摘要:

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.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/JA98702FX017

出版商:RSC    

年代:1987

数据来源: RSC

摘要:

JASPE2 2(5) 417-510, 133R-166R (1987) August 1987 Journal of Analytical Atomic Spectrometry Including Atomic Spectrometry Updates CONTENTS NEWS AND VIEWS 417 Atomic Spectrometry Viewpoint-Roger Stephens 421 Conference Reports 423 Book Review 424 ASU Highlights-David Littlejohn 425 425 Conferences and Meetings 428 Papers in Future Issues Awards t o UK Atomic Spectroscopists PAPERS 429 435 441 447 45 1 455 459 463 469 473 48 1 485 49 1 497 503 509 Laser-excited Atomic Fluorescence Spectrometry in an Atomic Absorption Graphite Tube Furnace-Joseph P. Dougherty, Francis R. Preli Jr, Robert G. Michel Determination of Selenium by Graphite Furnace Atomic Absorption Spectrometry. Part 2. Role of Nickel for Analyte Stability-JiFi Dedina, Wolfgang Frech, Anders Cedergren, lngela Lindberg, Erik Lundberg Lead Atomisation from Soil by Slurry Introduction Electrothermal Atomisation Atomic Absorption Spectrometry.Part 1. Effects of Matrix Components on the Absorbance versus Time ProfileMichael W. Hinds, Kenneth W. Jackson Determination of Selenium in Serum by Electrothermal Atomisation Atomic Absorption Spectrometry with Deuterium-arc Background Correction-Barry Sampson Determination of Lead in Atmospheric Aerosols by Electrothermal Atomisation Atomic Absorption Spectrometry with Direct Introduction of Filters into the Graphite FurnaceM. Jose M. P. Moura, M. Teresa S. D. Vasconcelos, Adelio A. S. C. Machado Determination of Cadmium, Copper, Manganese and Rubidium in Plastic Materials by Graphite Furnace Atomic Absorption Spectrometry using Solid Sampling-Uwe Vollkopf, Raimund Lehmann, Dietmar Weber Electrothermal Atomisation Atomic Absorption Spectrometric Determination of Silver, Beryllium, Calcium, Iron, Lead and Tin in Uranium without Preliminary Separation- Neelam Goyal, P. J.Purohit, A. R. Dhobale, B. M. Patel, A. G. Page, M. D. Sastry Effect a f Organic Solvents on the Flame Atomic Absorption Spectrometry of Copper using Discrete Nebulisation of Mixed Aqueous Solutions-lsao Kojima, Chuzo lida Feasibility of Solid Sample Introduction by Slurry Nebulisation for Inductively Coupled Plasma Mass Spectrometry-John G. Williams, Alan L. Gray, Philip Norman, Les Ebdon Analysis of Geological Materials by Inductively Coupled Plasma Mass Spectrometry with Sample Introduction by Electrothermal Vaporisation.Part 1. Determination of Molybdenum and Tungsten-Chang J. Park, Gwendy E. M. Hall Analysis of Ferrous Alloys by Spark Ablation Coupled t o Inductively Coupled Plasma Atomic Emission Spectrometry-Alain Lemarchand, Guillaume Labarraque, Patrick Masson, Jose A. C. Broekaert Analysis of Coal Fly Ash and Environmental Materials by Inductively Coupled Plasma Atomic Emission Spectrometry: Comparison of Different Decomposition Procedures- Maurizio Bettinelli, U. Baroni, N. Pastorelli Rapid Determination of Eight Elements in Cement and its Raw Mixes by Inductively Coupled Plasma Atomic Emission Spectrometry-M. L. Fernandez Sanchez, J. Palacio Suarez, E. Fernandez Molina, Alfredo Sanz Medel High-accuracy Analysis by Inductively Coupled Plasma Atomic Emission Spectrometry using the Parameter-related Internal Standa.d rMethod-Michael H. Ramsey, Michael Thompson Low-Z Element Analysis by Soft X-ray Line Emission of a Laser-produced Plasma- Hedser van Brug, Fred Bijkerk, Marnix J. van Q COMMU NlCATlON Production of Two Inductively Coupled Plasmas from One Free-running High-frequency Genera t o r-S t a n I e y G re e n f i e I d , M a ry a n n e Tho m sen Wiel, Bob van Wingerden ATOMIC SPECTROMETRY UPDATE 133R 155R References Chemicals, Iron, Steel and Non-ferrous Metals-David Littlejohn, Howard