lane, Beaconsfield, Buckinghamshire HPO 1QH UWEuropean Agent ARL Applied Research Laboratories , Wingate House, Wingate Road, Luton, Bedfordshire LU4 8PU Baird Atomic Ltd., 4 Warner Drive, Springwood Industrial Estate, Brain tree, Essex CM7 7YL Baird Corporation, 125 Middlesex Turnpike, Bedford, MA 01730, USA Scintrex, 22 Snidercroft Road, Concord , Ontario L4K lBS, Canada Techmation Ltd., 58 Edgware Way, Edgware, Middlesex H48 8SP GBC Scientific Equipment Pty, 22 Brooklyn Avenue, Danedong, Victoria 3175, Australia Ltd, Techmation Ltd., 58 Edgware Way, Edgware, Middlesex H48 8SP Shimadzu (Europa) GmbH, Acker Strasse 11 1, D-4000 Dusseldorf 1, FRG V.A. Howe & Co. Ltd., 12-14 St. Anne’s Crescent, London SW18 2LS Hilger Analytical Ltd., Westwood, Mar gate, Kent CT9 4JL, UK Siemans A. G. , Infoservice 213-71e, Postfach 156, 8510 Furth, FRG Siemans Ltd. , Analytical Systems, Eaton Bank, Congleton, Cheshire CW12 1PH Jobin-Yvon, Division d’hstruments , 16-18 Rue du Canal, 91160 Longjumeau, France EDT Research, 14 Trading Estate Road, London NW14 7LU Spectro GmbH, Bosch Strasse 10, D-4190 Kleve, FRG Spectro Analytical UK Ltd. , Fountain House, Great Cornbow, Halesowen, West Midlands B63 3BL Kontron Instruments, Blackmoor Lane, Croxley Centre, Watford, Hertfordshire WD18XQ Kontron GmbH, PO Box 8057, Oskar-von-Miller Str. 1, 8057 Eching b. Munchen, FRG Spex Industries Inc., 3880 Park Avenue, Eddison, NJ 08820, USA Glen Creston Instruments, 16 Dalston Gardens, Stanmore, Middlesex HA7 1DA Labtam International Pty., 43 Malcolm Road, Braeside, Victoria 3195, Australia Techmation Ltd., 58 Edgware Way, Edgware, Middlesex H48 8SP Sopra, 68 Rue Pierre Joigneaux, F9 2270 Bois-Colombes, France Labtest Equipment GmbH Tal Str. 35, D4030 Ratingen, FRG Labtest Equipment Ltd., 11828 La Grange Avenue, Los Angeles, CA 90025, USA Thermo Jarrell Ash, Corporation , 590 Lincoln Street, Post Office Box 9036, Waltham, USA MA 02254-9036, Thermo Electron Ltd., Analytical Instrument Division, 830 Birchwood Boulevard, Birchwood, W arrington, Cheshire WA3 7QZ Leeman Labs Inc. , 600 Suffolk Street, Lowell, MA 01854, USA Varian Techtron Pty., Ltd. , 679-701 Springvale Road, Mulgrave, Victoria 3170, Australia Varian Associates Ltd., 28 Manor Road, Walton-on-Thames, Surrey KT12 2QK Nissei Sangyo (America) Co. 460E Middlefield Road, Mountain View, CA 94043, USA Ltd. (Hitachi), Nissei Sangyo Co. Ltd., London Road, Sutton Industrial Park, Reading, Berkshire RG6 1AZ VEB Carl Zeiss Jena, Carl Zeiss Str. 1, 6900 Jena, GDR Carl Zeiss Scientific Instruments Ltd., PO Box 43,2 Elstree Way, Boreham Wood, Hertfordshire WD6 1NH Perkin-Elmer Corporation, Spectroscopy Division, 901 Ethan Allen Highway, Ridgefield, CT 06877, USA Perkin-Elmer Ltd., Post Office Lane, Beaconsfield, Buckinghamshire HPO 1QH Philips Industrie SA, Spectrochemistry Department , 131 Boulevard de L’Europe, B-1301 W avre , Belgium Philips Analytical Department, Pye Unicam Ltd., York Street, Cambridge CB12PX VG Instruments Inc. , Inorganic Division, 300 Broad Street, Stamford, CA 06901 , USA VG Isotopes Ltd. , Ion Path, Road Three, Winsford, Cheshire CW7 3BXJOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, JUNE 1987, VOL. 2 113R LOCATION OF REFERENCES The full references cited in this Update have been published as follows: 861710-8611030, J . Anal. At. Spectrom., 1986, 1(3), 75R-85R. 8611031-8611460, J. Anal. At. Spectrom., 1986, 1(4), 107R-120R. 8611461-8611834, J. Anal. At. Spectrom., 1986, 1(5), 155R-168R. 8611835-8612039, J. Anal. At. Spectrom., 1986, 1(6), 193R-200R. 8711-871395, J . Anal. At. Spectrom.) 1987, 2( 1) , 29R-42R. 871396-871637, J. Anal. At. Spectrom., 1987, 2(3), 69R-77R. Abbreviated forms of the literature references quoted (excluding those to Conference Proceedings) are given below for the convenience of readers.The full references, names and addresses of authors and details of the Conference presentations can easily be found in the appropriate issue of JAAS cited above. Abbreviated List of References Cited in Update 861717. Anal. Chem., 1985, 57, 1048A. 861720. Anal. Chem., 1985, 57, 2311.. 861725. Fresenius 2. Anal. Chem., 1985, 321, 448. 861727. Am.Lab. (Fairfield Conn.), 1985, 17(8), 20. 861728. Anal. Chem., 1985, 57, 2229. 861729. Exp. Tech. Phys., 1985, 33, 229. 86lC786. 861970. Anal. 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ISSN:0267-9477    

DOI:10.1039/JA987020079R

出版商:RSC    

年代:1987

数据来源: RSC

摘要:

JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, JUNE 1987, VOL. 2 115R ATOMIC SPECTROMETRY UPDATE REFERENCES The address given in a reference is that of the first named author and is not necessarily the same for any co-author. 871638. 871639. 871640. 87/64 1. 871642. 87t643. 871644. 87f 645. 871646. 871647. 871648. 87/649. Hunt, D. T. E., Winnard, D. A., Appraisal of selected techniques for the determination of lead and cadmium in waters by graphite furnace atomic absorption spec- trometry, Analyst, 1986, 111, 785, (WRc Environment, Medmenham Lab., PO Box 16, Henley Rd., Medmen- ham, Marlow, Buckinghamshire SL7 2HD, UK). Uchida, T., Kojima, I., Iida, C., Goto, K., Discrete nebulisation in inductively coupled plasma atomic emis- sion spectrometry of manganese, Analyst, 1986, 111,791.(Lab. Anal. Chem., Nagoya Inst. Technol., Gokiso-cho, Showa-ku, Nagoya 466, Japan). Alvin, J. F., Gardiner, F. 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Spectrosc., 1986, 40, 877. (Dept. Chem., Northern Illinois Univ., DeKalb, IL 60115, USA).Molin Christensen, J., Kirchhoff, M., Determination of nickel, cadmium and chromium in whole blood and urine by Zeeman atomic absorption spectrophotometry, Znt. Congr. Ser.-Excerpta Med., 1986, 676, (Health Hazards Bio. Eff. Weld. Fumes Gases), 181. (Dan. Natl. Inst. Occup. Health, Hellerup, DK-2900, Denmark). Andersen, K. J., Wikshaaland, A., Utheim, A., Julshamn, K., Vik, H., Determination of silver in biological samples using graphite furnace atomic absorption spectrometry based on Zeeman-effect background correction and matrix modification, Clin. Biochem. (Ottawa), 1986, 19, 166. (Med. Dept. A, Univ. Bergen, N-5016 Bergen, Norway). Gowans, E. M. S., Fraser, C. G., Five methods for determining urinary calcium compared, Clin.Chem. (Winston-Salem, N. C . ) , 1986, 32, 1560. (Med. Sch., Ninewells Hosp., Dundee DD1 9SY, UK). Parr, R. 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T., Atomic emission sources for solution spectrochemistry, Anal. Chem., 1986, 58, 1139A. (North Am. Instrum. Div., Perkin-Elmer Corp., Norwalk, CT Faires, L. M., Fourier transforms for analytical atomic spectroscopy, Anal. Chem., 1986, 58, 1023A. (Chem. Div., Los Alamos Natl. Lab., Los Alamos, NM 87545, USA).Littlejohn, D., Ellis, H. J., Hughes, H., Atomic Spec- trometry Update+hemicals, iron, steel and non-ferrous metals, J . Anal. At. Spectrom., 1986,1,87R. (Dept. Pure Appl. Chem., Univ. Strathclyde, 295 Cathedral St., Glasgow G1 lXL, UK). RiifiEka, J., Flow injection analysis-a survey of its potential for spectroscopy, Fresenius Z . Anal. Chem., 1986, 324, 745. (Chem. Dept., Tech. Univ. Denmark, Lyngby, DK-2800, Denmark). Sneddon, J., Approaches to sample introduction in atomic spectroscopy, Spectroscopy (Springfield, Oreg.) , 1986, 1(9), 34. (California State Polytech. Univ., Pomona, CA, USA). Strasheim, A,, Approaches to multi-element analysis of metals using optical atomic spectroscopy, Fresenius 2. Anal. Chem., 1986, 324, 793. (Chem. Dept., Univ. Pretoria, Pretoria 0002, South Africa).Omenetto, N., Smith, B. W., Hart, L. P., Laser-induced fluorescence and ionisation spectroscopy: theoretical and analytical considerations for pulsed sources, Fresenius Z . Anal. Chem., 1986,324,683. (Jt. Res. Cent., IspraEstab., 1-21020 Ispra, Italy). Ebdon, L., Hill, S., Ward, R. W., Directly coupled chromatography - atomic spectroscopy. Part 1. Directly coupled gas chromatography - atomic spectroscopy. A review, Analyst, 1986, 111, 1113. (Dept. Environ. Sci., Plymouth Polytechnic, Drake Circus, Plymouth PLA 8AA, UK). GamC, I., Balabanoff, L., Valdebenito, R., Vivaldi, L., Use of a matrix modifier and L'vov platform in the determination of copper in pooled human saliva by electrothermal atomic absorption spectrometry, Analyst, 1986, 111, 1139.(Facultad de Ciencias, Departamento de Quimica, Universidad de Concepci6n, Casilla 3-C, Con- cepci6n , Chile). Anderson, R. K., Thompson, M., Culbard, E., Selective reduction of arsenic species by continuous hydride genera- tion, Analyst, 1986, 111, 1143. (Appl. Geochem. Res. Group, Dept. Geology, Imperial Coll. Sci. Technol., London SW7 2BP, UK). International Union of Pure and Applied Chemistry, Determination of manganese in biological materials, Pure Appl. Chem., 1986,58, 1307. Okutani, T., Oishi, Y., Uchida, K., Arai, N., Selective separation of trace amounts of cadmium(I1) and copper (11) ions from solution on activated carbon impregnated with 2,4,6- tris( 2-pyridy1)- 1,3,5- triazine , Nippon Kagaku Kaishi, 1986, (7), 853. (Coll. Sci. Technol., NihonUniv., Tokyo 101, Japan).06859-0905, USA). 871678. 871679. 871680. 871681. 871682. 871683. 871684. 871685. 871686. 871687. 871688. 871689. 871690. 87/69 1. Vackova, M., Smirnova, L., Kozakova, E., Atomic absorption spectrometric determination of lead and cad- mium in manganese ores and in fly-ash from their technological processing, Chem. Lkly, 1986,80,635. (Fac. Sci., Comenius Univ., Bratislava, Czechoslovakia). Matsumoto, A., Hirao, Y., Iwasaki, M., Fukuda, E., H a n d , H., Nara, S., Kimura, K., Determination of lead in environmental samples by graphite furnace AAS, Bunseki Kaguku, 1986,35,590. (Coll. Sci. Eng., Aoyama Gakuin Univ., Tokyo 157, Japan). Kharlamov, I. P., Lebedev, V. I., Persits, V. Yu., Eremina, G. V., Influence of cations and anions on the analytical signals of zinc, cadmium, lead, tin, bismuth and antimony introduced with solutions of steels and allovs ,- into eleckothermal atomisers, Zh.Anal. Khim., 1986,41, 1004. (USSR). KOMO, H., Kimura, J., Takada, K., Analysis of rhodium- base intermetallic compound, white metal and high speed steel by ICP-AES (inductively coupled plasma atomic emission spectrometry), Bunseki Kaguku, 1986, 35, T57. (Res. Inst. Iron, Steel Other Met., Tohoku Univ., Sendai 980, Japan). Inamoto, I., Turuhara, K., Uesugi, Y., Determination of microgram amounts of silicon in iron oxide for ferrite by fluoride separation - graphite furnace AAS (atomic absorption spectrometry) and Molybdenum Blue spectro- photometry, Bunseki Kugaku, 1986, 35, T67. (Res. Dev. Lab., Nippon Steel Corp., Kawasaki 211, Japan).Seckin, M. A., Aygun, S., Ataman, 0. Y., Determination and speciation of mercury in a dental work-place by cold vapour atomic absorption spectrometry and gas - liquid chromatography, Znt. J . Environ. Anal. Chem., 1986, 26, 1. (Dept. Chem., Middle East Tech. Univ., Ankara, Turkey). Torgov, V. G., Terent'eva, L. A., Afanas'eva, L. D., Extraction - atomic absorption method for joint determi- nation of arsenic and antimony in geological samples, Zzv. Sib. Otd. Akad. NaukSSSR, Ser. Khim. Nauk, 1986, (4), 116. (Inst. Neorg. Khim., Novosibirsk, USSR). Liu, J., Cai, Z., Simultaneous determination of thirty- three elements in cassiterite by atomic emission spec- trometry, Yankuang Ceshi, 1986, 5(1), 22. (Inst. Miner. Deposits Geol., China Nonferrous Met.Ind. Co., China). Li, Q., Determination of trace amounts of beryllium by atomic absorption spectrometry, Yankuang Ceshi, 1986, 5(1), 29, (Qinghai Prov. Geol. Cent. Lab., China). Xu, J., Dai, M., Adsorbability study and application of phosphorylated cellulose4etermination of ten trace ele- ments in pyrite and iron ores, Yankuang Ceshi, 1986,5(1), 48. (Exp. Cent., Hubei Prov. Bur.Geo1. Miner. Deposits, China). Geng, X., Determination of trace amounts of selenium and tellurium in ores and geochemical exploration samples by hydride generation atomic absorption spectrometry, Yan- kuang Ceshi, 1986, 5(1), 58. (Zhongnan Inst. Metall. Geol., China). Hardy, J. M., Aerosol deposition - carbon furnace atomi- sation for simultaneous multi-element atomic absorption spectrometry, J .Anal. At. Spectrom., 1986, 1, 287. (Beltsville Hum. Nutr., US Dept. Agric., Beltsville, MD 20705, USA). Janousek, I., Determination of selenium in steel by flame atomic absorption spectrometry, J . Anal. At. Spectrom., 1986, 1, 309. (Cent. Res. Inst., Skoda, 31600 Plzen, Czechoslovakia). Fan, J., Mo, X., Luo, L., Determination of manganese in tungsten and tungsten oxide by using the enhancing effect of sodium dodecyl sulphate, Zhongnan Kuangye Xueyuan Xuebao, 1986, (2), 78. (Dept. Chem., Central South Inst. Min. Technol., Changsha, China).JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, JUNE 1987, VOL. 2 117R 871692. Wu, C. I., Chang, F. C., Wang, S. J., The simultaneous determination of trace dysprosium, europium, gadolinium and samarium in nuclear grade uranium oxide by induc- tively coupled plasma atomic emission spectrometry (ICP- AES), J .Chin. Chem. SOC. (Taipei), 1986, 33(1), 35. (Nucl. Anal. Chem. Cent., Inst. Nucl. Energy Res., Taiwan). Aihara, M., Tanaka, E., Atomic absorption spectrometry as a chromatography detector. 11. Determination of polyaminopolycarboxylic acids, Fukuoka Joshi Diagaku Kaseigakubu Kiyo, 1986, 17, 11. (Fac. Home Life Sci., Fukuoka Women’s Univ., Fukuoka 813, Japan). Papers 871C694-871C854 were presented at the 13th Annual Meeting of the Federation of Analytical Chemistry and Spectroscopy Societies, St. Louis, MO, USA, September 28th-October 3rd, 1986. 871693. 87lC694. 87lC695. 871C696. 87lC697. 871C698. 87lC699. 87lC700. 871C701. 87lC702. 87x703. 87lC704. 87lC705. 871C706.87lC707. Olesik, J. W ., Fundamental studies of inductively coupled plasmas: a multidimensional approach, (Dept. Chem., Venable and Kenan Lab., Univ. North Carolina, Chapel Hill, NC 27514, USA). Michlewicz, K.’G., Carnahan, J. W., A moderate power He-MIP as a selective detector for aqueous halides with liquid chromatography, (Dept. Chem., Northern Illinois Univ., DeKalb, IL 60115, USA). Mohamad, A. H., Caruso, J. A., Determination and elemental ratios for dioxins using capillary-GC with microwave-induced plasma detection, (Dept. Chem., Univ. Cincinnati, Cincinnati, OH 45221-0172, USA). Dominski, P. C., Hockman, A. J., Scypinski, S., Analysis of cisplatin in biological fluid by LC-AAS, (Varian Instrument Group, 25 Hanover Rd., Florham Park, NJ 07932, USA). McClendon, E., Koirtyohann, S.R., Improved fluorine detection by GC-MIP, (Univ. Missouri, Columbia, MO 65211, USA). Allen, G. M., Coleman, D. M., Dual inductively coupled plasma atomic emission spectroscopy-characterisation and assessment of segregated sampling and excitation, (Wayne State Univ., Dept. Chem., 175, Detroit, MI 48202, USA). Weiss, A. D., Boss, C. B., Metal oxide dissociation in tandem flame atomic spectroscopy, (Dept. Chem., Box 8204, North Carolina State Univ., Raleigh, NC 27695- 8204, USA). Goode, S. R., Creech, R. R., Kimbrough, L. K., Napthali, J., Instrumentation and data handling for fundamental measurements in spectroscopic plasmas, (Dept. Chem., Univ. South Carolina, Columbia, SC 29208, USA). Winn, D. H., Koropchak, J. A., Fundamental characteris- tics of thermospray sample introduction for ICP-AES, (Dept. Chem.and Biochem., Southern Illinois Univ., Carbondale, IL 62901, USA). McGeorge, S., Moak, H., Marra, S., Signal acquisition considerations for photodiode array based spectrometer systems, (PRA International Inc., 45 Meg Drive, London, Ontario N6E 2V2, Canada). McGeorge, S., Moak, H., Marra, S., The spectrometric performance of the “Plasmarray” spectrometer system, (PRA International Inc., 45 Meg Drive, London, Ontario N6E 2V2, Canada). Rayson, G. D., Herrenbruck, K., Hieftje, G. M., Electros- tatic nebulisation within a graphite furnace for sample introduction into an ICP, (New Mexico State Univ., Dept. Chem., Las Cruces, NM 88003, USA). Pak, Y., Koirtyohann, S. R., Non-metal excitations in a moderate power He-MIP, (Dept.Chem., Univ. Missouri, Columbia, MO 65201, USA). David, P. A., Galante, L. J., Hieftje, G. M., Luffer, D. R., Novotny, M. V., Selby, M., Evaluation of a surface-wave sustained plasma (Surfatron) as an element-specific detec- tor for supercritical fluid chromatography, (Dept. Chem., Indiana Univ., Bloomington, IN 47405, USA). 871C708. 87lC709. 87lC7 871C7 871C7 87lC7 87lC7 0. 1. 2. 3. 4. 87lC715. 871C716. 87lC717. 87lC7 1 8. 87lC719. 87lC720. 871C721. 87lC722. 87lC723. 87lC724. 87lC725. 87lC726. Tyson, J., Evaluation of conventional calibration strate- gies and some unconventional alternatives, (Dept. Chem., Univ. Technol., Loughborough, Leicestershire LEll 3TU, UK). van der PIS, P. S. C., de Galan, L., van Dalen, H. P. J., Kornblum, G. R., The use of strongly curved calibration graphs in flame atomic absorption spectrometry, (Labora- torium voor Analytische Scheikunde, de Vries van Heyst- plantsoen 2, 2628 RZ Delft, The Netherlands).Barnett, W. B., Calibration for atomic absorption, (Per- kin-Elmer Corp., 761 Main Ave., Norwalk, CT 06859- 0906, USA). Watters, R. L., Jr., Spiegelman, C. H., Carroll, R. J., ICP calibration over wide concentration ranges, (Cent. Anal. Chem., National Bureau of Standards, Gaithersburg, MD 20899, USA). Boss, C. B., Gentry, J. S., Effects of self-absorption on DCP working curves, (Dept. Chem., N.C. State Univ., Box 8204, Raleigh, NC 27695-8204, USA). O’Haver, T. C., Kindervater, J., Calibration by curve- fitting in the wavelength domain, (Dept. Chem., Univ. of Maryland, College Park, MD 20742, USA).Lindahl, P. C., Huff, E. A,, Fox, I. M., Determining major and minor elements in coal ash-AA or ICP?, (Anal. Chem. Lab,, Chem. Technol. Div., Argonne Natl. Lab., 9700 S. Cass Ave., Argonne, IL 60439, USA). Conrad, V. B., Determination of trace elements in coal and coal ash by graphite furnace atomic absorption spectrometry, (Conoco Coal Res. Div., 4000 Brownsville Rd., Library, PA 15129, USA). Roychowdhury, S. B., Koropchak, J. A., Trace element analysis of organic extracts of coal by ICP-AES, (Dept. Chem. and Biochem., Southern Illinois Univ., Carbon- dale, IL 62901, USA). Nygaard, D. D., Sotera, J. J., Analysing “impossible” solvents by ICP emission spectrometry, (Allied Analytical Systems, 590 Lincoln St., Waltham, MA 02254, USA).Olesik, J. W., Den, S.-J., Williamsen, E., Supercritical fluid sample introduction for ICP atomic spectrometry, (Dept. Chem., Venable and Kenan Lab., Univ. North Carolina, Chapel Hill, NC 27514, USA). Epler, K., Epstein, M. S., Koch, W. F., O’Haver, T. C., Improving the accuracy and sensitivity of atomic spectro- scopic methods using ion chromatography, (Natl. Bureau of Standards, Chem. Building, Room B-222, Gaithers- burg, MD 20899, USA). Beckwith, P. M., Mullins, R. L., Coleman, D. M., Analysis of coal fly ash using separated sampling and excitation atomic emission spectroscopy, (Detroit Edison Co., 6100 W. Warren, Detroit, MI 48210, USA). Michlewicz, K. G., Gehlhausen, J., Carnahan, J. W., Aqueous sample introduction for metals and nonmetals with a He-MIP, (Dept.Chem., Northern Illinois Univ., DeKalb, IL 60115, USA). Evans, S. J., Applications of ultrasonic nebulisation to plasma spectrometry, (Baird Corp., 125 Middlesex Turn- pike, Bedford, MA 01730, USA). Stec, R. J., Koirtyohann, S. R., On-line pre-concentration of trace elements in aqueous solutions by osmosis, (Dept. Chem., Univ. Missouri, Columbia, MO 65211, USA). Ottaway, J. M., Absorption or emission with graphite furnaces, (Dept. Pure and Appl. Chem., Univ. Strathclyde, 295 Cathedral St., Glasgow G1 lXL, UK). Lundberg, E., Baxter, D., Frech, W., Optimisation of a graphite furnace atomic emission spectrometry system, (Dept. Anal. Chem., Univ. UmeA, S-901 87 UmeH, Sweden). Falk, H., Recent developments in the FANES technique, (Central Inst. Optics and Spectrosc., Acad.Sci., GDR, 1199 Berlin-Adlershof, Rudower Chaussee 5, GDR).118R 87lC727. 871C728. 871C729. 871C730. 87lC731. 871C732. 87lC733. 871C734. 87lC735. 87lC736. 87lC737. 87lC738. 87lC739. 871C740. 87lC741. 871C742. 