J. Ellis, Hugh Hughes Typeset and printed by Black Bear Press Limited, Cambridge, EnglandJASPE2 2(5) 417-510, 133R-166R (1987) August 1987 Journal of Analytical Atomic Spectrometry Including Atomic Spectrometry Updates CONTENTS NEWS AND VIEWS 417 Atomic Spectrometry Viewpoint-Roger Stephens 421 Conference Reports 423 Book Review 424 ASU Highlights-David Littlejohn 425 425 Conferences and Meetings 428 Papers in Future Issues Awards t o UK Atomic Spectroscopists PAPERS 429 435 441 447 45 1 455 459 463 469 473 48 1 485 49 1 497 503 509 Laser-excited Atomic Fluorescence Spectrometry in an Atomic Absorption Graphite Tube Furnace-Joseph P.Dougherty, Francis R. Preli Jr, Robert G. Michel Determination of Selenium by Graphite Furnace Atomic Absorption Spectrometry. Part 2. Role of Nickel for Analyte Stability-JiFi Dedina, Wolfgang Frech, Anders Cedergren, lngela Lindberg, Erik Lundberg Lead Atomisation from Soil by Slurry Introduction Electrothermal Atomisation Atomic Absorption Spectrometry. Part 1.Effects of Matrix Components on the Absorbance versus Time ProfileMichael W. Hinds, Kenneth W. Jackson Determination of Selenium in Serum by Electrothermal Atomisation Atomic Absorption Spectrometry with Deuterium-arc Background Correction-Barry Sampson Determination of Lead in Atmospheric Aerosols by Electrothermal Atomisation Atomic Absorption Spectrometry with Direct Introduction of Filters into the Graphite FurnaceM. Jose M. P. Moura, M. Teresa S. D. Vasconcelos, Adelio A. S. C. Machado Determination of Cadmium, Copper, Manganese and Rubidium in Plastic Materials by Graphite Furnace Atomic Absorption Spectrometry using Solid Sampling-Uwe Vollkopf, Raimund Lehmann, Dietmar Weber Electrothermal Atomisation Atomic Absorption Spectrometric Determination of Silver, Beryllium, Calcium, Iron, Lead and Tin in Uranium without Preliminary Separation- Neelam Goyal, P.J. Purohit, A. R. Dhobale, B. M. Patel, A. G. Page, M. D. Sastry Effect a f Organic Solvents on the Flame Atomic Absorption Spectrometry of Copper using Discrete Nebulisation of Mixed Aqueous Solutions-lsao Kojima, Chuzo lida Feasibility of Solid Sample Introduction by Slurry Nebulisation for Inductively Coupled Plasma Mass Spectrometry-John G. Williams, Alan L. Gray, Philip Norman, Les Ebdon Analysis of Geological Materials by Inductively Coupled Plasma Mass Spectrometry with Sample Introduction by Electrothermal Vaporisation. Part 1. Determination of Molybdenum and Tungsten-Chang J. Park, Gwendy E. M. Hall Analysis of Ferrous Alloys by Spark Ablation Coupled t o Inductively Coupled Plasma Atomic Emission Spectrometry-Alain Lemarchand, Guillaume Labarraque, Patrick Masson, Jose A.C. Broekaert Analysis of Coal Fly Ash and Environmental Materials by Inductively Coupled Plasma Atomic Emission Spectrometry: Comparison of Different Decomposition Procedures- Maurizio Bettinelli, U. Baroni, N. Pastorelli Rapid Determination of Eight Elements in Cement and its Raw Mixes by Inductively Coupled Plasma Atomic Emission Spectrometry-M. L. Fernandez Sanchez, J. Palacio Suarez, E. Fernandez Molina, Alfredo Sanz Medel High-accuracy Analysis by Inductively Coupled Plasma Atomic Emission Spectrometry using the Parameter-related Internal Standa. d rMethod-Michael H. Ramsey, Michael Thompson Low-Z Element Analysis by Soft X-ray Line Emission of a Laser-produced Plasma- Hedser van Brug, Fred Bijkerk, Marnix J. van Q COMMU NlCATlON Production of Two Inductively Coupled Plasmas from One Free-running High-frequency Genera t o r-S t a n I e y G re e n f i e I d , M a ry a n n e Tho m sen Wiel, Bob van Wingerden ATOMIC SPECTROMETRY UPDATE 133R 155R References Chemicals, Iron, Steel and Non-ferrous Metals-David Littlejohn, Howard J. Ellis, Hugh Hughes Typeset and printed by Black Bear Press Limited, Cambridge, England

ISSN:0267-9477    

DOI:10.1039/JA98702BX019

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 informationiv NEWBOOKSFOR ORGANIC CHEMISTS Amino Acids and Peptides Vol. 18 This series was previously entitled ’Amino Acids, Peptides, and Proteins: The latest volume in the series covers the literature published on the subject during 1985.Brief Contents: Amino Acids; Peptide Synthesis; Analogue and Conformational Studies on Peptide Hormones and Other Biologically Active Peptides; Cyclic Modified and Conjugate Peptides; 8-Lactam Antibiotic Chemistry; Metal Complexes of Amino Acids and Peptides. Specialist Periodical Report Senior Reporter: J. H. Jones, University of Oxford Hardcover 314pp ISBN 0 85186 164 4 Price 264.00 ($96.00) RSC Members price €42.00 General and Synthetic Methods Vol. 9 Hardcover 134pp ISBN 0 85186 904 1 Price € 120.00 ($230.00) RSC Members price €65.00 Senior Reporter: G.Pattenden, University of Nottingham A review of the literature published during 1984. Brief Contents: Saturated and Unsaturated Hydrocarbons; Aldehydes and Ketones; Carboxylic Acids and Derivatives; Alcohols, Halogeno-compounds, and Ethers; Amines, Nitriles and Other Nitrogen-containing Functional Groups; Organometallics in Synthesis; Saturated Carbocyclic Ring Synthesis; Saturated Heterocyclic Ring Synthesis; Highlights in Total Synthesis of Natural Products; Reviews on General and Synthetic Methods. Specialist Periodical Report Topics in Lipid Research From structural elucidation to biological function Over the last decade many lipid chemists and biochemists have made a conscious effort to move from purely structural investigations to those which throw more light on the biological function of lipid molecules.For many years lipids were considered to be molecules containing just C, H and 0, related to fatty acids and hydrocarbons, with high oil-water partition co-efficients; more recently, however, it has been realized that the more complex structures such as glycolipids and lipoproteins, and indeed glycolipoproteins, are fascinating both as structural challenges and as functional elements of the cell. developments in lipid research. Brief Contents: Platelet Activating Factor; Eicosanoids; Glycolipids; Probes and Anaesthetics; Membrane Structure and Function; Environmental Adaptation. The book includes both reviews and research papers dealing with recent Edited by R.A. Klein and B. Schmitz Mol ten0 Inst. University of Cambridge Hardcover 348pp ISBN 0 85186 353 1 Price €37.50 ($65.00) RSC Members price €24.50 Chemical Aspects of Food Enzymes Softcover 326pp ISBN 0 85186 686 7 Price €37.50 ($72.00) RSC Members price €24.50 Edited by A. T. Andrews AFRC Institute of Food Research, Reading This publication reviews current applications of enzymes in food processes. It Contents: Enzyme Structure and Specifity: Factors Affecting Enzyme Activity and Kinetics; should stimulate interest and point the way forward in this area of vital importance. Genetic Engineering: Basic Considerations; The Potential for Chemical modifications of Enzymes; Applications of Immobilized Enzymes and Cells in the Food Industry; Encapsulation of Enzymes and other Agents in Liposomes; Developments in the Microencapsulation of Enzymes in Food Technology; Protein Engineering of Food Enzymes; Extending Enzyme Applications in the Food Industry; Enzymatic Modification of Lipids; Enzymatic Modification of Food Carbohydrates; Genetic Engineering of Lactic Acid Bacteria; The Molecular Biology of Plant Thiol Proteinases; Production of Heterologous Products in Escherichia coli and Yeast; Enzymic Modification of Dairy and Other Food Proteins; Biosensors: Principles and Potential; The SERC Biotechnology Directorate’s Programme in Protein Engineering; Food Enzymes: Industrial Potential and Scientific Challenges; Subject Index. 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ISSN:0267-9477    