87/C743. JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, JUNE 1987, VOL. 2 Baxter, D., Frech, W., Lundberg, E., Determination of aluminium in biological materials by constant-temperature graphite furnace atomic emission spectrometry, (Dept. Anal. Chem., Univ. Umei, S-901 87 Urnel, Sweden). Cook, S., Littlejohn, D., Ottaway, J. M., Fell, G. S., Low-resolution monochromator system for electrothermal atomic emission spectrometry with computer controlled background correction, (Dept. Pure and Appl. Chem., Univ. Strathclyde, 295 Cathedral St., Glasgow G1 lXL, UK) .Bernhard, A. E., Piepmeier, E. H., Kim, H. J., A new look at atomic absorption spectrometry using direct solids atomisation, (ANALYTE Corp., 611 SE “L” St., Grants Pass, OR 97526, USA). Routh, M. W., Liddell, P. R., Effect of sampling frequency on analytical accuracy in GFAAS, (Applied Research Laboratories, 9545 Wentworth St., Sunland, CA 91040, USA). Slavin, W., Modern experiences with Zeeman corrected furnace AAS, (Perkin-Elmer Corp., 901 Ethan Allen Hwy., Ridgefield, CT 06877, USA). Ottaway, J. M., Littlejohn, D., Marshall, J., Carroll, J., O’Haver, T. C., Accuracy of wavelength modulation background correction in atomic absorption spectrometry, (Dept. Pure and Appl. Chem., Univ. Strathclyde, 295 Cathedral St., Glasgow G1 lXL, UK). Steele, A.W., Hieftje, G. M., A detailed study of noise sources in selective line modulation atomic spectrometry, (Dept. Chem., Indiana Univ., Bloomington, IN 47405, USA). Leighty, D. A., Murphy, L. C., Application of Smith - Hieftje background correction to flame AAS, (Allied Analytical Systems, 590 Lincoln St., Waltham, MA 02254, USA). van der Plas, P. S. C., Uitbeyerse, E., de Galan, L., The use of a photodiode array for automated background correction in ICP-AES, (Laboratorium voor Analytische Scheikunde, de Vries van Heystplantsoen 2, 2628 RZ, Delft, The Netherlands), Smith, S. B., Jr., Sainz, M. A., Schleicher, R. G., Background correction techniques in emission spectro- scopy, (Allied Analytical Systems, 590 Lincoln St., Wal- tham, MA 02254, USA). McLaren, J. W., Beauchemin, D., Berman, S.S., Calibra- tion strategies for analysis of marine sediments by ICP- MS, (Anal. Chem. Section, Chem. Div., Natl. Res. Council of Canada, Ottawa, Ontario K1A OR9, Canada). Beauchemin, D., McLaren, J. W., Berman, S. S., Applica- tion of ICP-MS to the analysis of a river water reference material, (Anal. Chem. Section, Chem. Div., Natl. Res. Council of Canada, Ottawa, Ontario K1A OR9, Canada). Gray, A. L., Date, A. R., The reduction of spectroscopic interferences from polyatomic ions in ICP-MS, (Dept. Chem., Univ. Surrey, Guildford, Surrey GU2 5XH, UK). Gregoire, D. C., Ion sampling effects in inductively coupled plasma mass spectrometry, (Geological Survey of Canada, 601 Booth St., Ottawa, Ontario K1A OE8, Canada). Vickers, G. H., Wilson, D.A., Hieftje, G. M., The detection of negative ions by ICP-MS, (Dept. Chem., Indiana Univ., Bloomington, IN 47405, USA). Wilson, D. A., Vickers, G. H., Hieftje, G. M., Spatial profiling of ions in the inductively coupled plasma by mass spectrometry, (Dept. Chem., Indiana Univ., Blooming- ton, IN 47405, USA). Satzger, R. D., Fricke, F. L., Brown, P. G., Caruso, J. A., A microwave induced plasma as an ion source for plasma MS, (Elemental Analysis Res. Cent., USFDA, Cincinnati, OH 45202. USA). 871C744. 87lC745. 871C746. 87lC747. 87lC748. 87lC749. 871C750. 87lC75 1. 87lC752. 87lC753. 871C754. 87lC755. 871C756. 87lC757. 87lC758. 87lC759. Fulford, J. E., Gillson, G. R., Douglas, D. J., Fundamental characteristics affecting routine analysis by ICP-MS, (SCIEX, 55 Glen Cameron Rd., Thornhill, Ontario L3T IP2, Canada).Dabeka, R. W., Lacroix, G., A matrix modifier for graphite furnace atomic absorption spectrometric determi- nation of arsenic in food-derived matrices, (Food Res. Div., Food Directorate, Health Protection Branch, Health and Welfare Canada, Ottawa, Ontario K1A OL2, Canada). Beach, L. M., Graphite furnace AA: new approaches to matrix modification, (Varian Instrument Group, AARC, 205 W. Touhy Ave., Park Ridge, IL 60068, USA). Vollkopf, U., Baasner, J., Grobenski, Z., Huber, B., Data handling in atomic absorption spectrometry, (Bodenseewerk Perkin-Elmer & Co. GmbH, PO Box 1120, D-7770 Uberlingen, FRG). Giddings, R. C., Carnrick, G. R., Barnett, W. B., New approaches to automation for atomic absorption spectro- scopy, (Perkin-Elmer Corp., 761 Main Ave., Norwalk, CT Delles, F., Hoobin, D., Computer enhanced automatic methods development in atomic absorption spectrometry, (Varian Instrument Group, AARC, 205 W.Touhy Ave., Park Ridge, IL 60068, USA). Abdallah, A. M., El-Sherif, M. A., El-Defrawy, M. M., Elbester, S. F., Pre-concentration and atomic absorption determination of lead, zinc, copper and cadmium in urinary excretion of auto workers, (Dept. of Community Medicine, Fac. of Medicine, Univ. Mansoura, PO Box 30, Mansoura, Egypt). Welz, B., Curtius, A. J., Schlemmer, G., Determination of phosphorus using graphite furnace AAS, (Dept. Appl. Res., Bodenseewerk Perkin-Elmer & Co. GmbH, D-7770 Uberlingen, FRG). 06859-0906, USA). Ericson, S. P., McHalsky, M. L., Jaselskis, B., Molybde- num determinations in serum using graphite furnace atomic absorption, (Travenol Laboratories, 6301 Lincoln Ave., Morton Grove, IL 60053, USA).White, J. S., Scheeline, A., Theta pinch as a sampling and excitation source for atomic emission spectroscopy, (Sch. of Chem. Sci., Univ. Illinois, 1209 W. California St., Urbana, IL 61801, USA). Goldberg, J., Carney, K., Allston, R., Imploding thin film plasma sources for atomic spectrometry, (Dept. Chem., Univ. Vermont, Burlington, VT 05405, USA). Sacks, R., Brewer, S., Jr., Albers, D., Direct determina- tion of metallic elements in powder samples with a magnetically confined, electrically vaporised thin film plasma, (Dept. Chem., Univ. Michigan, Ann Arbor, MI 48109, USA). Archontaki, H. A., Crouch, S. R., Laser-induced break- down spectroscopy for the analysis of solutions, (Dept.Chem., Michigan State Univ., East Lansing, MI 48824, USA). Piepmeier, E. H., Lee, G. H., Shields, J. P., McGuire, J. A., Lacock, R. G., Improved multielectrode D.C. plasma sources for atomic spectroscopy, (Dept. Chem., Oregon State Univ., Corvallis, OR 97331, USA). Guecheva, M., Analysis of spruce needles by use of ICP spectroscopy, (Swiss Federal Inst. Forestry Res., CH-8903 Birmensdorf, Switzerland). Bradshaw, D. K., The analysis of arsenic in sea water using the stabilised temperature platform furnace and Zeeman background correction, (Central Chemical Lab., Florida Power Corp., PO Drawer 1090, Crystal River, FL 32629, IJSA).JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, JUNE 1987, VOL.2 119R 871C760. 87lC761. 87lC762. 871C763. 87lC764. 87lC765. 87lC766. 871C767. 87lC768. 87lC769. 87lC770. 87/C771. 87lC772. 87lC773. 87lC774. 87lC775. 87lC776. Colina de Vargas, M., Romero, R. A., Mercury determina- tion in marine samples by cold vapour atomic absorption spectroscopy, (Laboratorio de Instrumentacih Analitica, Facultad Experimental de Ciencias, Universidad del Zulia, Maracaibo, Zulia 4011, Venezuela). Navarro, J. A., Parra, 0. E., *Romero, R. A., Aluminium analysis in whole blood and dialysis solutions by flameless atomic absorption spectroscopy, (Laboratorio de Instrumentaci6n Analitica, Facultad Experimental de Ciencias, Universidad del Zulia, Marcaibo, Zulia 4011, Venezuela). Kinsey, W. J., Automated solution handling systems coupled to direct current plasma emission spectrometers, (Beckman Instruments Inc., 2500 Harbor Blvd., Fuller- ton, CA 92634, USA).Watson, P. S., Kinsey, W. J., DCP-AES analysis of nutritional formula, (Beckman Instruments Inc., 5810 Hillcroft, Houston, TX 77036, USA). Meranger, J. C., Lo, B., Dissolution rates of Cu, Pb, Cd and Zn from copper and galvanised pipes using a recircu- lating system, (Natl. Health and Welfare, Environmental Health Directorate, Ottawa, Ontario K1A OL2, Canada). Bradley, C., Viscomi, A. S., Carnahan, J. W., Oxygen selective detection for gas chromatography with a helium microwave induced plasma, (Amoco Corporation, PO Box 400. Naperville, IL 60566, USA). Bray, J. T., Waymer, R. C., Williams, R. T., Ryan, P. J., Merrill, R. H., Element analysis of cell populations utilising X-ray fluorescence spectrometry, (School of Medicine, East Carolina Univ., Greenville, NC 27834, USA).Koons, R. D., Fiedler, C., Rawalt, R. C., Discrimination between sources of glass fragments using elemental composition, (FBI Lab., Forensic Sci. Res. Group, FBI Acad., Quantico, VA 22135, USA). Martin, C., Williams, J. C., Total selenium in biologicals by GFAAS with matrix modification, (Dept. Chem., Memphis State Univ., Memphis, TN 38152, USA). McDonald, J. T., Williams, J. C., Williams, J. C., Jr., The determination of sodium and potassium in microsamples of renal fluids by spark emission spectroscopy, (Dept. Chem., Memphis State Univ., Memphis, TN 38152, USA). Davis, R. L., Ryu, J.-Y., Williams, J. C., Williams, J. C., Jr., Microanalysis with a water cooled hollow cathode device in biological samples, (Dept.Chem., Memphis State Univ., Memphis, TN 38152, USA). Alendt, G., Montgomery, J., Bazzi, A., Indirect atomic absorption and voltammetric determination of caffeine, (Dept. Natural Sci., Univ. Michigan-Dearborn, Dear- born, MI 48128, USA). Burns, B. A., Boss, C. B., Dielectric probe sleeves: HELP (high efficiency low power) for the MIP, (Dept. Chem., Box 8204, North Carolina State Univ., Raleigh, NC Crowe, A. T., Deavor, J. P., Trace metals in Charleston, SC, waters by graphite furnace atomic absorption, (Dept. Chem., The College of Charleston, Charleston, SC 29424, USA). Blades, M. W., Walker, Z. H., Caughlin, B. L., Burton, L. L., Application of excited state level population measure- ments to the study of excitation mechanisms in the ICP, (Dept.Chem., Univ. British Columbia, Vancouver, BC V6T 1Y6, Canada). Seliskar, C. J., Chemical and energy transfer processes in a helium ICP, (Dept. 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W., Separation and pre-concentration of heavy metals in environmental sam- ples by nicotinium molybdophosphate resin, Bull. Envi- ron. Contum. Toxicol., 1986, 36, 924. (Dept. Chem., Makerere Univ., Kampala, Uganda). Terashima, S., Determination of trace elements in rocks and minerals by atomic absorption spectrometry, Bunseki, 1986, (l), 34. (Geol. Survey of Japan, Tsukuba, Ibaraki 305, Japan). Meddings, B., Anderson, H., Kaiser, H., Ng, R., Design and use of a high-precision, low-operating cost nebuliser - torch system for ICP analysis, S. Afr. J. Chem., 1986, 39(1), 1. (Res. Centre, Sherritt Gordon Mines Ltd., Fort Saskatchewan, Alberta T8L 2P2, Canada). Hall, G.E. M., Pelchat, J.-C., Determination of boron and other refractory elements in geological materials by inductively coupled plasma emission spectrometry, Pap. - Geol. Surv. Can., 1986, 86-1A, 89. (Geol. Survey of Canada, 601 Booth St., Ottawa, Ontario K1A OE8, Canada). Drobyshev, A. I., Turkin, Yu. I., Yakimova, N. 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M., Pelchat, J.-C., Inductively coupled plasma emission spectrometric determination of boron and other 0x0-anion forming elements in geological materials, Analyst, 1986, 111, 1255. (Geol. Survey of Canada, 601 Booth St., Ottawa, Ontario K1A OE8, Canada). Dovofeev, V.S., Sensitivity of laser-source spectrometric methods of analysis in determination of trace elements in various substances, Zh. Anal. Khim., 1986, 41, 411. (All-Union Sci. Res. Inst. Phytopathol, Golitsyno, Mos- cow, USSR). 871976. Galli, P., Magistrell, C., Recent instrumental develop- ments in the background correction systems for flame and furnace atomic absorption, Chem. Ecol., 1986, 2, 195. (Instrum. Lab.-Milano, 20128 Milan, Italy). Oreshkh, V. N., Malofeeva, G. I., Vnukovskaya, G. L., Petrukhin, 0. M., Belyaev, Yu. I., ZOlotov, Yu. A., Sorption - atomic absorption determination of cadmium and lead in natural water, Zh. Anal. Khim., 1986,41,481. (V. I. Vernadskii Inst. Geochem. and Anal. Chem., Acad. Sci. USSR, Moscow, USSR).871977. 87IC978. 87lC979. 87lC980. 87lC981. 871C982. 871C983. 87lC984. 871C985, 87lC986. 871C987. 87lC988. 87lC989. 87lC990. 87lC991. Papers 871C978-87fC1164 were presented at Analytiktreffen 1986 and IX CANAS, Neubrandenburg, GDR, 15th-19th September, 1986. Matschat, R., Borchert, H., Findeisen, B., Gadow, P., Klewe, M., Analytik an hochgereinigten Spektralkohlen fur die OES, (Akademie der Wissenschaften der DDR, Zentralinstitut fur physikalische Chemie, Berlin, GDR) . Adeberg, V., Hinz, R., Kirsch, D., Einsatz eines stabili- sierten Gleichstrombogens zur Bestimmung hoher und niedriger Elernentkonzentrationen, (Kombinat VEB Che- mische Werke Buna, Schkopau, GDR). Bombach, H., Weinhold, E., Der Einsatz der Hydrid-AAS in der metallurgischen Analytik, (Bergakademie Freiberg, Sektion Metallurgie und Werkstofftechnik, Freiberg, GDR).Wrembel, H. Z., Mercury assay using RDP-AES, (Dept. Physics, Pedagogical Univ. in a p s k ul. 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Marczewski, A,, Mierzwa, J., Comparison of XRF and laser microspectral analyses of ancient bronzes, (Central Laboratory, M. Curie-Sklodowska Univ., 20-031 Lublin, Poland). Georgieva, L., Petrakiev, A., Atanasov, S., Combination between LMA with AAS and LMA with ICPs and their application for analysis of rocks and minerals, (Higher Inst. Geology and Mining, Sofia, Bulgaria). Niebergall, K., Wennrich, R., Dittrich, K., Direkte Feststoff-Multielementanalyse im Mikrobereich durch Kopplung von Laserverdampfung und ICP (Laser-ICP) , (Sektion Chemie der Karl-Mam-Univ. Leipzig, Analytisc- hes Zentrum, 7010 Leipzig, Talstr.35, GDR). Daskalova, N., Marinkovic, M., Krasnobaeva, N., Pav- IoviC, B., Possibilities of rare earths determination by atomic emission spectroscopy, (Inst. General and Inorg. Chem., Bulgarian Acad. Sci., Sofia 1040, Bulgaria). 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Miinx, M., Kirst, H., Kotewitz, R., Die Analyse von Buntmetallegierungen unter Anwendung der ICP-Spek- trometrie, (VEB Mansfeld Kombinat Wilhelm Pieck, Forschungsinstitut fur NE-Metalle Freiberg, GDR).Markova, I., Removal of the matrix effect when determin- ing noble metals in geological samples with ICP, (KNIPPI “NIPRORUDA,” Sofia, Bulgaria). Ohls, K., Dewies, J., Loepp, H., Simultane ICP-Spek- trometrie mit elektrothermischer Verdampfung Fester und Fliissiger Proben, (Hoesch Stahl AG Dortmund, Chemische Laboratorien, Dortmund, FRG). Pyrlik, H., Slickers, K., Analyse von Fliissigkeiten mit Spectroflame-ICP, (Spectro Analytical Instruments GmbH, D-4190 Kleve, FRG). VecsernyCs, L., Determination of trace impurities in gold electroplating bath with a DCP radiation source, (Res. Inst. Telecommunication, Budapest, Hungary). Catasus Portuondo, M. R., Petrov, A. A., Alvarez, A., A general criteria for the selection of auxiliary signals when correlation relationships are used in emission spectral analysis, (Univ.Havana, Fac. Chem., Havana, Cuba).JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, JUNE 1987, VOL. 2 127R 87/C1025. Mikkeleit, W., Singer, R., Hofmann, Ch., Dressler, B., Danzer, K., Halbquantitative emissionsspektrographische Spurenbestimmung in Oxiden auf Grundlage des Harvey- Verfahrens, (Friedrich-Schiller-Univ., Sektion Chemie, Jena, GDR). 87/C1026. Wysocka-Lisek, I., Some remarks on MnC12 applicability as an internal standard in the spectrographic REE analysis, (M. Curie-Sklodowska Univ., Inst. Chem., PI. M. Curie- Sklodowska 2, 20-031 Lublin, Poland). 87/C 87/C 027. Jaxa-Bykowski, W., Spectrochemical determination of contaminations in high purity calcium phosphate, (Res.Develop. Cent. , Polam, Warsaw, Poland). 028. Luft, B., Zimmermann, R., Eckstein, H.-J., Quantitative spektrographische Analyse von elektrochemisch isolierten ausscheidungen mikrolegierter Baustahle, (Bergakademie Freiberg, GDR). 87/C1029. Paszkowska, B., Comparison of usefulness of tantalum and titanium electrodes in the spectrographic determina- tion heavy rare earth elements, (M. Curie-Sktodowska Univ., Inst. Chem., P1. M. Curie-SkYodowska 2, 20-031 Lublin, Poland). 87/C1030. Sulewa, A., Brakalow, L., Chaladjowa, Z., Atomemis- sionsanalyse von Eisen- und Titanverunreinigungen in Schlickern der Porzellanherstellung, (Hochschule fur che- mische Technologie, Sofia, Bulgaria). 87/C1031. Dmowska, G., Kowalska, E., Spektrographische Untersu- chung biologischer Stoffe auf Zinngehalt und andere chemische Elernente, (OSrodek Badawczo-Rozwojowy Elektroniki Prbzniowej , Zaklad Badan Fizykochem- icznych, Warsaw, Poland). 87/C1032.Mauser, K. E., Miiller, L., Neue Einsatzmoglichkeiten der Rontgenfluoreszenzanalyse mit Sequenzspektrometern, (Siemens AG, Analysentechnik D-7500 Karlsruhe, FRG) . 87/C1033. Piatek, K., Die Rolle der Hilfselektrode in der Spektrala- nalyse von Kupferlegierungen, (Institut Metali Nieze- laznych, Poland). 871C1034. Meray, L., Study of the processes affecting the determina- tion of surface contaminations with isotope induced XRF method, (Univ. Chemical Engineering, Dept. of Radio- chem. and Phys., VeszprCm, Hungary). 87/C1035. Hlavay, J., Antal, L., Karpati, J., Mineralogical and metal content analysis of respirable dust samples, (Inst.Anal. Chem., Univ. Chemical Engineering, VeszprCm, Hun- 87IC1036. Karaiwanowa, E., Tschotschov, S., Rontgenfluoreszenza- nalyse von Feststoffen im Schwarzmeeresgewasser , (Geol- ogischer Betrieb fur Laborforschung, Sofia, Bulgaria). 87K1037. Rossiger, V., Naherungsverfahren zur Behandlung der Interelementanregung bei der Rontgenfluoreszenza- nalyse, (Zentralinstitut fur Isotopen- und Strahlenforsc- hung der AdW der DDR, Leipzig, GDR). gary). 871C1038. Stankiewicz, W., Matusiak, H., Problem of chlorine determination in copper - and zinc - lead materials using XRF method, (Inst. Non-Ferrous Metals, Anal. Chem. Dept., Gliewice, Poland). 871C1039. Buhl, F., Klima, Z., Rontgenfluorimetrische Bestimmung von Quecksilberspuren in Abwassern nach Anreicherung durch Falungsaustauschreaktion, (Schlesisches Universi- tat, Chemisches Institut, GDR).87/C1040. Eggert, F., Scholz, W., Eine einfache und leistungsfahige Methode zur Entfaltung Uberlagerter Linien fur die energiedispersive Rontgen spektrometrie, (Akademie der Wissenschaften der DDR, Zentrum f. wiss. Geratebau, 1190 Berlin, Schnellerstr. 138, GDR). 87/ClO41. Thieme, H., Einsatz der energiedispersiven Rontgenfl u- oreszenzanalyse zur Beurteilung von Schussverletzungen, (Zentrales Expertisenlabor, Berlin, GDR). 87/C1042. Kowalczyk, J., Application of LiB02 flux for EDXRF analysis of zirconia concentrates, (Tech. Univ. Wrodaw , Inst. Inorg. Chem. and Metallurgy of Rare Elements, Wrochw, Poland).87K1043. Ehrhardt, H., Sanner, G., Krippendorf, C., Partzscht, H., Kandler, A., Uber Moglichkeiten zur Verminderung des Einflusses von Linien-koinzidenzen in der RFA Mittels Analysatorkristallauswahl, (VEB Mansfeld Kombinat, Forschungsinstitut fur NE-Metalle Freiberg, GDR). 87/C1044. Dostal, K.-P., Rossiger, V., Bestimmung der Spektral- dichte von Rontgenrohren aus Rontgenfluoreszenz-Aus- beutemessungen, (Zentralinstitut fur Isotopen- und Strah- lenforschung der AdW der DDR, Leipzig, GDR). 87/C1045. Sanner, G., Kandler, A., Ehrhardt, H., Partzscht, H., Vergleichsuntersuchungen mit rontgenrohren untersc- hiedlicher Anoden zur Messung leichter Elemente mit dem Rontgenspektrometer VRA-30, (VEB Mansfeld Kombinat Wilhelm Pieck, Forschungsinstitut fur NE- Metalle Freiberg, GDR).87/C1046. Surowska, B., Olejarski, B., Application of FWA for investigation of metallic layers, (Tech. Univ. Lublin, Dept. Mechanics and Organization, Lublin, Poland). 87/C1047. Kluge, A., Wehner, B., Thiele, C., Miersch, H., Flussig- keitisanalyse mit dem Rontgenfluoreszenzspektrometer VRA 30, (AdW der DDR, Zentralinstitut fur Festkor- perphysik und Werkstofforschung, GDR) . 87/C1048. Raeymaekers, B., Dorrine, W., Liu, X. D., Van Espen, P., Adams, F. C., Broekaert, J. A. C., Characterisation of spark erosion aerosols by automated electron probe microanalysis, (Univ. Antwerp (U.I.A.), Dept. Chem., Universiteitsplein 1, B-2610 Wilrijk, Belgium). 87/C1049. Kiessling, R., Ackermann, G., Dittrich, P., Ein Verfahren zur Probenherstellung aus minimalen Massen feinteiliger Festkorper fur die RFA, (Bergakademie Freiberg, Sektion Chemie, Freiberg, GDR).87/C1050. Stec, H., Venvendung von Fliesspapier - Kollektoren zur Abtrennung und Rontgenfluoreszenzspektrometrischen Bestimmung von Schwermetallspuren in anorganischen Rohstoffen, (Instytut Materialow Ogniotrwalych, Gliew- ice , Poland). 87/C1051. Ehrhardt, H., Sanner, G., Effektivitatserhohung bei der Praparation von Pulverproben zur Rontgenfluoreszenza- nalyse mit der Press-Technik, (VEB Mansfeld Kombinat Wilhelm Pieck, Forschungsinstitut fur NE-Metalle Freiberg, GDR). 87/C1052. Tilch, J., Zum nachweisvermogen Atomabsorptionsspek- trometrie (AAS) und laserangeregte Atomfluoreszenz (LAFS), (Zentralinstitut fur Optik und Spektroskopie der AdW der DDR, Rudower Chaussee 5, Berlin 1199, GDR).87/C1053. Markowicz, A., Quantitative analysis of particulate materials by X-ray fluorescence; potentials and limita- tions, (Inst. Phys. Nuclear Techniques, Acad. Mining and Metallurgy, Al. Mickiewicza 30, PI-30-059 Cracow, Pol- and). 87K1054. Mierzwa, J., Zyrnicki, W., Determination of rare earths in a hollow-cathode discharge, (Cent. Lab., M. Curie-Sklo- dowska Univ., 20-031 Lublin, Poland). 87K1055. Jiihrling, R., Schulze, M., Anwendung der Glimmentlad- ungsanregung bei der Entwicklung einer normalproben- reihe Schnellarbeitsstahle, (Amt fur Standardisierung, Messwesen und Warenprufung, FG Metallurgische Nor- malproben und Fertigungsmesstechnik, 3040 Magdeburg, PSF 233, GDR). 87K1056. Matschat, R., Giinther, H., OES-Multielement-Ultras- purenanalytik durch heisse Hohlkathodenentladungen an der Glimmentladungslampe nach Grimm, (Akademie der Wissenschaften der DDR, Zentralinstitut fiir phys.Chem. Berlin, GDR).128R JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, JUNE 1987, VOL. 2 87/C1057. Borkowska-Burnecka, J., Zyrnicki, W., Application of a hollow-cathode discharge to spectrochemical analysis of metals4omparison of atom and ion spectra excited in d.c. and HF hollow-cathode discharges, (Inst. Inorg. Chem. Metallurgy of Rare Elements, Techn. Univ. Wroctaw, 50-370 Wroclaw, Poland). 87/C1058. Dittrich, K., Eismann, G., Fuchs, H., Bestimmung von spuren seltener Erden durch AAS-ETA und FANES/ FINES-Technik, (Sektion Chemie der Karl-Marx-Univ. Leipzig, Analytisches Zentrum, DDR-7010 Leipzig, Talstr.35, GDR) . 87/C1059. Dittrich, K., Glaubauf, Th., Fuchs, H., Mauersberger, K., Bestimmung von Technetiumw-Spuren durch AAS-ETA und FANES (ETA), (Sektion Chemie der Karl-Marx- Univ. Leipzig, Analytisches Zentrum, DDR-7010 Leipzig, Talstr. 35, GDR). 87/C1060. Dittrich, K., Glaubauf, Th., Fuchs, H., Sychra, V., FANES mit Wolframatomisierung - ein neues Messprin- zip fur die Bestimmung carbidbildender-Elemente, (Sek- tion Chemie der Karl-Marx-Univ. Leipzig, Analytisches Zentrum, DDR-7010 Leipzig, Talstr. 35, GDR). 87/C1061. Czerwensky, M., Falk, H., Hoffmann, E., Liidke, Ch., Matschat, R., Giinther, H., Analytische Untersuchungen zur FANES-Multielement-Spuren-Analyse in einfachen Matrices (H20 , HN03, HCl), (Akademie der Wissensc- haften der DDR, Zentralinstitut fur physikalische Che- mie, Berlin, GDR).87/C1062. Henrion, G., Henrion, A., Urban, P., Clusteranalysen atomspektroskopischer Ergebnisse rnit Basic-Program- men, (Humboldt-Universitat, Sektion Chemie, Berlin, GDR) . 87/C1063. Falk, H., Hoffmann, E., Ludke, Ch., Sorge, R., Bergann, L., Skole, J., Schubert, M., Florek, S., Becker-Ross, H., Sanders, H., Tischendorf, R., Brautigam, H., Das FANES-Echellespektrometer, (Zentralinstitut fur Optik und Spektroskopie der AdW der DDR, 1199 Berlin, Rudower Chaussee 5, GDR). 87/C1064. WyciSlik, A., Neue Art der Eichung mit anwendung einer Eich-Basis in der Analyse der metallegierungen Mittels der Methode AAS , (Technische Univ., Sektion Metallur- gie, Katowice , Poland). 87/C1065. Bukowski, J., Analysis of glasses by SSMS method, (OSrodek Badawczo-Rozwojowy Elektroniki Pr6zniowej, Zaklad Badan Fizykochemicznych, Warsaw, Poland).87/C1066. Claos, E., Odinets, V., Kinetic atomic-absorption determi- nation of element traces in argillites, (Inst. Chem., Akadeemia tee 15, 200026 Tallin, Estonian SSR, USSR). 87lC1067. Sucmanova, M., Sucman, E., Zima, S., Synek, O., The determination of some trace elements in sludges, (Univ. School of Veterinary Medicine, Brno, Czechoslovakia). 87/C1068. Raue, B., Lorenz, G., Vergleichende Untersuchungen zur 87/C 87/C Bariumbestimmung mittels AAS und FES in metaliurgisc- hen Produkten, (VEB Mansfeld Kombinat Wilhelm Pieck, Forschungsinstitut fur NE-Metalle Freiberg, GDR). 069. Aneva, Z., Arpadjan, S., Alexandrov, S., Flame atomic absorption determination of microimpurities in high-pur- ity platinum, (Refinery and Petrochemical Res.Inst., 8104 Burgas, Bulgaria ). 070. Lorenz, G., Borrmann, D., Beitrage zur Silber- und Palladium-Bestimmung in Produkten der Metallurgie mit- tels Atomabsorptions- und Spektral-Photometrie, (VEB 87/C1071. Borrmann, D., Raue, B., Bestimmung von Lithium in metallurgischen Produkten mittels FES und AAS, (VEB Mansfeld Kombinat Wilhelm Pieck, Forschungsinstitut fur NE-Metalle Freiberg, GDR). 87/C1072. Chmielewska, K., Kowalczyk, E., Determination of impurities in chromates by flame atomic absorption spectrometry, (Osrodek Badawczo-Rozwojwy Elektroniki Prozniowej , Zaklad Badan Fizykochemicznych, Warsaw, Poland). 87/C1073. Schweder, P., Analytische Anwendung der Atomabsorp- tionsspektrometrie (AAS) in der agrochemischen Unter- suchung, (Institut fur Pflanzenernahrung Jena der Akade- mie der Landwirtschaftswissenschaften der DDR, Bereich ACUB, Abteilung ACUB Rostock, GDR).87lC1074. Popova, S., Djulgerova, R., Arsenova, D., Some problems of Ag atomic absorption determination in Pb - Zn concentrates, (High Inst. of Chem. Eng., ZNTL, 1156 Sofia, Bulgaria). 87/C1075. Mauersberger, K., Bayerl, B., Bestimmung von Techne- tium-99 durch FAAS, (Zentralinstitut fur Isotopen- und Strahlenforschung der AdW, Leipzig, GDR). 87/C1076. Seracu, D. I., A new interference in the determination of calcium by air - acetylene flame AAS, (Res. Inst. Sugar Beet, Sugar Manufacturing and Sweeteners, R-8264 Fun- dulea, Rumania). 871C1077. Muller, E., Bestimmung von Spurenverunreinigungen im Zinndioxid mittels FAAS nach Abtrennung der Matrix, (Zentralinstitut fur Festkorperphysik und Werkstofforsc- hung 8027 Dresden, Helmholtzstr.20, GDR). 87/C1078. Rautschke, R., Udelnow, C., Pforte, U., Atomisierungs- verhalten des Zinns bei der AAS rnit der Flamme und der Graphitrohrkuvette, (Martin-Luther-Univ., Sektion Che- mie, Halle/S, GDR) . 87/C1079. Eschke, H.-D., Griin, M., Bestimmung von Cd und Pb mittels Flammen-AAS und Einsatz eines Quarzrohres mit Langsschlitz am Atomabsorptionsspektralphotometer AAS 3, (Akademie der Landwirtschaftswissenschaften der DDR, Institut fur Pflanzenernahrung Jena, GDR). 87/C1080. Brashnarova, A., Georgieva, M., Possibilities for free of interference atomic absorption determination of calcium in plants, (N.Poushkarov Inst. Soil Sci. and Yield Prediction, Sofia 1080, Bulgaria). 87/C1081. Lakatos, I., Lakatos, J., Effect of cations on FAAS analysis of macromolecular solutions containing ionised polymers, (Res. Lab. for Mining Chem., Hungarian Acad. Sci., Miskolc-Egyetemvhros, PO Box 2, H-3515, Hun- 87/C1082. Steglich, F., Stahlberg, R., Lufter, M., Pawlik, H., Zur Genauigkeit flammenatomabsorptionsspektrometrischer Hauptkomponentenbestimmungen - Vergleich von Ein- und Zweistrahlmessungen, (VEB Robotron-Elektronik Radeberg , GDR). 87/C1083. Falk, H., Atomic spectroscopy-from King oven to FANES (furnace atomic non-thermal excitation spec- trometry), (Zentral-Institut fur Optik und Spektroskopie der Akademie der Wissenschaften der DDR, Berlin, GDR). 87/C1084. Schiittig, R., Meissner, D., Anwendung der Injektion- stechnik zur Bestimmung klinisch relevanter Spurenelemente rnit FAAS, (BKH Dresden-Friedrich- stadt , Institut fur Klinische Chemie und Laboratoriums- diagnostik, Dresden, GDR).87/C1085. Friese, K.-H., Matschiner, H., Spurenbestimmung von Mn, Cr, Pb in biologischem Material durch FAAS rnit Fliessinjektions-Probenzufiihrung, (Arbeitshygienisches Zentrum der chem. Industrie, Leuna, GDR). 871C1086. Lakatos, J., Lakatos, I., Bagdi, G., Potential of emulsions as a sample introduction technique in FAAS, (Res. Lab. for Mining Chem., Hungarian Acad. Sci., Miskolc- EgyetemvAros, PO Box 2, H-3515, Hungary). 87/C1087. Stupar, J., An improved nebuliser system for name atomic absorption spectroscopy (FAAS), (Joief Stefan Inst., E.Kardelj Univ., Jamova 39,61000 Liublijana, Yugoslavia). 87/C1088. Gruner, K., Bestimmung der Abriebwerkstoffe Fe und Cu in Hydraulikolen mittels AAS, (VEB Rohrkombinat Stahl- und Walzwerk Riesa, GDR). 87/C1089. Esser, P., Krebs, B., Kurfiirst, U., Matrixmodifikation von Feststoffproben mit Graphitpulver fur die direkte AAS-ETA-Analyse, (Anneliese Zementwerke AG, Ennigerloh, FRG). gary).JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, JUNE 1987, VOL. 2 129R 87/C1090. Martin, M.-L., Danzer, K., Zur Anvendung der Standard- Additionsmethode bei der Spurenbestimmung mittels AAS-ETA, (Friedrich-Schiller-Univ., Sektion Chemie, Jena, GDR). 87/C1091. Bezur, L., Kantor, T., Gimesi, O., Determination of trace elements in high-purity acids and organic solvents by graphite furnace AAS and ICP-AES methods, (Inst.General and Anal. Chem., Tech. Univ., Budapest, H-1521, Hungary). 87/C1092. Mohl, C., Narres, H,-D., Stoeppler, M., Direkte Bestim- mung von Spurenmetallen in biologischen und Umwelt- proben mit Graphitrohrofen-AAS, (Inst. fiir Angewandte Physikalische Chemie (ICH-4) der Kernforschungsanlage (KFA) Julich GmbH, FRG). 87/C1093. Takacs, S., Tatar, A., Concentration of copper, zinc, lead and cadmium in human organs, (Hygienic and Epidemiol- ogical Station of County Borsod, Hungary). 87/C1094. Schroter, H., Winnefeld, K., Tennigkeit, E., Weiland, G., Die quantitative Bestimmung von Aluminium in Serum und Dialysewassern, (Friedrich-Schiller-Univ., Bereich Medizin, Chirurgische Klinik, Jena, GDR). 87/C1095. Andrki, E., Tenczer, T., Zimmer, K., Spectrochemical investigations of trace element contents in several parts of human brain with different methods of sample prepara- tion, (Inst.Inorg. and Anal. Chem., L. Eotvos Univ., Budapest, Hungary). 87/C1096. Wennrich, R., Feustel, A., Dittrich, H., Vorberg, B., Untersuchungen zur Elementverteilung in menschlichen Gewebeproben mittels flammenloser AAS, (Sektion Che- mie, Karl-Marx-Univ. Leipzig, 7010 Leipzig, Talstr. 35, GDR). 87/C1097. Dittrich, K., Mohamad, I., Untersuchungen zur Verbesse- rung der Bestimmung von Bi-Spuren durch elektrother- mische Atomisierung, (Sektion Chemie der Karl-Marx- Univ. Leipzig, Analytisches Zentrum, DDR-7010 Leipzig, Talstr. 35, GDR). 87/C1098. Komhrek, J., Phlkova, I., Sommer, L., Determination of copper in body fluids by electrothermal atomic absorption spectrometry, (Dept.Anal. Chem., J. E. Purkyni: Univ., Brno, Czechoslovakia). 87/C1099. Peters, H.-J., Versieck, J., Vanballenberghe, L., Vorberg, 87/C 87/C B., de Kesel, A., Bestimmung von Mn, Cu, Zn in standardisierten Biologischen Materialien: ein Vergleich zwischen NAA und AAS, (Bereich Medizin, Karl-Marx- Univ. Leipzig, 7010 Leipzig, Talstr. 35, GDR). 100. Kollnerova, Z., Determination of Cu, Cd, Pb and V in solid portion of snow samples by AAS using graphite furnace, (Inst. Geol. and Geotechnique, Czechoslovak Acad. of Sci., Prague, Czechoslovakia). 101. Aneva, Z., Iancheva, M., Simultaneous extraction and determination of traces of lead and arsenic in petrol by electrothermal AAS, (Dept. Anal. Chem., Refinery and Petrochemical Res.Inst., Burgas, Bulgaria). 87/C1102. Lindberg, I., Frech, W., Cedergren, A., Lundberg, E., Dedina, J., Factors influencing the determination of selenium with GFAAS, (Univ. Umei, Dept. Anal. Chem., S-901 87 Umei, Sweden). 87jC1103. Preu, E., Schroter, H., Winnefeld, K., Schmidt, U., 87/C1 87/C1 Bestimmung von Mangan im Serum mittels ETA-AAS, (Medizinische Akademie, Abteilung fur Klinische Chemie und Laboratoriumsdiagnostik und Klinik fur Innere Medi- zin, Erfurt, GDR). 04. Doleial, J., Musil, J., Sychra, V., Krnak, P., Conditions for full analytical utilisation of ETA-AAS in a clean laboratory, (Dept. Tech. Phys. and Electronics, Inst. Chem. Technol., 166 28, Prague 6, Czechoslovakia). 05. Fara, M., Pospichalova, D., Spirkova, R., Petfikova, J., The effect or iron on the determination of Cu, Cr, Mn, Ni, Ti, V and Zr with WETA tungsten atomiser, (Power Res.Inst., 250 97 Prague 9, Czechoslovakia). 