DOI:10.1039/JA98702FP029

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年代:1987

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vii Applications of Spin - Spin C&plingi Nuclear Spin Relaxation in Liquids and Gases; Solid State N.M.R.; Natural Macromolecules; Synthetic Macromolecules; Conformational Analysis; Nuclear Magnetic Resonance of Living Systems; N.M.R. of Paramagnetic Species; N.M.R. of Liquid Crystals and Specialist Periodical Report Hardcover 569pp ISBN 0 85186 392 2 Price €99.00 ($149.00) Micellar Solutions. RSC members price €58.00 ROYAL SOCIETY OF C H EM I ST RY lnformat ion Services Ordering: RSC Members should send their orders to: The Royal Society of Chemistry, Membership Manager, 30 Russell Square, London WClB 5DT, UK. Non-RSC Members should send their orders to: The Royal Society of Chemistry, Distribution Centre, Blackhorse Road, Letchworth, Herts SG6 IHN, UK. Circle 010 for further information PITTSBURGH CONFERENCE 1988 NEW ORLEANS, 22-26 February 1988 The RSC Travel Club is organising an economical full service package for RSC Members and their colleagues attending the 1988 Pittsburgh Conference.Scheduled flights, hotel accommodation, coach transport between airports and hotels, courier service at airports and taxes will be included in the package price. Low cost personal itineraries can be arranged for those wishing to visit other cities in the USA, or take advantage of the opportunity for a holiday. Most visitors to New Orleans choose to stay in the French Quarter, where hotel accommodation is limited. The RSC Travel Club has already reserved rooms in the Monteleone Hotel, the most popular hotel in the French Quarter. Allocation will be on a first come, first served basis.If you or your colleagues are thinking of attending the 1988 Pittsburgh Conference, please contact us through the Reader Enquiry Service. We will send you full details of tour options and prices as soon as arrangements have been finalised with the airlines. IN SPECTURAL SOURCES High quality High intensity High spectural purity 0 High stability& long life Hollow cathode lamps at the lowest available prices! 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 to 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) 221 295. r Telex: 826932 Circle 005 for further information Circle 007 for further information... Vlll SPECTROCHIMICA MQLECULAR SIICTROSCOIY SPECTROCHIMICA ACTA Part B: Atomic Spectroscopy Editor-in-Chief: P W J M BOUMANS, Philips Research laboratories, Department of Spectrochernistry, PO Box 80.000,56OO JA Eindho ven, The Netherlands Edit o rs : W S LAV I N , Perkin -Elmer Corporation, USA and H OECHSNER, Univerity of Kaiserslautern, Federal Republic of Germany Assistant Editor: J A C BROEKAERT, lnstitut fur Spektrochemie und Angewandte Spektroskopie (ISAS), Federal Republic of Germany Spectroehimica Acta, Part B, covers topics from rapidly expanding areas in atomic spectroscopy, mass spectroscopy for inorganic analysis, and surface, interface, thin fiim and micro analysis.The articles deal with: theory and fundamentals, metho do tog y development, instrum en ta tion, and a p p k a tions. Recent years have seen the publication of an ever increasing number and variety of articles contributed by the teading authors in spectroscopy who have understood the impact of Spectrochimica Acta, Part B, on the development of atomic spectroscopy and related fields. Therefore the journat is an indispensable source of information for all analytical spectroscopists. Authors can feel assured that the submittance of their manuscripts is followed by fast, thorough and efficient refereeing, substantial editorial advice and rapid pubIication of the revised text in the journat with the longest tradition in spectroscopy and the unrivalled standard.Patents Section - The journal contains abstracts and i I I u st rat i on s of recent I y issued United States Patents and published patent applications filed from over 30 countries under the Patent Co-operation Treaty. Subscription Information Published monthly (Volume 42) Annual subscription (1987) DM 1245.00 Two-year rate t 1987/88) DM2365.50 A selection of papers An automated direct sample insertion system for the inductively coupled plasma, W E PETTIT& G HORLICK. A steady-state approach to evaluation of proposed excitation mechanisms in the analytical ICP, G D RAYSON & G M HIEFTJE.The determination of trace elements in geochemical exploration samples by ICP- MS, A R DATE & D HUTCHtSON. Interference minimization using second surface atomizer for furnace atomic absorption, T M RETTBERG & J A HOLCOMBE. Spatial resolution enhancement for linear p hotodiode array atomic spectrometry, S W McGEORGE & E D SALIN. Experimental control of the solvent load of lCPs and effects of