87/C1106. Koehler, P., Scharf, H., Matschat, R., Licht, K., Emrich, G., Abscheidung und atomspektroskopische Bestimmung partikularer Verunreinigungen in Phosphin, Arsin und Ihren Abmischungen, (AdW der DDR, Zentralinstitut fur physikalische Chemie, Berlin, GDR). 87/C1107. Heinrich, H.-J., Emrich, G., Bestimmung von Aluminium in organischen Extrakten mittels flammenloser AAS, (AdW der DDR, Zentralinstitut fur physikalische Che- mie, Berlin, GDR). 87/C1108. Dittrich, K., Glaubauf, Th., Sychra, V., Vergleichende Betrachtungen zur Anwendbarkeit von Graphitrohr - (EA 3) und Wolframrohr - (WETA 82) Atomisatoren fur nicht carbidbildende Elemente in Halbleiterproben, (Sek- tion Chemie der Karl-Marx-Univ.Leipzig, Analytisches Zentrum, DDR-7010 Leipzig, Talstr. 35, GDR). 87/C1109. Sager, M., Bestimmung von Organozinnverbindungen in Sedimenten mit AAS, (BVFA-Arsenal, Geotechnisches Institut, Vienna, Austria). 87/C1110. Findeisen, B., AAS-Plattformtechnik mit pyrokohlen- stoffbeschichtetem Rohr und Glaskohlenstoff-Plattform, (VEB Elektrokohle Lichtenberg, Berlin, GDR). 87/C1111. Hulanicki, A., Bulska, E., Effect of inorganic matrices on cadmium determination by platform atomisation in atomic absorption spectrometry, (Warsaw Univ., Fac. Chem., Warsaw, Poland). 87/C1112. Palkova, I., Coufal, O., Komarek, J., Kuban, V., The computer calculation of high temperature equilibria of copper in electrothermal atomisation processes, (J.E. Purkyne Univ., Dept. Anal. Chem., 61137 Brno, Czechos- lovakia). 87/C1113. Gadow, P., Findeisen, B., Gunther, H., Beeinflussung der 87/C 87/C 87/C Verdampfung von Matrix und Analyten in der ETA-AAS durch Einsatz eines CUP-Analysenprobentragers aus verschiedenen Materialien, (Zentralinstitut fur Elek- tronenphysik der AdW der DDR, Berlin, GDR). 114. Findeisen, B., Borchert, H., Gadow, P., Gunther, H., Matschat, R., Grenzen der Hochstreinigung von Kohlen- stoffwerkstoffen fur Zwecke der Atomspektroskopie, (VEB Elektrokohle Lichtenberg, Berlin, GDR). 115. Slovak, Z., DoEekal, B., Untersuchung von Eigenschaften von tschechoslowakischen graphitischen Materialien fur ETA, (Forschungsinstitut fur reine Chemikalien, Lachema, Brno, Czechoslovakia).116. Findeisen, B., Emrich, G., Heinrich, H. J., Einfluss verschiedener Kohlenstoffwerkstoffe als Rohrund Platt- formmaterial in der ETA-AAS, (VEB Elektrokohle Lichtenberg, Berlin, GDR). 87/C1117. Findeisen, B., Schonherr, H., Heinrich, H. J., Zum Einfluss der Reaktivitat des Kohlenstoffes bei der Alumi- nium-Bestimmung mittels ETA-AAS, (VEB Elektro- kohle Lichtenberg, Berlin, GDR). 87/C1118. Debus, H., Gross, M., Hermann, G., Scharmann, A., Seib, M., Spurenanalyse durch Spektrometrie der Koharenten optischen Vonvartsstreuung, (I. Physikalisches Institut der Justus-Liebig-Universitat D-6300 Giessen, FRG). 87/C1119. Kurfurst, U., Herber, R. F. M., Scheer, J., Longitudinale Zeeman-AAS ohne zusatzlichen Magneten mit dem Zee- man-Elektrothermalen-Atomisator (ZETA), (Fach- hochschule Fulda, Postfach 1269, 6400 Fulda, FRG).87/C1120. FIBriAn, K., Lineare und nichtlineare Eichung in der Spektrographie, (Technische Hochschule, Lehrstuhl fur Chemie, KoSice, Czechoslovakia). 87/C1121. Zimmer, K., Atomspektroskopie und Archaeologie, (L. Eotvos Universitat, Institut fur Anorganische und Analy- tische Chemie, Budapest, Hungary). 87/C1122. Bolshov, M. A,, Zybin, A. V., Koloshnikov, V. G., Smirenkina, 1. I., Trace concentration analysis by laser excited atomic fluorescence spectrometry, (Inst. Spectros. Acad. Sci., Moscow obl., Troizk, USSR).130R JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, JUNE 1987, VOL. 2 87/C1123. Khtor, T., Interpreting analytical characteristics of ther- mal dispersion methods used for sample introduction in OAS, (Inst.General and Anal. Chem., Technical Univ. of Budapest, Budapest 1521, Hungary). 87/C1124. Barnett, N. W., Evaluation of three sample introduction techniques for use with a microwave-induced plasma, (Dept. Environ. Sci. , Plymouth Polytechnic, Drake Cir- cus, Plymouth, Devon PL4 8AA, UK). 87/C1125. Ramsza, A. P., Entwicklungsperspektiven fur MIP- Losungsspektrometrie, (Inst. fur Technologie der elektro- nischen Stoffe, Warsaw, Poland). 871C1126. Rautschke, R., Probleme der Atomspektroskopie in der Umweltanalytik, (Martin-Luther-Universitat, Sektion Chemie , Halle/S . , GDR) . 87/C1127. Tschopel, P., Kollotzek, D., Tolg, G., Uber den Einsatz 87/C 87/C -. . mikrobelleninduzierter . Plasmen in der analytischen Atomspektroskopie , (Max-Planck-Institut fur Metall- forschung, Laboratorium fur Reinstoffanalytik; Bunsen- Kirchhoff-Str.13, 4600 Dortmund 1, FRG). 128. Stoeppler, M., Strategcien der Spurenmetallanalytik bei der Umweltuberwachung und im Rahmen von Umwelt- probenbanken, (Institut fur Angewandte Physikalische Chemie (ICH-4) der Kernforschungsanlage (KFA) Julich GmbH, FRG). 129. Schramel, P., DCP- und ICP-Emissionsspektroskopie in der biologischen- und umwelt-Analytik, (Gesellschaft fur Strahlen- und Umweltforschung mbH, Institut fur Okolo- gische Chemie, D-8042 Neuherberg, FRG). 87/C1130. Knapp, G., Elementanreicherung-Quo Vadis, (Institut fur Analytische Chemie, Mikro- und Radiochemie, Tech- nische Universitat Graz, Graz, Austria). 87/C1131. Gegus, E., Spektrochemische Analysenverfahren zu Spurenelementbestimmungen unter Anwendung von Anreicherungsverfahren, (Veszpr&m Universitat, Institut fur Analytische Chemie, Veszprem, Hungary).87/C1132. Meisel, A., Anwendungsmoglichketten der Photo- und Auger-Elektronenspektroskopie, (Karl-Man-Universi- tat, Sektion Chemie, Leipzig, GDR). 87/C1133. Bothe, H.-K., Neuere Entwicklungen zur Rontgenfluores- zenz-Multielementspurenanalyse mit Radionuklidanre- gung, (Zentralinstitut fur Isotopen und Strahlenforschung, Leipzig, GDR). 87/C1134. Wehner, B., Fortschritte in der energiedispersiven Ront- genfluoreszenzanalyse, (Technische Universitat, Sektion Physik, Dresden, GDR). 87/C1135. Mudrack, D., Dumecke, G., Zum Einfluss der Partikel- grosse bei der Rontgenfluoreszenzanalyse von gepulver- tem Glasmaterial, (Zentralinstitut fur Anorganische Che- mie der AdW der DDR, Bereich Analytik, GDR).871C1136. Gray, A. L., Analytical applications and matrix related interferences in ICP source mass spectrometry, (Dept. Chem., Univ. Surrey, Guildford, Surrey GU2 5XH, UK). 87/C1137. Knull, B., Neue Geratetechnische Aspekte zur Atom- Absorptions- und Emissionsspektroskopie im Kohlerohr, (Kombinat VEB Carl Zeiss JENA, Forschungszentrum, 6900 Jena, Carl-Zeiss-Strasse 1, GDR). 87lC1138. Doerffel, K., Rudolph, D., Weiterentwicklungen an zwei- elektroden-Gleichstromplasmen fur die atomemissionss- pektrometrische Spurenanalyse, (Technische Hochschule fur Chemie “Carl Schorlemmer” Merseburg, GDR). 87/C1139. Barnes, R. M., Modern developments of inductively coupled plasma from emission to mass spectrometry, (Dept.Chem., Univ. Massachusetts, GRC Towers, Amherst, MA 01003-0035, USA). 87/C1140. Pavloviir, B. V., Recent research of arc excitation sources, (Fac. Technol. and Metallurgy, Univ. Belgrade, Belgrade, Yugoslavia). 87IC1141. PISko, E., Atomspektroskopische Bestimmung seltener Erden in geologischen Proben, (Komenskg Universitat , Geologisches Institut, Bratislava, Czechoslovakia). 87/C1142. Fijdkowski, J., Modern developments in spectral detec- tion and determination of non-metallic elements, (Inst. Nuclear Chem. and Technol., Warsaw, Poland). 87/C1143. Kranz, E., Phvsikalische Eigenschaften und Unterschiede 87/C1 87/C1 87/C1 von ICP und Bogenplasmen-fur die Analytik, (Technische Hochschule Ilmenau, Abteilung Plasmatechnik, Mei- ningen , GDR) .44. Ottaway, J. M., Carroll, J., Hall, D. H., Littlejohn, D., Marshall, J., O’Haver, T. C., Computer controlled wavelength modulated instrumentation for AAS and AES, (Dept. Pure Appl. Chem., Univ. Strathclyde, 295 Cathedral St., Glasgow G1 lXL, UK). 45. Caroli, S., Analytische Anwendungen der Hohlka- thodenentladung, (Istituto Superiore di SanitA, Viale Regina Elena 299, 00161 Rome, Italy). 46. Ehrlich, G., Stahlberg, U., Ubersichtsanalyse an anorgan- ischen Festoffen - ein Vergleich von Funkenmassenspek- trographie und optischer Emissionsspektralanalyse, (Akademie der Wissenschaften der DDR, Zentralinstitut fur Festkorperphysik und Werkstofforschung Dresden, GDR). 87/C1147. Van Grieken, R., Verbueken, A., Bruynseels, F., Vande- putte, D., Goossenaerts, C., Otten, Ph., Wouters, L., Laser microprobe mass analysis (LAMMA): characteris- tics and applications, (Dept. Chem., Univ.Antwerp (UIA) B-2610 Antwerp-Wilrijk, Belgium). 871C1148. Broekaert, J. A. C., Methoden der Probenzufuhrung fur die ICP-Emissionsspektrometrie, (Institut fiir Spektroche- mie und angewandte Spektroskopie, Bunsen-Kirchoff-Str. 11, D-4600 Dortmund 1, FRG). 87/C1149. Jurczyk, J., Metallanalyse durch atomspektroskopische 87/C 87/C 87/C VerfahrerdOptische und Rontgenspektrometrie, (Eisen- forschungsinstitut, Abetilung Chemie und Umweltschutz, 44-101 Gliwice, Poland). 150. Boumans, P. W. J. M., Spektrale Storungen im ICP und spektrale Auflosung, (Philips Res. Labs., Postfach 80.000, 5600 JA Eindhoven, The Netherlands). 151. Mermet, J.-M., Murillo, M., Behaviour of line intensities as a function of the operating parameters in inductively coupled plasma atomic emission spectrometry, (Laborat- oire des Sciences Analytiques, Bat.308, Universitk Claude Bernard-Lyon I, 69622 Villeurbanne Cedex, France). 152. de Galan, L., An appraisal of current developments in optical atomic spectrometry, (Laboratorium voor Analy- tische Chemie, Technische Hoogeschool, De Vries van Heystplantsoen 2, 2628 RZ Delft, The Netherlands). 87/C1153. Zil’berstein, Ch. I., New applications of ICP-AES and LAFS in trace analysis, (Institute of Silicate Chemistry, Acad. Sci. of the USSR, Leningrad, USSR). 87IC1154. Havezov, I., Einfuhrung der Probe in das AA-Suek- 87/C1 87/C1 87/C1 87/C1 trometer - Probleme und Losungen, (Institut fur -All- gemeine und Anorganische Chemie der BAW, Sofia, Bulgaria).55. Gilmutdinov, A. Kh., The formation of an analytical signal in electrothermal atomic absorption spectrometry, (V. I. Ulyanov - Lenin University, Physics Faculty, Kazan, USSR). 56. Sychra, V., Ortner, H., Doleial, J., HlavaE, R., Kolihova, D., VyskoEilova, O., Piischel, P., Formanek, Z., New advances in tungsten-furnace AAS, (Inst. Chem. Tech- nol., 166 28 Prague 6, Czechoslovakia). 57. Sturgeon, R. E., Willie, S. N., Berman, S. S., Analytical applications of sorption and atomisation of metallic hydrides in a graphite furnace, (Div. Chem., Natl. Research Council of Canada, Ottawa, Ontario KIA OR9, Canada). 58. Frech, W., Cedergren, A., Lundberg, E., Baxter, D., Eine neue Graphitkuvette fur die AAS und AES, (Universitat UmeH, Dept.Analytische Chemie, S-901 87 Umei, Sweden).JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, JUNE 1987, VOL. 2 131R 87/C1159. Holcombe, J. A., McNally, J., Interactions at the graphite surface in electrothermal atomisers, (Dept. Chem., Univ. Texas, Austin, TX 78712, USA). 87/C1160. Welz, B., Schlemmer, G., Radziuk, B., Heterogene Reaktionen im Graphitrohr der elektrothermischen Ato- mabsorptionsspektrometrie, (Abteilung fur Angewandte Forschung, Bodenseewerk Perkin-Elmer & Co GmbH, D-7770 Uberlingen, FRG). 871C1161. Chakrabarti, C. L., Gilchrist, G. F. R., Rademeyer, C. J., Delgado, A. H., Mechanisms of matrix interferences in graphite furnace atomic absorption spectrometry, (Dept. Chem., Carleton Univ., Ottawa, Ontario K1S 5B6, Canada). 871C1162. Slavin, W., The STPF concept in furnace AAS, (Perkin- Elmer Corp., 901 Ethan Allen Hwy., Ridgefield, CT 06877, USA). 87/C1 87/C 1 63. Dittrich, K., Nichtthermische Anregungsverfahren (LAFS, LAMOFS, FANES, MONES) zur Verbesserung der analytischen Moglichkeiten der AASIETA, (Sektion Chem. der Karl-Marx-Universitat Leipzig, Analytisches Zentrum, DDR-7010 Leipzig, Talstr. 35, GDR). 64. Werner, G., Anforderungen an die quantitative Analytik und ihre Erfullung durch die Atomspektroskopie, (Karl- Marx-Universitat, Sektion Chemie, Leipzig, GDR). 87/1165. Rojas de Olivares, D., Flame atomic emission determina- tion of ruthenium, At. Spectrosc., 1986, 7 , 56. (Dept. Quim., Fac. Cienc., Univ. Los Andes, Merida 5101-A, Venezuela). 87/1166. 8711 167. 87/1168. 87/1169. British Standards Institution, Powder metallurgical materials and products. Part 4. Methods of testing and chemical analysis of hardmetals. Section 4.17. Chemical analysis by flame atomic-absorption spectrometry. Subsec- tion 4.17.3. Determination of cobalt, iron, manganese and nickel in contents from 0.01% to 0.5% (mlm), British Standard, BS 5600: Subsection 4.17.3: 1986 (IS0 7627/3- 1983), 30 Jun 1986, pp. 4. (Linford Wood, Milton Keynes MK14 6LE, UK). British Standards Institution, Powder metallurgical materials and products. Part 4. Methods of testing and chemical analysis of hardmetals. Section 4.17. Chemical analysis by flame atomic-absorption spectrometry. Subsec- tion 4.17.2. Determination of calcium, potassium, magne- sium and sodium in contents from 0.001% to 0.02% (m/m), British Standard, BS 5600: Subsection 4.17.2: 1986 (IS0 7627/2-1983), 30 Jun 1986, pp. 4. (Linford Wood, Milton Keynes MK14 6LE, UK). British Standards Institution, Powder metallurgical materials and products. Part 4. Methods of testing and chemical analysis of hardmetals. Section 4.17. Chemical analysis by flame atomic-absorption spectrometry. Subsec- tion 4.17.4. Determination of molybdenum, titanium and vanadium in contents from 0.01% to 0.5% (mlm), British Standard, BS 5600: Subsection 4.17.4: 1986 (IS0 762714- 1983), 30 Jun 1986, pp. 4. (Linford Wood, Milton Keynes MK14 6LE, UK). British Standards Institution, Powder metallurgical materials and products. Part 4. Methods of testing and chemical analysis of hardmetals. Section 4.17. Chemical analysis by flame atomic-absorption spectrometry. Subsec- tion 4.17.5. Determination of cobalt, iron, manganese, molybdenum, nickel, titanium and vanadium in contents from 0.5% to 2% (mlm), British Standard, BS 5600: Subsection 4.17.5:1986 (IS0 7627/5-1983), 30 Jun 1986, pp. 4. (Linford Wood, Milton Keynes MK14 6LE, UK).JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, JUNE 1987, VOL. 2 132R Glossary of Abbreviations Whenever suitable, elements may be referred to bv their chemical svmbols and compounds by their formulae. The following abbreviations are used extensivefy in the Atomic Spectrometry Updates. ax. AA AAS AE AES AF AFS APDC ASV CMP CRM cw d.c. DCP DMF DNA EDL EDTA ETA FAAS FAES FAFS FI GC GDL HCL h.f. HPLC IBMK alternating current atomic absorption atomic absorption spectrometry atomic emission atomic emission spectrometry atomic fluorescence atomic fluorescence spectrometry ammonium pyrrolidinedithiocarbamate (ammonium te t rame th ylenedi t hio- carbamate) anodic-stripping voltammetry capacitively coupled microwave plasma certified reference material continuous wave direct current d.c. plasma N, N-dimet h ylformamide deoxyribonucleic acid electrodeless discharge lamp ethylenediaminetetraacetic acid electrothermal atomisation flame AAS flame AES flame AFS flow injection gas chromatography glow discharge lamp hollow-cathode lamp high-fr equency high-performance liquid chromatography isobutyl methyl ketone (4-methylpentan- 2-one) ICP IR LC LTE MECA MIP MS NAA NaDDC NTA OES PMT p.p.b. p.p.m. PTFE r.f. REE RM RSD SBR SEM SNR SSMS TCA TLC TOP0 u.h.f. uv VDU vuv XRF inductively coupled plasma infrared liquid chromatography local thermal equilibrium molecular emission cavity analysis microwave-induced plasma mass spectrometry neutron activation analysis sodium diethyldithiocarbamate nitrilotriacetic acid optical emission spectrometry photomultiplier tube parts per billion parts per million polytetrafluoroethylene radiofrequency rare earth element reference material relative standard deviation signal to background ratio scanning electron microscopy signal to noise ratio spark-source mass spectrometry trichloroacetic acid thin-layer chromatography trioctylphosphine oxide ultra-high-frequency ultraviolet visual display unit vacuum ultraviolet X-ray fluorescence