chloroform plasma load on their analytical performance, F J M 3 MAESSEN etal. Influence of the generator frequency and the plasma gas inlet area on torch design in J M MERMET. An improved interface for ICP-MS, D J DOUGLAS & J B FRENCH. Scanning electron microscopy studies on surfaces from electrothermal AAS, B WELZI et al. Qualitative and semi-quantitative ICAP-AES analysis using a computer-controlled monochromator, P D P TAYLOR & J DE DONDER.tCP-AES, E MICHAUD-POUSSEL & Pergamon Press FREE SAMPLE COPIES AVAiLABtE ON REQUEST Advertising rate card avaitabte on request. Back issues and current subscriptions are also available in microform. The Deutsch Mark prices shown inctude postage and insur- ance. For subscription rates in Africa, Asia, Australasia, UK and Eire and the Americas apply to your nearest Pergamon Headington Hill Hall, Oxford OX3 OBW, UK Fairview Park, Elmsford, New York 70523, USA 5A. 17 10,86 office. Prices are subject to change without notice. Circte 01 1 for further information... Vlll SPECTROCHIMICA MQLECULAR SIICTROSCOIY SPECTROCHIMICA ACTA Part B: Atomic Spectroscopy Editor-in-Chief: P W J M BOUMANS, Philips Research laboratories, Department of Spectrochernistry, PO Box 80.000,56OO JA Eindho ven, The Netherlands Edit o rs : W S LAV I N , Perkin -Elmer Corporation, USA and H OECHSNER, Univerity of Kaiserslautern, Federal Republic of Germany Assistant Editor: J A C BROEKAERT, lnstitut fur Spektrochemie und Angewandte Spektroskopie (ISAS), Federal Republic of Germany Spectroehimica Acta, Part B, covers topics from rapidly expanding areas in atomic spectroscopy, mass spectroscopy for inorganic analysis, and surface, interface, thin fiim and micro analysis.The articles deal with: theory and fundamentals, metho do tog y development, instrum en ta tion, and a p p k a tions. Recent years have seen the publication of an ever increasing number and variety of articles contributed by the teading authors in spectroscopy who have understood the impact of Spectrochimica Acta, Part B, on the development of atomic spectroscopy and related fields.Therefore the journat is an indispensable source of information for all analytical spectroscopists. Authors can feel assured that the submittance of their manuscripts is followed by fast, thorough and efficient refereeing, substantial editorial advice and rapid pubIication of the revised text in the journat with the longest tradition in spectroscopy and the unrivalled standard. Patents Section - The journal contains abstracts and i I I u st rat i on s of recent I y issued United States Patents and published patent applications filed from over 30 countries under the Patent Co-operation Treaty.Subscription Information Published monthly (Volume 42) Annual subscription (1987) DM 1245.00 Two-year rate t 1987/88) DM2365.50 A selection of papers An automated direct sample insertion system for the inductively coupled plasma, W E PETTIT& G HORLICK. A steady-state approach to evaluation of proposed excitation mechanisms in the analytical ICP, G D RAYSON & G M HIEFTJE. The determination of trace elements in geochemical exploration samples by ICP- MS, A R DATE & D HUTCHtSON. Interference minimization using second surface atomizer for furnace atomic absorption, T M RETTBERG & J A HOLCOMBE. Spatial resolution enhancement for linear p hotodiode array atomic spectrometry, S W McGEORGE & E D SALIN. Experimental control of the solvent load of lCPs and effects of chloroform plasma load on their analytical performance, F J M 3 MAESSEN etal.Influence of the generator frequency and the plasma gas inlet area on torch design in J M MERMET. An improved interface for ICP-MS, D J DOUGLAS & J B FRENCH. Scanning electron microscopy studies on surfaces from electrothermal AAS, B WELZI et al. Qualitative and semi-quantitative ICAP-AES analysis using a computer-controlled monochromator, P D P TAYLOR & J DE DONDER. tCP-AES, E MICHAUD-POUSSEL & Pergamon Press FREE SAMPLE COPIES AVAiLABtE ON REQUEST Advertising rate card avaitabte on request. Back issues and current subscriptions are also available in microform. The Deutsch Mark prices shown inctude postage and insur- ance. For subscription rates in Africa, Asia, Australasia, UK and Eire and the Americas apply to your nearest Pergamon Headington Hill Hall, Oxford OX3 OBW, UK Fairview Park, Elmsford, New York 70523, USA 5A. 17 10,86 office. Prices are subject to change without notice. Circte 01 1 for further information$5.2 I 22g BUSINESS REPLY SERVICE Licence No. WD 106 Reader Enquiry Service Journal of Analytical Atomic Spectrometry The Royal Society of Chemistry Burl i ngton House, Piccadil ly LONDON WIE 6WF England 9 TELEPHONE NO I I I I I I 2i I I I I I I I I I I I I I I I I I I I I I 2. g 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

ISSN:0267-9477    

DOI:10.1039/JA98702BP033

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年代:1987

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JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, AUGUST 1987, VOL. 2 133R ATOMIC SPECTROMETRY UPDATE-CHEMICALS, IRON, STEEL AND NON-FERROUS METALS David Littlejohn+ Department of Pure and Applied Chemistry, University of Strathclyde, Cathedral Street, Glasgow GI IXL, UK Howard J. Ellis 23 Blake Avenue, Ross-on- Wye, Herefordshire HR9 5JP, UK Hugh Hughes 2 The Rise, Trearddur Bay, Holyhead, Anglesey, Gwynedd LL65 2UY, UK Summary of Contents 1 Chemicals 1.1. Petroleum and Petroleum Products 1.1.1. Petroleum 1.1.2. Lubricating oils 1.1.3. Gasoline Table 1.1. Summary of Analyses of Petroleum and Petroleum Products 1.2. Chemicals and Miscellaneous Materials 1.2.1. Organic chemicals 1.2.2. Inorganic chemicals 1.2.3. Microelectronic components 1.2.4. Gases, acids and solvents 1.2.5. Nuclear fuels and related materials 1.2.6.On-line process control Table 1.2. Summary of Analyses of Chemicals and Miscellaneous Materials 2 Iron and Steel 2.1. Atomic Emission Methods 2.2. Atomic Absorption Methods Table 2. Summary of Analyses of Iron and Steels 3 Non-ferrous Metals 3.1, Atomic Emission Methods 3.1 .l. Arc methods 3.1.2. Spark methods 3.1.3. Plasma methods 3.1.4. Discharge lamp methods 3.2. Atomic Absorption Methods 3.3. Atomic Fluorescence Methods Table 3. Summary of Analyses of Non-ferrous Metals This review describes developments in atomic spectrometry relevant to the analysis of chemicals, iron, steel and non-ferrous metals. It is based on publications and conference reports received during the year ending December 1986. The review therefore follows chronologically from the Atomic Spectrometry Update published in JAAS, Volume 1 (J.Anal. At. Spectrorn., 1986,1,87R). The full references, names and addresses of authors can be found from the Atomic Spectrometry Updates References in JAAS, Volume 1, Issues 4-6 (86/1031-86/2039) and Volume 2, Issues 1, 3 and 4 (87/1-87/1169). An abbreviated form of each literature reference quoted in this review (except for those to Conference Proceedings) is given at the end. The format of the review is the same as last year. * Review Topic Co-ordinator, to whom all correspondence should be addressed.134R JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, AUGUST 1987, VOL. 2 1. CHEMICALS Research published during 1986 in the broad area of chemicals analysis has been reviewed under the same categories as last year.There was an over-all reduction in the number of papers received and most of the abstracts either described the application of recently introduced instrumentation or pro- vided an update on established lines of research. The development and application of ICP-AES procedures con- tinue to grow in importance and the most interesting research in this area concerned instrument automation and advances in on-line process control. Separation and pre-concentration routines are still widely used, even with ICP-AES and ETA-AAS methods, which indicates that matrix interference and sensitivity problems are still frequently encountered in many analyses. 1.1. Petroleum and Petroleum Products Table 1.1 summarises the papers concerning petrochemicals analysis reported in Atomic Spectrometry Updates References in JAAS, Volume 1, Issues 4-6 and Volume 2, Issues 1 , 3 and 4.The number of papers reviewed was substantially smaller than last year and no major developments were reported. The application of ICP-AES to the analysis of petroleum and lubricating oils continues to attract attention and the problems of particle size effects in the determination of wear metals have been reconsidered. 1.1.1. Petroleum Although there were comparatively few new proposals of any significance in the area of petroleum analysis, a number of papers described some interesting developments in the application of inductively coupled plasmas in atomic emission spectrometry and mass spectrometry. Xylene is a widely used solvent in oil analysis by ICP-AES, but errors may be encountered if the sample solutions and calibration standards are not reasonably well matched with respect to oil content and type. For example, a 5-2570 suppression effect was observed (86K1160) for elements contained in a 20% m/V solution of base oil in xylene.It was suggested that increasing amounts of heavy oils in xylene produce a significant plasma cooling effect that suppresses the emission intensities of “hard” lines to a greater extent than for “soft” lines. By replacing xylene with tetralin, which has a lower vapour pressure but similar solvent properties to xylene, no plasma cooling effect was observed and no more than a 3% suppression of analyte intensities occurred when aspirating tetralin solutions of heavy oils into the ICP. These observa- tions can be explained by considering the thermodynamics of the atomisation processes and the organic aerosol - vapour loading of the ICP.Organic solutes or solvents having higher WC ratios require higher atomisation energies and according