ISSN:0267-9477    

DOI:10.1039/JA987020115R

出版商:RSC    

年代:1987

数据来源: RSC

摘要:

V H istorica I Perspectives Towards a Definitive History of Optical Spectroscopy Part I. Simple prismatic spectra: Newton and his predecessors D. Thorburn Burns Department of Analytical Chemistry, The Queen’s University of Belfast, Belfast BT9 5AG, UK Review of the prism refraction studies made by Porta (1593), Descartes (1637), Kircher (1646), Marci (1648), de la Cham- bre (1650) and by Boyle (1664) demon- strates that Newton was not, as popularly held, the first to contrive or observe the solar spectrum. Attention is drawn to the significant influences of Descartes on Boyle and, of Boyle on Newton’s spectral studies. The erroneous view that Newton was the first to contrive or observe the solar spectrum by the dispersion of white light has been made, implied, or given pride of place by many authors.1-9 This well estab- lished error of fact or emphasis most probably owes its continuance to Twymans’s view3 of Kayser’s account of the history of spectral analysis,lO “Kayser was my chief guide .. . the more I sought the more I was impressed by the thor- oughness of his historical survey. ”3 More careful reading of Kayser, however, shows that he was aware of earlier work by Marcus Marci of Kronland, published C D1 habe cui pIur; pona fcilic rtrin oculc dia q dem bunt v Fig. 1. The biprism in Maurolyci, Photisrni de lurnine. . ., (1611) in 1648.11 The origins of contrived spectra are much earlier as noted by Sabra12 and by Henderson.13 Man-made spectra have been known from at least the thirteenth century when experiments using globes of water were often used to imitate rain- drops by those trying to explain the rainbow. For example, Leonard0 da Vincil4 wrote: “.. . if you place this glass full of water on the level of the window, so that the suns rays strike it on the opposite side, you will then see the aforesaid colours [of the rainbow] producing them- selves, in the impression made by the solar rays which here penetrated through this glass of water, and terminated on the floor in a dark place at the front of the window; and since the eye is not employed we clearly can say with cer- tainty that these colours do not derive in any way from the eye.” Extensive studies on the transmission of ideas on the rainbow up to the seventeenth century have been made and reported by Crom- biel5 and by Boyer.16 The first time the use of a prism was studied and recorded in a book of optics was, according to Ronchi,l7in the book of Maurolicols published in 1611 (Fig.1) possibly based upon the time the work was carried out to which he pays parti- cular attention. Ascribing priority to the date work was carried out and not to the date of publication or date material was submitted for publication can cause prob- lems. Maurolico’s book was, as noted in the text, written in several parts at differ- ent times (1521,1553 and 1554), added to (1555), edited and indexed later (1575), and finally published in 1611. None of Maurolico’s prism diagrams indicate dis- persion or the formation of a spectrum. Studies of refraction of light had been published earlier than 1611 by Alhazeni (1572),19 Della Porta (1593)2O and by Kepler (1604)21 but only Della Porta showed a prism and noted colour forma- tion.Della Porta’s diagram of the prism and the ray paths is highly speculative (Fig. 2). It is difficult to understand why the prism diagram is so poor in view of the detail and accuracy of knowledge of optics, shown in other sections of the text. The first reasonably accurate diagram of the formation of a spectrum appears to be that of Descartes. Descartes (1637) is very important in his own right and for his influence on later 10. BAPTISTAE PORTAS 0 n Fig. 2. Triangular prism, the sun and colours, in De Refractione, Portae (1593) workers, such as Boyle and Newton. In an appendix to his Discours de la Methode,22.23 Dioptric, he formulated the hitherto elusive law of refraction, independently it is considered of Snell.12 In another appendix, Mktkores, he gave a diagram (Fig. 3) showing rays of the sun impinging on a glass prism or triangle with the refracted rays forming a rainbowed- hued patch on cloth or white paper placed on a vertical wall. The green, blue and violet colours were seen towards H, the red, orange and yellow towards F, widen- ing the aperture DE destroyed the colours near G. Descartes’ theory of colour and refraction was complicated and corpuscu- larianl2: the speed of rotation of light particles varied with colour, light had speed and a “determination to move in aJOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, JUNE 1987, VOL. 2 m8 Da A R ~ Y 344 7, L E qudd B A C ;n tkidnguIs ifogena fit grad: 60, iadinatia autcm K T grad: 1 9 prim: x 5 S.3 6. ccli refraBio cornpetit grad: 4 prim: 47 So 3 9 .- quz ad- Fig. 5. Production of colours by refraction and difference in path length in Marci, Thau- mantis (1648) Fig. 3. differing angles of incidence at the first being the brighest colour while green and ours in Descartes, Dioptrique (1637) refraction which caused differing path purple rays emerged in order, lower down particular direction,” which changed lengths in the refracting medium. Thus in the prism face. the drawing shown in Fig. 5 the small Boyle’s (1664) contributions to optics upon refraction. difference in the angles DKB and HFK and the study of colour were important in than 2000 extant letters attest to his (0.5” due to the size of the sun’s disc) gives themselves at the time and for their extraordinary variety of interests and a shorter path length, FG, for the purple influence on Newton, yet were over- intellectual endowment. He sought to light appearing at E, and a longer one, KI, looked by Ronchil7 and by Henderson.13 disseminate the knowledge at his dispo- for the red light appearing at L.Both Boyle wrote in Colours28Jo “The Trian- sal, his printed comprehensive and refractions were stated to be essential to gular Prismatical Glass being the Instru- illustrative, became popular. In produce colour. Marci is commemorated ment upon whose Effects we may the Magna Lucis et umbrae24 he argued that in a medal of the Czechoslovak SpeCtrO- most Commodiously speculate the Nature light was connected to the heavens by an scopic Society,25 as was recently drawn of Emphatical Colours, (and perhaps that of Others too;) we thought it useful to unknown chain but behaved like magnets.attention to by Ure*26 He gave an illustration of a triangular M. C. de la Chambre (1650) was observe the several Reflections and Re- prism and the separation of light into another court physician interested in the fractions which the Incident Beams of production of colours by refraction.27 Light suffer in Rebounding and Passing colours, shown in Fig. 4. Like Marci he thought that the path through it . . .”30a His diagram, Fig. 7, length was important but that interaction shows a pleasing precision as compared between the refracted and internally re- with the earlier representations.Boyle flected rays was necessary, as shown in also described the effect of a double Fig. 6. “The reflected rays mixing with the convex lens and a concave mirror to luminous mass traversing the triangle recombine the spectrum into white light infect it with their colours.” He attemp- and colour mixing using two prisms but ted, not very convincingly, to explain how did not venture a theoretical explanation. the red rays emerged nearest the prism “But upon this we must not now stay to apex where the opacity was least, red Speculate.”30b From Colours and later works it is clear that Boyle regarded light as small corpuscules or globuli but was not sure as to the correct description,30c “in order to such an undertaking (perfect account of the theory of Vision and Colour) I would first Know what Light is, and if it be a Body (as a Body or the motion of a Body it seems to be) what Kind of Corpuscules for Size and Shape it consists of, with what Swiftness they move Forwards, and Whirl about their own Centres.Then I would Know the Nature of Refraction, which I take to be one of Marcus Marci of Kronland in Bohemia, the Abstrusest things (not to explicate a court physician in Prague described the Plausibly but to explicate Satisfactorily) spectral colours obtained by refraction that I here meet with in Physicks; . . .” through a triangular prism11 and the The influence of earlier works on Boyle is persistance of colours, once separated, in far from clear. Boyle wrote in Physiolog- subsequent refractions but did not men- ical Essays31332 “For .. . I have purposely tion the reconstitution of the spectrum Fig. 6. Production of colours by refraction refrained, though not altogether from into white light. He believed that the and reflection in de la Chambre, Nouvelles consulting about a few particulars, yet different colours to result from slightly Observations . . . sur I’Iris (1650) from seriously and orderly reading over Refraction and the formation of col- The Jesuit Kircher’s 44 books and ?*, \ \ ,,\ \ Fig. 4. Refraction and the formation of col- ours in Kircher, Ars Magna Luck . . ., (1646, illustration taken from Second Edition 1671) wJOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY’ JUNE 1987, VOL. 2 345 Y \ B acroaiPnpIrr Cryhllinr Prifi, oncd MP0 An w r c cdga P, is l a d dirt#lytowords the Sun.Tworays trom i c sun fa1lu-q on the hirm at BB. and thtncc partly rcRtacd towards c 6’ and pnly rd&cd towards D 6 C, B C 6’ By, Thorc dc&d Rays B D & 6 8, Thoc refraM Rays which arc partly r&&d tc.wardsE & t. and tkrc paint an Iris I 2 3 4 5,dcno- ting tk fivc conkutionr of cofo~n Rcd Gmn; Blew, and Purplc ; and arc p l y r d a d towards F 6 f. D F & 6 f. Thofc RcfMcd Rays which arc part1 rCfro&d wards H 6’ e, FH 6 t t ~ Thofc rctldcd Rays which arc rcfn&d to- wards I & I. and t k c pint an other fdinrct Iris, thc colours of which arc contrary to the f m r 4 3 2 1:. fignifying Puvlc, Blew, Ctccn, Yellow, id, fothat tk Prif“ in chis poltutc txhibits four Rainbows. Y c h v towards G & U. ~olourlds, and partly re I a, to- Fig.7. Robert Boyle’s diagram of the sun’s spectrum in Colours (1664) their excellent (though disagreeing) books . . . that I might not be pre- possessed with any theory or particu- lars.”32a The books specifically listed were Gessendus’ Sytagrna, Descartes’ Prin- ciples of Philofophy and Bacon’s Novum Organum. In the Sceptical Chemist33 he states “. . . I, who had the good fortune to learn the operations [chemistry] from illiterate persons, upon whose credit I was not tempted to take up any opinion . . .”34a Boas35 is of the opinion that these statements should not be taken at face value for in other places Boyle indicates he was proud to be well read, his guarded approach avoided much controversy. Boyle frequently gave credit and often references in almost the modern style and it is quite clear he had read the work of Descartes and of Kircher carefully as his citations and references36 to Descartes exceed 60 and those to Kircher number about 20, indeed in Excellency of Theol- ogy37938 Boyle talks of “Des Cartes’s excellent Diopticks.”38a F. Grimaldi (1665) was one of the many Jesuit experimental physicians. His illus- tration of refraction by a prism39 (Fig. 8) clearly shows increased dispersion upon each passage of a beam through the prism. Grimaldi favoured a fluid nature for light. His primary contribution was the discovery of optical diffraction when the demonstrated coloured fringes at the edges of shadows from a narrow rod and other objects which extended far beyond what rectilinear projection would have predicted. m Fig.8. Grimaldi’s representation of prism, refraction and dispersion from De Lurnine (1665) Newton began his prism spectra studies in 1666 and six years elapsed before the first publication the now famous Phil. Trans. paper in 1672.40 It is clear from his wording “I procured me a triangular glass, to try therewith the celebrated Phae- nomena of Colours”40 that he was aware of earlier work but unlike Boyle, Newton was sparing with references and normally only referred to other work when devel- oping counter arguments to experiments or conclusions. The key spectral experi- ments including the use of a double concave lens (see Fig. 9) and a concave mirror to recombine the colours to white were an unreferenced repeat of Boyles’. The powerful influence of Boyle on New- ton’s spectral studies is based on Hall’s examination of one of Newton’s early scientific note books which contain detailed notes from Boyle’s book Col- ours28 and other of his works.41 Newton also studied Descartes and Hooke.42 His acquisition of prisms their quality and the sequence of the experiments which were carried out and reported over a long346 JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, JUNE 1987, VOL.2 prt Y I Fig. 9. Newton’s analysis and synthesis of white light, from Phil. Trans. (1672) Fig. 10. Newton’s analysis and synthesis of white light in Opticks (1704) period of time have been analysed by Mills.43 There was a 32 year gap between Newton’s first and second publication, Opticks,44 although the results of his studies were given in his Cambridge lectures on optics delivered from 1669,42945 these were not published until 1729,46 based upon the second draft manuscript of about 1671.Newton’s model of light was corpuscular, although he found it necessary to invoke waves in the ether to explain the “Newton’s Rings” phenomena. He worried about explana- tion of the diffraction phenomena, des- cribed by Grimaldi, and wrote to Boyle, February 28th 1679,47 discussing a pos- sible explanation based upon variable density of the aether within and without solid bodies. Newton was the first to use the term spectrum48 (Latin for appear- ance) for the elongated coloured image whereas Boyle uses the term iris49 (Greek for rainbow), both noted five main col- ours, purple, blue, green, yellow and red.In addition, Newton reported orange and indigo, based upon observations of an assistant “whose eyes were more critical for distinguishing colours than mine. ”44a These two colours he then promoted to fundamental divisions, by analogy with the notes in a musical scale. Newton’s discussion on the nature of white light, colour mixing complimentary colours were more detailed and the observations more refined in Opticks (compare Fig. 9 with Fig. 10) but they were not totally original, hence it cannot be held that Newton was the first to contrive or observe the spectrum. The author is grateful to the Library of the Wellcome Institute for the History of Medicine for study facilities and for per- mission to reproduce photographs (Figs. 1 and 2), to Professor E.Roth for assistance and to the Bibliotheque Centrale Du Museum National D’Histoire Naturelle, Paris, for the photograph for Fig. 6 , and to his long-time friend and colleague Dr. M. Malit, Charles University, Prague, for obtaining the photograph of Marci’s text, Fig. 5. 1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. References Roscoe, H. E., “Spectrum Analysis,” Macmillan , London, 1869. Judd Lewis, S . , “Spectroscopy in Science and Industry,” Blackie, Glasgow, 1933. Twyman, F., “Metal Spectroscopy,” C. Griffen, London, 1951. Szabadvhry, F., “History of Analytical Chemistry,” Pergamon Press, Oxford, 1966. Thorburn Burns, D., Proc. Anal. Div. Chem. SOC., 1975, 11, 155. Latinen, H. E., and Ewing, G. W., “A History of Analytical Chemistry,” Divi- sion of Analytical Chemistry, American Chemical Society, Washington, DC, 1977.Szabadvhry, F., and Robinson, A., “The History of Analytical Chemistry,” in Svehla, G., Editor, “Comprehensive Analytical Chemistry,” Volume X, Elsevier, Amsterdam, 1980. Campbell, W. A., “Analytical Chem- istry,” in Russell, C. A., Editor, “Recent Developments in the History of Chemistry,” Royal Society of Chem- istry, London, 1985. Bennett, J. A., “The Celebrated Phae- nomena of Colours: the early history of the spectroscope,” Whipple Museum, Cambridge, 1984. Kayser, H., “Handbuch der Spectros- copie,” Volume I, S. Hirzel, Leipzig, 1906. Marci, J. M., “Thaumantis, Liber arca coelesti deque colorum . . .,” Typis Academicis, Pragae, 1648. Sabra, A. I., “Theories of light from Descartes to Newton,” Oldbourne, London, 1967.Henderson, S. T., “Daylight and its spectrum,” Second Edition, Adam Hilger, Bristol, 1977. 14. 15. 16. 17. 18. 19. 20. 21. 22. 23. 24. 25. 26. 27. 28. 29. 30. 31. 32. 33. 34. 35. da Vinci, L., Translated by MacCurdy, E., “The Notebooks of Leonard0 da Vinci,” Volume 2, Jonathan Cape, London, 1956, p. 279. Crombie, A. C., “Robert Grosseteste and the Origins of Experimental Science,’’ Second Impression, Claren- don Press, Oxford, 1962, (first published 1953). Boyer, C. B., “The Rainbow from Myth to Mathematics,” T. Yoseloff, New York, 1959. Ronchi, V., “The Nature of Light, an Historical Survey,” Heinemann, London, 1970, (originally published in Italian as “Storia della Luci,” 1939). Maurolyci, F., “Photosmi de lumine et umbra . . . ,” T. Longi, Neopoli, 1611.Alhazeni, Translated by Risnero, F., “Opicae,” E. Episcopics & N. F. Haeredes, Basileae, 1572, Baptistae, J. B., “De Refractione,” J. Carlinum & A. Pacem, Neopoli, 1593. Kepler, J., “Ad Vitellionen paralip- mena . . .,” C. Marnium & H. J. Aubrii, Francofurti, 1604. Descartes, R., “Discours de la Methode . . .,” J. Maire, Leiden, 1637. Descartes, R., “Principia Philosophi- nae,” ultima editio, 1677; “Specimena Philosophiae: seu Dissertatio de Methodo . . . Diotrice, et Meteora,” 1677; “Passiones Animae,” 1677, D. Elsevirium, Amstelodami. Issued as three works in one volume, used in this study. Kircheri, A., “Ars Magna Lucis et Umbrae,” L. Grignani for H. Scheus, Romae, 1646; Second Edition, J. Jans- sonium, Amstelodami, 1671. Vobecky, M., Editor, “The Czecho- slovak Spectroscopic Society by the Czechoslovak Academy of Sciences 1949-1984,” Prague, 1984.Ure, A. M., “The Origin of Spectra. Who was the first?”, J . Anal. A t . Spec- trom., 1986, 1, 6. de la Chambre, M. C., “Nouvelles Observations et Coniectures sur YIris,” P. Rocolet, Paris, 1650. Boyle, R., “Experiments and considera- tions touching colours . . . ,” H. Herring- man, Anchor, New Exchange, London, 1664; reprinted by Johnson Reprint Corp., New York, 1964. (Second Edi- tion, 1670.) “The Works of the Honourable Robert Boyle. In six volumes to which is pre- fixed a Life of the Author, A New Edition,” J. and E. Rivington et al., London, 1772. Ref. 29, Volume I, pp. 662-799; (a), p. 726; (b), p. 727; (c), p. 695. Boyle, R., “Certain Physiological Essays, written at distant times and on several occasions,” H.Herringman, London, 1661; Second Edition, 1669. Ref. 29, Volume I, pp. 298-457; (a), p. 302. Boyle, R., “The Sceptical Chemist . . .,” J. Caldwell for J. Crooke, London, 1661; Second Edition, H. Hall, Oxford, for R. Davies and B. Took, London, 1680. Ref. 29, Volume I, pp. 458-661; (a), p. 463. Boas, M., “Robert Boyle and Seven- teenth-century Chemistry,” University Press, Cambridge, 1958.JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, JUNE 1987, VOL. 2 347 36. 37. 38. 39. 40. 41. 42. Index to “Works” ref. 29 gives 31 entries for Descartes and 14 for Kircher, balance are in the text and unindexed. Boyle, R., “The Excellency of The- ology, compared with Natural Philos- ophy . . .,” T. N. for H. Herringman, London, 1674. Ref. 29, pp. 1-84; (a); p. 18. Grimaldo, F. M., “De Lumine, Colori- bus et Iride . . .,” H. V. Benatij, Bononiae, 1665; reprinted by Dawson, London, 1966. Newton, I., Phil. Trans., 1672, 6 , 3075. Hall, A. R., Ann. Sc., 1955, 11, 27. Shapiro, A. E., Editor, “The Optical 43. 44. 45. papers of Isaac Newton,” Volume I, “The Optical Lectures 1670-1672,” Cambridge University Press, Cam- bridge, 1984. Mills, A. A., Notes and Records, Roy. SOC., 1981, 36, 13. Newton, I., “Opticks . . . ,” S . Smith and B. Walford, London, 1704; Fourth Edi- tion, W. Innys, London, 1730, was re- printed by Dover Publications, New York, 1952 and 1979; (a) reprint, p. 128. Whiteside, D. T., Editor, “The Unpub- lished first version of Isaac Newton’s Cambridge Lectures on Optics 1670- 1672,” Cambridge Library, Cambridge, 46. 47. 48. 49. 1973. (Facsimile reprint + commentary.) Isaaci Newtoni, “Lectiones opticae, annis MDCLXIX MDCLXX MDCLXXI. In scholis publicis habitae . . .,” G. Innys, Londoni, 1729. Ref. 29, Volume I, in “Life,” pp. cxii- cxvii . Murray, J. A. H., et al., Editors, “A New English Dictionary on Historical Principles; . . .,” Volume IX, p. 557, Clarendon Press, Oxford, 1919. Murray, J. A. H . , et al., Editors, “A New English Dictionary on Historical Principles; . . .,” Volume V, p. 476, 1901.

ISSN:0267-9477    

DOI:10.1039/JA9870200343

出版商:RSC    

年代:1987

数据来源: RSC

摘要:

JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, JUNE 1987, VOL. 2 347 Atomic Spectrometry Viewpoint Angello Grillo Questron Corporation, PO Box 2387, Princeton, NJ 08540, USA Peter Stockwell P.S. Analytical Ltd., Cray Avenue, Orpington, Kent BR5 3TR, UK Since the Pittsburgh Conference is primarily about an instrument exposition Les Ebdon, Chairman of our Editorial Board, took the opportunity to interview the principals of two of the many companies exhibiting at PittCon-Angello Grillo of Questron Corporation and Peter Stockwell of P.S. Analytical Ltd. L.E. The first question I’d like to ask is about your thoughts on the exhibition this year, and how it compares with previous exhi bitions ? A.G. The exhibition has been a terrific success this year. It is even better than previous years, and we seem to have a much higher attendance.I’m sorry to see that it’s not going to be in Atlantic City next year. However, and I believe I am speaking for other small companies with exhibits downstairs in the “parking lot ,” we had a terrific time and we are looking forward to next year in New Orleans. L.E. Peter, you represent one of the growing number of British companies which exhibit at PittCon, are you pleased with the response you have had here? P.S. I think it’s been a very good show, there are lots of people and a lot of interest and I think that the Americans are beginning to pay heed to what is done across the water in the UK, and I think more British companies should be encouraged to come across here. L.E. To the rest of the world this show is absolutely enormous with nearly 30 000 people coming along.How influential is it within the American market? How much do your orders for the whole year depend upon the contacts that people make at this particular show? A. G. Essentially, my promotional budget and my marketing for the year, revolve around this show. This is the one single show in which a company my size should make a strong investment. We attend several other shows but in a much smaller way. I will be receiving business directly from this show over the next four to six months and it will probably represent at least 2070, maybe 3070, additional busi- ness for me. L.E. It’s very interesting to hear that kind of comment from what I guess is technic- ally speaking, still one of the smaller companies exhibiting here, although I’m sure you’d want to talk to us about your growth statistics. I suppose for many people PittCon is associated with the big- ger company, the big instrument company with a complete range of instruments.How much of the show do they represent and do you see any trends in them becoming more dominant or less dominant in this par- ticular show? A.G. Representing the small companies throughout the world, I see a trend toward the larger companies becoming less dominant at the Pittsburgh Confer- ence. The East Hall and the “parking lot” are full of small companies, scratching and fighting for an extra booth here and there. People come to the Pittsburgh Conference to shop. For the most part they’re coming to see a particular prod- uct, of a larger company, that they have seen advertised.But they’re also coming in droves to the lower floors, the “bar- gain” basement, to see what new services or technologies the young companies are showing. P.S. One of the other interesting things which is more particular this year I’ve noticed is that people are not just coming to look at instruments, they are acutally shopping for services. One person I sat down and discussed analytical chemistry with was promoting the view that in America certainly, you’re often dealing with people who are not qualified in analytical chemistry. Often they are using sophisticated instrumentation, such as ICPs. This is generating a growth industry of people who are doing software, selling training courses and all types of practical chemistry, which is a little surprising.The chemistry is going out of instrumentation but these small companies are coming in and actually selling chemistry packages so that the customer can do the analytical chemistry required for his samples. L.E. So do you think there’s a real vacancy in the market now for people to come into this in an entrepreneurial way and perhaps interface between the big instrument com- panies and the regular laboratory? P.S. I think it’s a good question. I think things are actually different in the UK, but obviously here in America there’s a big need for people to do such a thing. The other interesting thing is I suppose that more and more people are shopping around and not necessarily always buying the complete package from one instru- ment company.They are looking around for auto samplers or any devices which would fit on to an instrument and trying to tie it together. I think one of the things larger companies have to do is to make their instruments more accessible to this sort of operation.348 JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, JUNE 1987, VOL. 2 L.E. So perhaps I can ask the two of you whether you see the actual growth of your own companies within this continuing service and intermedaite area, or whether you think there is still the same track as there used to be of small companies growing bigger and hence becoming a big instrument company? A.G. Well there are certainly lots of possibilities for small companies to grow into giants. There are always new possibi- lities. Do I see Questron growing into a giant? The answer is no.We are a distributor, trying to fill a niche which requires product plus a very very per- sonalised service. Here in the United States you have many corporations with large direct sales and many corporations selling through very small representative companies. We are trying to grow by providing more services than both of these alternatives, at less expense to our clients and principals. I would like to grow to a point where Questron is big enough to provide comfortably a total product service; that would be enough. P.S. I think my company represents rather a different angle on that, in that what we try to do is interface with customers in new concepts and new ideas and try to get things on the market to them, before they are readily available from major instrument companies.Also we interface with major instrument com- panies because we try to develop an idea and a concept, make it into a product and then put it out as a sales item through large instrument companies. I think also because we can deal more directly with customers than a representative can and we have more knowledge in a small company of the products we are selling, we know them intimately, we understand the area better. We interface with academics and the customers who’ve got real problems. We have close contacts with universities in the UK and in America and this is a vital aspect to us. We have developed the ideas of academ- ics and have produced items on a one-off basis and several items which we fabricate have been developed in this manner, i.e., as small batches not by mass-production. These products are produced in units of up to 40-50 a year and we can make these attractively and introduce them to a wider audience quicker and more economically than many major companies. A.G. I think the Pittsburgh Conference is an important place to tie in all of these activities we are discussing. It allows us to get at so many people: new principals, consultants coming in with new ideas, young companies starting out. In fact this is how Peter and I met. We were both stalking PittCon, our briefcases filled with literature and drawings on new products and ideas for sale. So it’s an important meeting place for people to start and generate new deals. L.E. So far we’ve concentrated on the American dimension of the Pittsburgh Conference, but there are people here from all over the world and many companies of course come to make these international contacts.How significant in these terms is this conference? P.S. I think you cannot underestimate the significance of that. We’ve spoken to people from Japan. Last year we made contact with an agent in Japan and they are beginning to sell, and we first met here. They come here anyway because of the importance of it, and since we are here also then it’s an ideal opportunity to meet. We’ve met people from across the Con- tinents of Europe and Australia as well, who’ve come along both as customers and also people who are possible agents to sell our products. I think it is a fantastic show, I don’t think that there is any possibility that anybody can actually copy it, because it is typically American.I think the organisers all of whom are volunteers, except for two or three, should be con- gratulated on what they do. Like Angello I reserve judgement on New Orleans because I think that wasn’t such a success- ful show. But it still brought the interna- tional people, it didn’t bring as many of the buyers as such people are generally located on the East coast, being the market area that is most significant. L.E. Thankyouforsparingtimein whatisa very busy week, for you both, because I know that you’ve been inundated with people asking you questions and seeing people that you want to ask questions of in the typical Pittsburgh tradition. Although this may be the end of an era for the Pittsburgh Conference, if it is finally moving from Atlantic City, because it’s just outgrown the place and is now going to be moving to different cities around the US, perhaps it is also the beginning of another era that we’ve touched on. One which will see smaller companies interfacing between the larger companies and laboratories. It has certainly been very interesting to talk to you about that.

ISSN:0267-9477    

DOI:10.1039/JA9870200347

出版商:RSC    

年代:1987

数据来源: RSC

摘要:

348 JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, JUNE 1987, VOL. 2 Conference Reports 37th Pittsburgh Conference and Exposition on Analytical Chemistry and Applied Spectrometry: March 9th-l3th, 1987, Atlantic City, New Jersey, USA The experience of walking amongst what seemed to be a football crowd, half of whom seemed to be old friends, for four days, the persistent back-ache, two unex- pected memories of my first Pittsburgh Conference. Perhaps it is not surprising that this should be the feeling given the numbers of attendees, the total had reached 29538 by the middle day of the show, when I stopped counting, and the immense size of the exhibition halls. Another surprise was to have to struggle through crowds of aged gamblers, playing slot machines and cards in the casinos, in order to reach the lecture rooms, but we were in Atlantic City.This at least will change at PittConn, as it is affectionately termed, has grown too big for Atlantic City, just as it outgrew its original home in Pittsburgh. The attendance was up by 1.3% on 1986 and the number of exhib- itors exceeded 800. The scientific pro- gramme boasted some 1154 lectures in 127 sessions. Next year the meeting will move to bigger quarters in New Orleans (February 22nd-26th, 1988) and then on to Atlanta in 1989. Instrumentation for analytical atomic spectroscopy was prominent in the ex- position, although there were fewer in- novative presentations than in the recent past. Perkin-Elmer had on show a new bench top low-cost ICP instrument, the Plasma 40. This instrument operates at 40 MHz, with a free-running generator, and uses an argon cooled high-frequency coil.It incorporates an IBM PC and, while it only offers 0.19-nm resolution, the mono- chromator is purgable to allow use to 160JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, JUNE 1987, VOL. 2 nm. Without the computer it will sell for $49 000. Thermo Jarrell Ash, formerly Allied Analytical Systems, featured the Plasma-300 ICP instrument, also IBM PC compatible, and the new ICAP 61 a simultaneous plasma emission spec- trometer with a capability for up to 61 elements. The host computer was again an IBM PC and a new background correc- tion system was used. The ICAP 61 has a spark source sampling accessory which allows conducting solids to be analysed without dissolution. Improved software for the ICAP 1100 was also announced.Applied Research Laboratories featured the 3410 ICP system which uses a low- flow torch and is “bench height,” as a smaller r.f. generator can be used. Avail- able in vacuum, air or purged path con- figurations the instrument price starts at $56000. Baird also had new instruments on show. The PSX is a sequential ICP- AES system whereas the PSQ is simul- taneous with up to 30 channels, both use a 0.75-m monochromator, a 40-MHz low- flow, low-power plasma and IBM PCs for data capture and instrument control. Again they are particularly promoted as low-cost instruments, starting at $50 000. Leeman Labs exhibited their Plasma- Spec ICP/kchelle spectrometer with a supplementary IBM PC to run the new Dataspec I1 software.This new software has been developed by Ward Scientific. The high resolution and innovative Plas- marray instrument of PRA was exhibited operating at the show and attracted con- siderable attention. As did another approach to high resolution ICP spec- trometry, namely Fourier transform spec- trometry, and it was appropriate that the Chelsea Instruments FT 500 vacuum ultraviolet Fourier transform spec- trometer was featured on the Questron stand. Of interest to DCP users were the modifications to the Spectraspan instru- ment as shown on the ARL stand and reported in lectures. A new Spectraspan VB was introduced which is linked to an IBM PC. ARL also demonstrated their atomic emission spectrometers, with plasma, spark or GDL sources, as did several other companies including Baird, Thermo Jarrell Ash and Instruments SA.ISA had a lively display of Jobin-Yvon equipment. New to the show was the Shimadzu GMV-514 emission spec- trometer, a low-cost arc - spark system aimed particularly at the steel industry. There seemed to be less innovation in the AA instrumentation. Although a new German instrument the SIM-41 produced by AGW must be excluded from this comment. This instrument can determine 20 elements in a sample at the rate of 5 seconds per element. Equipped with the Atomsource Atomizer, a sputtering cell, solid samples can be analysed directly, provided they are conducting, with excel- lent detection limits. In order to achieve background correction a D2-arc beam is combined with the HCL beam. The instrument has furnace, flame , hydride, mercury and ICP accessories.The hydride generation unit being particularly flexible. A flash converter is used to provide computer control much faster than possible with analogue to digital conversion. In the United States this instrumentation will be sold by the Analyte Corporation at $50 000. Thermo 349 Jarrell Ash featured new software for their AA spectrometers, Varian their new range of instruments with Zeeman back- ground correction, Perkin-Elmer a new IBM PC data station for the 1100 and ARL the GBC System 2000 graphite furnace. The growth of companies selling XRF spectrometers continues and the variety of portable energy dispersive instruments was again noticeable. Naturally Philips were well represented with the PW 1800, claimed to be the first such instrument to incorporate robotics.ARL exhibited an updated 8400+ instrument with dual goniometer and new software. Rigaku showed their new 3030 spectrometer. This fully automated sequential instrument comes pre-programmed so that the user only has to press the appropriate element on a Periodic Table display to start the analysis. Diano demonstrated their new microcomputer controlled series 2000 X-ray vacuum spectrometer systems. This series is IBM PC compatible and demon- strates the growth of this new company since its formation in 1984. Jordan Valley Applied Radiation had on show their EX-3000 elemental analyser particularly designed for the industrial environment. Link Systems were prominent amongst the energy dispersive exhibitors , showing their XR 200/300 series.Nucleus featured their EX-2040 and -2030 XRF analysers both of which are personal computer based. The Portaspec automatic goniometer attachment was introduced by Cianflone, this can be retrofitted to all installed Portaspec portable X-ray spectrometers. Another new XRF moni- tor for on-stream analysis was the Asoma 8660, who also market the portable 8620. No dramatic advances in ICP-MS instrumentation were exhibited, but VG were kept busy demonstrating the Plas- maQuad in a seminar room away from the bustle of the main floor, and Perkin- Elmer Sciex talked about the new world- wide service now available for their Elan. However ICP-MS sessions attracted per-350 JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, JUNE 1987, VOL. 2 haps the biggest audiences in the scientific programme.The symposium organised by Sam Houk on the Thursday afternoon being particularly popular with invited lectures by Alan Gray, Gary Horlick, Jim McLaren and Roger Ng. The emphasis of the lectures was very much on interfer- ence effects, the extent and importance of which are still being evaluated in ICP-MS. While the honesty of this debate is wel- come, it should not be allowed to over- shadow the excellent results some work- ers are now obtaining on real samples; the examples given by Meddings and Ng being particularly impressive in this respect. As usual the five plasma emission sessions were well attended. The emphasis this year seemed to be on software and computing advances. Only three sessions were required for the atomic absorption presentations where furnace and hydride generation applications were prominent.Curtis Monnig and Gary Hieftje presen- ted some exciting results on the possibility of using magneto-optical rotation with polarisation modulation for trace metal determinations. Only half a session was devoted to X-ray fluorescence, and emis- sion spectroscopy (arcs and sparks) was also reduced to such a brief period. While these time allocations do not reflect the current usage of these techniques they mirror the present research effort into their development. It was good to hear compliments about JAAS from so many atomic spectroscop- ics at the conference and to know it is being well received all over the world. The Royal Society of Chemistry hosted a reception at the Golden Nugget Hotel on the Tuesday evening which was well attended despite counter attractions.Now the target for the RSC as indeed it is for all those involved in this, the biggest exhibition and conference in the world of analytical chemistry and applied spectro- scopy, is to do even better in New Orleans in 1988. Les Ebdon Plymouth Polytechnic, UK Thames Polytechnic, London, UK The Atomic Spectrometry Updates (ASU) Annual Symposium formerly the “Annual Reports on Analytical Atomic Spectrosopy” (ARAAS) , was held at Thames Polytechnic, London on the 8th April, 1987. The meeting has in the past been held in Sheffield and this was the first year of the new roving policy in which various UK sites will be visited, Prior to the meeting (7th April) the ASU Editorial Board met to discuss the format and presentation of the ASU reviews which appear at the end of each bimonthly issue of JAAS.As a variation from the meet- ing’s agenda we (the Editorial Board) witnessed two atomic spectroscopists (John Burridge and Barry Sharp) with totally unexpected aspirations as civil engineers as they compared the body weight to stress resistance of polytechnic furniture. Notable exceptions to this were the two largest board members (names withheld for fear of reprisal, see lateri under kebab). The meeting concluded, the board adjourned to the Trafalgar Tavern, Greenwich for the annual dinner. This was attended by our two invited overseas Board Members Roger Stephens (Halifax, Nova Scotia, Canada) and Gugielmo Rossi (Ispra, Italy) along with his wife.The after dinner speech by the Chairman, Malcolm Cresser, contained recollections of his days as a research student and the hardship experienced emptying beer barrels of their contents in conjunction with Roger Stephens and co-workers. All of which served to demonstrate that the friendship amongst past colleagues was warm and that wine had flowed freely during the dinner. After several minutes recital by the Chairman, presentations were made to Mrs. Rossi and to the two overseas speakers. The formal speech over, Steve Haswell Members of the ASU Board preparing for the Annual Meeting (Thames Polytechnic) provided us with the benefits of his many hours study by reciting a cheerful poem about life in the South of England. Everyone then ad- journed to the bar for liquid refreshment prior to the journey back to the hall of residence, a move not easily carried out in practice owing to the malfunction (broken rear axle to those mechanically minded) of the bus.Thus delaying our beauty sleep, some requiring more than others (no clues this time), for an hour; all of which gave Malcolm Cresser and Neil Barnett time to quell their hunger with a kebab. On to the meeting itself which was attended by approximately 45 delegates. In a plenary lecture Dr. Rossi described some of the activities of the spectroscopy sector of the European Community Research Centre at Ispra in Northern Italy. Three projects were described, the first one being the development of a remote sensing device for detection and characterisation of oil pollution at sea using laser induced fluorescence.Prelimi- nary investigations under controlled con- ditions have indicated the feasibility of detecting a range of heavy and light crude oils using fluorescence sensing. The first production instrument should be com- pleted towards the end of the year prior to testing in 1988. Secondly, a long-term series of experiments to examine the contribution of petrol lead to human blood lead is nearing completion (a similar evaluation is being carried out in the UK of which Trevor Delves at South- ampton is a participant). In the first experiment the lead isotopic composition in Italian petrol was altered by the use of lead from the Broken Hill Mine, Aus- tralia where the 206/207 Pb ratio is 1.04; this is in comparison with European leadJOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, JUNE 1987, VOL.2 35 1 Dr. G. Rossi and Dr. R. Stephens (invited overseas Board Members) at the Annual Dinner which has the isotopic composition for 206/207 of 1.18. Mass spectrometric determination of the native blood lead composition has indicated that approxi- mately 25% of the lead present is derived from car exhausts. The final report of this work is not yet available. In a separate experiment, the Athens lead experiment, started on 1st July 1983, the blood lead composition of 40 males/females/children and 30 traffic wardens (I don’t know if the lower number means more blood was removed?, the author) was monitored using ETA and XRF before and after reduction of the lead in premium petrol from 0.4 g 1-1 to a nominal 0.15 g 1-1. The results of this work have yet to be completed.Finally, a study of the trace metal (Cd, Cu and Pb) distribution in a freshwater ecosystem (Lake Maggiore, Northern Italy) as part of a comprehen- sive investigation into the pathway of toxic trace elements was outlined. The choice of the site on Lake Maggiore was entirely due to financial logistics coupled with the close proximity of Ispra. Results on the spatial distribution of the trace metals in the sediment and marine envi- ronment were presented in relation to a tributary river. In a lecture entitled “Trace Element Speciation-Does it Work in Theory?” by Steve Haswell (Thames Polytechnic) the requirement to determine elemental forms in biologcal and environmental samples was answered in the affirmative with the proviso that suitable methodol- ogy is developed (see later, Sparkes).Direct coupling and fraction collecting techniques for the introduction of the high-performance liquid chromatography (HPLC) eluent into an ETA were dis- cussed. The experimental determination of trace element complexes in polar dis- solved organic compounds in soil pore water was outlined together with more recent work on the simulation of the gastro-intestinal digestion of foodstuffs [a method developed by Crews et al., Ministry of Agriculture, Fisheries and Food (MAFF), Nonvich, UK]. The latter method was applied to crabmeat, with the determination of the cadmium speciation. The final lecture of the morning session was given by Simon Sparkes, a research fellow at AERE, Harwell, on the specia- tion of organic compounds of radio- nuclides by HPLC - ICP-MS.ICP-MS has received little attention as a chromat- ographic detector (except notably by MAFF, Food Science Laboratory, Nor- wich and Caruso et al., Cincinnati, USA) even though it provides many of the advantages for an ideal HPLC detector, e.g., long linear dynamic range, multi- element capability, good detection power, flow uptake rates of nebulisers compatible with HPLC flow-rates, as well as the additional advantage of isotopic information. These advantages were out- lined in the lecture and the capability for the determination of 238U, 232Th and 99Tc demonstrated. After an enjoyable lunch, the second of our overseas Board Members Roger Stephens presented a plenary lecture on new novel methods of elemental detec- tion.The lecture was entitled, “Fields, Photons and Elemental Analysis.” Two techniques were described in detail, Zee- man corrected absorption (ZAA) and magneto-optic rotation (MOR). ZAA operating without a monochromator, and hence non-dispersive was described. The emission from the hollow-cathode lamp passing through a flame atomiser to a photomultiplier tube, selectivity being achievable by either a magnetic field (situated around the atomiser) or polari- sation modulation (situated in front of detector) of the radiation. This system offers the advantages of a simple optical system, good sensitivity and the feasibility for multi-channel operation (a series of hollow-cathode lamps). A more versatile technique is MOR which arises from either the amplitude (dichroism) or the phase differences (birefringence) between orthogonal polarisation states.One particular application of MOR allows detection of the variation in iso- tope composition by determination of the ratio between dichroic and birefringent signals. This ability was demonstrated with respect to 208Pb. The associated technique of electro-optic rotation (EOR), produced by a radiofrequency field on a He - Ne laser source, was described. This technique can be applied for detection in solution or the vapour phase. The technique was demonstrated by measurement of the charge carried by adsorbed ions on a suspension of Bento- nite clav. Even though EOR is charge specific, detection limits in the ng ml-1 range are achievable as well as informa- tion on the oxidation state of the adsorbed species.“Chromatographic Separation and Detection Methods for Speciation Stud- ies” was the title of the lecture given by Peter Fielden from DIAS, UMIST, Man- Chester. The lecture considered the advantages of using separation techniques coupled with element/species selective detection. The advantages of utilising separation techniques were described as: ( a ) species resolved in time, (b) minimum sample pre-treatment for complex mix- tures, ( c ) integrated analysis procedure, ( d ) small sample volumes and (e) pre- concentration techniques possible, e.g. , ion-exchange chromatography. Three types of detector were considered: UV (non-specific) , electrochemical (select- ive) and atomic spectrometric (element specific).The question of the alternative detection techniques to atomic spec- trometry were considered in view of the information available and the instrumen- tation cost. A reminder was given that speciation studies have been performed for many years in electrochemistry with- out the need for separation techniques, providing species selective detection. Also, the versatility of electrochemical detection when used in conjunction with HPLC was demonstrated. Future metho- dology for speciation studies incorporat- ing the use of electrochemical cells for selective screening of species prior to separation by HPLC and detection by atomic spectroscopy was proposed. The use of electrochemical cells for pre-con- centration has already been applied in ICP-AES methodology. The final lecture of the symposium was presented by Steve Hill (Plymouth Poly- technic) who provided a review of recent work on arsenic speciation in environ- mental and food samples at Plymouth. The techniques described were directly coupled gas chromatography - flame atomic absorption spectrometry (GC - FAAS) and HPLC - atomic absorption spectrometry (HPLC - AAS). Details of the column type, mobile phase and flow rates for both GC and HPLC were given. The results of the arsenic speciation in pore waters, estuarine waters, seaweeds and some foodstuffs (fish, fruit and vege- tables) were shown. The continuity of the meeting was attributable to its Chairman, Malcolm Cresser and the hospitality extended by Thames Polytechnic, and in particular Steve Haswell. John R. Dean Research Fellow, Plymouth Polytechnic at MAFF, Food Science Laboratory, Norwich. UK

ISSN:0267-9477    

DOI:10.1039/JA9870200348

出版商:RSC    

年代:1987

数据来源: RSC

摘要:

352 JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, JUNE 1987, VOL. 2 Book Reviews Mass Spectrometry in the Analysis of Large Molecules. Edited by C . J. McNeal. Pp. x + 221. John Wiley. 1986. Price &24. ISBN 0 471 91262 X. This book contains the proceedings of the third Texas A & M Symposium on Mass Spectrometry, which had the theme “Suc- cess and failure at mlz 10000 and beyond. ” The format of the book is excellent with a series of review papers presented by leading researchers in the field, rather than shorter reports on specific topics such as the recently published volume “Ion Formation from Organic Solids 111,” (Springer Proc. Phys. Vol. 9, Springer Verlag, 1986). Both books cover much of the same ground but the reviewing style of the McNeal book makes it a more general introduction to high field mass spec- trometry for the average spectroscopist. Although the conference had as its theme mlz 10000 and beyond in fact the majority of the authors worked with molecules smaller than this.This does not detract from the value of the book as most of the contributors concentrating on the analysis of peptides (7 out of 13 papers) presented strategies involving a combina- tion of enzymatic and chemical degrada- tion of small proteins (>lo 000 u) fol- lowed by mass spectrometric analysis of the fragments (2000-5000 u). Three authors specifically addressed the mechanisms and kinetics of ionisation of these large molecules; and it is appar- ent that an increasing understanding of the manner in which ions are formed by heavy particle bombardment is gradually coming about.However there is as yet little evidence that these theoretical con- siderations have been used to improve the efficiency of ionisation of real samples. The most exciting possibility for the next conference would appear to be a use of the better theoretical understanding to improve the oyer-all sensitivity of the ionisation methods. This book was compared with two earlier publications covering similar ground, namely “Soft Ionisation Biolog- ical Mass Spectrometry,” edited by H. R. Morris, Heyden 1981 and “Mass Spec- trometry of Large molecule^,'^ edited by S. Facchetti, Elsevier 1985. The pace of progress has been high and perhaps the most obvious changes are the accepted routine analyses at 3000-4000 u and the increasing use of MS-MS techniques for structural analysis.However the lack of published data on the analysis of medium weight peptides (10 000-15 000 u) and small proteins (40 000-100 000 u) coupled with the extensive use of enzymatic tech- niques highlights the fact that the analysis of these molecules as intact moieties creates many problems which will need solving before the spectra of these com-JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, JUNE 1987, VOL. 2 353 pounds becomes more than just a serendi- pitous occurrence. As Frank Field said in the book under review “one can only speculate whether such monstrous gaseous ions can be produced . . . but the remarkable discovery of massive particle bombardment mass spectrometry . . . leads me to the opinion that anything may be possible.” Possible maybe, but it remains doubtful whether there is an analytical requirement to go much beyond 5000 u.Personally I found this a useful and interesting book, and I would recommend it as a good review of the current state of the art. N. J. Haskins Smith, Kline and French, Welwyn, UK Mass Spectrometry in Biomedical Research. Edited by Simon J. Gaskell. Pp. xvi + 492. John Wiley. 1986. Price S38.50. ISBN 0 471 91045 7. The appearance of a book of this nature is both appropriate and timely, given the major developments which have occurred in the mass spectrometry in recent years. The book consists of 26 chapters which are classified into three parts: Part I, Analyses of labile and polar compounds; Part 11, Analyses at high mass; and Part 111, Trace analyses.Each part is prefaced with “Overview” chapters by the Editor. These chapters provide background material to the specialist work of the invited contributors. They serve to add the essential continuity, which is often lacking in multi-author works of this sort. It is in the biomedical field that the developments which have taken place in mass spectrometry have made perhaps their strongest impact. Particularly signif- icant have been the advances in ionisation techniques, such that it is now possible to analyse previously intractable, involatile molecules. This area is well covered with contributions on sample preparation for FAB and FD (C. E. Costello), analysis of biochemical reactions in aqueous solution (R. M. Caprioli), analysis of bile salts (J.0. Whitney), characterisation of nucleic acid constituents (J. A. McClos- key), new methods for the analysis of acylcarnitines and acyl-coenzyme A com- pounds (D. S. Millington), screening for polar drug metabolites using FAB MS- MS (K. M. Straub), high-mass FAB studies of peptides , oligosaccharides and glycoconjugates (A. Dell and M. Panico), structure elucidation of complex carbohy- drates (V. Reinhold), FAB MS of oligo- nucleotides (L. Grotjahn), high-mass capabilities of sector mass spectrometers (B. N. Green and R. S. Bordoli), CID of peptide ions (M. M. Sheil and P. J. Derrick), plasma desorption MS of high molecular weight biomolecules (P. Roep- stoff and B. Sundqvist), MS analysis of biological oligomers (I. Jardine), high- mass FT-MS (D. H. Russell and M.E. Castro) and MS measurement of neuro- peptides (D. M. Desiderio and G. H. Fridland). Although generally thought of as a “mature” technique, GC-MS is indispen- sible in areas of biochemical trace analy- sis. Recent advances which have greatly improved the quality (selectivity and sen- sitivity) of trace analyses are exemplified in chapters on high sensitivity determina- tions of steroids in physiological fluids and tissues (S. J. Gaskell, V. J. Gould and H. M. Leith), trace analysis of cannabi- noids (D. J. Harvey), analysis of drugs in biological matrices (W. A. Garland and M. P. Barbalas) and neurotransmitters and related compounds (K. F. Faull and 0. Beck) using electron capture negative chemical ionisation GC-MS, and micro- determination of prostaglandins and thromboxane B2 by GC-high resolution selected ion monitoring MS (M.Ishiba- shi, K. Yamashita, K. Watanabe and H. Migazaki). Developments in the mass spectrometry of leukotrienes are dis- cussed in detail (R. c. Murphy and T. W. Harper). The roles of triple quadrupole MS-MS (J. V. Johnston, M. S. Lee, M. R. Lee, H. 0. Brotherton and R. A. Yost) and LC-MS and LC-MS-MS (J. Henion and T. Covey) in biomedical research are well represented. All the contributions are from estab- lished innovators in their respective fields. For the most part their contribu- tions summarise their own work and set it in the context of that of others. There is a good blend of qualitative (structural) and quantitative discussion. In summary, the book is very up-to- date, and leaves the reader with a clear impression of the role of modern mass spectrometry in biomedical research and the directions in which it might proceed in the near future. Apart from various symposia volumes this is the only book currently available which collects special- ist material of this nature into a single readable volume; hence it is a highly recommended reference work. R. P. Evershed University of Liverpool, UK

ISSN:0267-9477    

DOI:10.1039/JA987020352b

出版商:RSC    

年代:1987

数据来源: RSC