to the author, a xylene aerosol - vapour stream may consume 10-20% of the total plasma power available under typical operating conditions. It was suggested therefore that tetralin was the preferred solvent for the analysis of heavy fuel oils and lubricating oils. proposed (86/C1577) for the determination of trace metals in oil by ICP-AES. A robotic arm was used to weigh and dilute the sample, add an internal standard and then introduce the solution to the ICP-AE spectrometer. Operating parameters such as power, nebuliser flow-rate, viewing height and wavelength were optimised under computer control. During the analysis of one sample, the next specimen was prepared by the robotic arm.A similar ICP system was developed (86/C1157) based on a direct-reading spectrometer and flow injection sample introduction. A robot weighed an aliquot of the oil, dispensed a known mass of xylene, mixed the solution and placed the container in a sample tray. A 25-200 p1 volume was then automatically injected into a flowing xylene stream which was aspirated into the plasma. It was claimed that automation of the complete procedure improved productivity and precision, and reduced torch maintenance and the need for frequent re-calibration. The removal of metals, sulphur and nitrogen from crude oils is an important step in the manufacture of marketable products.The coupling of size-exclusion chromatography and inductively coupled plasma atomic emission spectrometry (SEC - ICP-AES) can provide significant information on the molecular size distributions of compounds of these and other elements of interest (see JAAS, 1986, 1, 88R). As might be expected, not all of the bulk concentrations of Fe, Ni, V, etc. are organically bound, and so considerable discrepancies often exist between the concentrations obtained for “total” metal and the values obtained chromatographically. A study was undertaken (86K1162) to investigate changes in metal speciation that are caused by refining procedures. Chromato- graphic analysis of fractions obtained by extraction and short-path distillation showed that V compounds in unprocessed crude oils fall into three distinct size regimes, with the smallest in size being the metalloporphyrin com- ponent.The variation in the relative contribution made to the bulk V content of a crude oil by each size regime was found to be considerable, with younger, immature crude oils usually having the greatest porphyrin content. Subsequent catalytic or thermal processing of the crude oils resulted in distinctly different profiles. In comparison, Ni profiles were much less distinct, and only marginal resolution of the metalloporphy- rins was reported. In contrast to V, the Ni metalloporphyrins normally contributed a smaller fraction of the total metal. The authors reported that up to 50% of the bulk Fe did not undergo chromatographic separation and the organically bound Fe that did exist was associated with the largest size components of the crude oil.The chromatographic detection limits reported for Fe, Ni and V (as tetraphenylporphene complexes) and S (as dibenzothiophene) were in the range 10-40 p.p.m. It has been suggested (861C1476) that inductively coupled plasma mass spectrometry (ICP-MS) can be used to determine the concentrations of Ag, As, Ba, Cd, Cr, Hg, Pb and Se in crude oils and fuel oils with a significant decrease in analysis time compared with standard instrumental methods based on Hy-AAS, ETA-AAS and ICP-AES. According to the author, a combination of these optical techniques would be required to determine the above list of elements at the levels present in most petroleum-based samples.Although the ICP-MS analy- sis of NBS SRM 1634A (a residual fuel oil) resulted in an average error of 18% when compared with the certified values, it was claimed that the agreement at low concentra- tions was better than a similar analysis by ICP-AES. 1.1.2. Lubricating oils In the determination of additive and wear metals in lubricating oils, interest has been focused on the development of direct methods that are insensitive to the size effects of metal particles present in the used oils. A modified Babington nebuliser was constructed (86/1463) which was capable of producing an aerosol directly from undiluted oils, for intro- duction into an ICP. A small heater incorporated in the nebuliser increased the temperature of the sample stream prior to nebulisation, which increased the output of aerosol and reduced variations in analyte emission intensity due to differences in oil type and viscosity.It was shown that the type of organometallic complex used €or the preparation of standards was unimportant if the plasma observation region was properly optimised by, for example, a Simplex method (87/C212). When the modified Babington nebuliser was used in the analysis of used lubricating oils, the concentrations of Fe obtained were on average 61 YO of the values obtained after dryJOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, AUGUST 1987, VOL. 2 135R ~~ Table 1.1. SUMMARY OF ANALYSES OF PETROLEUM AND PETROLEUM PRODUCTS Technique ; atomisation; analyte form* AE; ICP; L Element h/nm Matrix Concentration Diesel engine oil - Sample treatmentlcomments Reference Ag (for Cl) As As Cd c u Fe K Pb - - 197.7 - - - 766.490 283.3 Method to assess oil consumption of engine; fumes scavenged with Ag to give AgCl which was analysed 8611064 8611056 871C1101 87/86 8611 722 8611722 861C 1577 8611629 Fats and petroleum Trace levels products AA; Hy; G AA; ETA; L Decompose in O2 bomb, acid digest and reduce to form hydride under automatic control Pipette 20 ml into a 250-ml separating funnel, add 5 ml5% iodine in toluene, shake and leave for 60 s; add 10 ml1% HNO, and extract for 60 s; repeat two separate extractions, combine aqueous phases, evaporate, add 10 ml1% HN03 and inject 20-yl volumes; add 10 ~ 1 1 % Ni(N03)2 for within-tube matrix modification for As Direct method using platform atomisation and Zeeman-effect background correction Petroleum and 6(1-100 pg 1-1 gasoline Crude oil and petroleum products 0.03-0.17 pg 1-1 Lubricating oil - AA; ETA; L AA;-; L AA; -; L AE; ICP; L Ignite at 600 _+ 50 "C for 3-4 h; dissolve ashes in concentrated HCl or 3 + 1 HCl - HN03 See Cu, ref.860722 Description of system that automatically weighs, dilutes, mixes and introduces the sample to tht! ICP Method for tetraalkyl and ionic alkyl Pb; complex ionic alkyl Pb with 0.5 M Na diethyldithiocarbamate, followed by extraction into hexane, derivatisation with butyl- or propyl-magnesium chloride to give tetraalkyl Pb compounds. Hexane extract separated by GC (column: 10% OV-101 on Chromosorb W) 50 ml propan-2-01 by dilution to 100 ml with H20; aspirate and analyse using either standard additions or standards prepared from Pb-free gasoline Total Pb as PbEt, and PbMe, is determined after decomposition with a mixture of mercaptoacetic acid (HSCH2C02H) and NaN02 in the presence of HC1 Treat with iodine and Aliquat 336 (tricaprylammonium chloride), dilute with 4-methylpentan-2-one and inject 100 pl into a flowing acetone stream aspirated into an AA spectrometer Evidence of organolead hydride formation during the reduction step with NaBH,; method applied to solutions containing R,Pb+ and R2Pb2+ compounds Emulsify a mixture of 1 ml gasoline and (R = CH3, CH3CHZ) See As, ref.871C1101 Lubricating oil - Oil - - >0.1 ng AA; GC-heated silica cell; G Pb 217.0 Gasoline > 0.07 mg 1-1 AA; F; -; L 8612032 Pb 217.0 8719 Gasoline 256-328 p.p.m.Gas o 1 in e 300-400 mg 1-1 AA; F, air - C2H2; L Pb AA; F, -; L 87185 Alkyllead solutions >5 ng 1-1 AA; Hy; G 871482 Pb AA; ETA; L AA; Hy; G AA; Hy; G 87lC1101 8611056 87187 Pb Se Se 283.3 Petroleum and 5.3-21.2 pgl-1 Fats and petroleum Trace levels Coal 0.4-2.6 mg kg-1 gasoline products See As, ref. 8611056 Decompose with H2S04 - HN03, with application of a cooling system; eliminate interference of NO, on Se by use of H2NS03H; increase efficiency of Se*V reduction by NaBH, with addition of I- Add 100 p1 HCI to 1 g in a dry tube, heat in an ultrasonic bath for 10 min at 60-80 "C, add 10 p1 HN03 and treat again in bath; cool and dilute 10 ml with 2 + 1 xylene - butylcellosolve K added to minimise ionisation effects Automatic dilution, flow injection sample introduction and simultaneous multi-element analysis ICP analysis with toluene, xylene or tetralin Automated system for sampling, dilution and Study of matrix effects when samples diluted Various - Lubricating oils - AE; ICP; L 8611063 Various - Various - Lubricating oils mg g-1 level Lubricating oils - AA; F, -; L AE; ICP; L 8611065 86lC1157 Various - Lube and heavy - Lube and heavy fuel oils fuel oils pg g- levels AE; ICP; L AE; ICP; L 86/C1158 86lC1160 Various - (21)136R JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, AUGUST 1987, VOL.2 Table 1.1. SUMMARY OF ANALYSES OF PETROLEUM AND PETROLEUM PRODUCTS-continued Technique; atomisation; analyte form* AE; SEC - ICP; L Matrix Crude oils Concentration p.p.m.levels Sample treatmentlcomments used in the size-exclusion chromatographic separation of Fe, Ni and V tetraphenylporphine complexes; S as dibenzothiophene was also measured Heat samples prior to nebulisation into an ICP via a modified Babington nebuliser Dilute with xylene; add 2% 0, to the Ar auxiliary gas flow to remove trace amounts of carbon in determination of Ag, As, Ba, Cd, Cr, Hg, Pb and Se Anode is in the form of a graphite braid on to which the sample is deposited; the braid forms a miniature conveyor belt Inject 30 pl on to disc-shaped graphite lobes of a rotating disc cathode; ash as the cathode is rotated at 100 rev min- and resistively heated; arc each lobe in conjunction with a graphite anode for determination of Ag, Al, Cr, Cu, Fe, Mg, Mo, Ni, Si, Sn and Ti Determination of various volatile organometallic species including organoselenium compounds Dilute with xylene; use Simplex optimisation to determine best conditions for 14 wear metals and 3 additives Samples were vaporised from a small graphite o-Xylene - pyridine - o-cresol mobile phase Reference 86lC1162 Element Wnm Various - (4) Lubricating oils Fuel oil AE; ICP; L MS; ICP; L 463 476 518 Various - 861 861C 861C - Trace levels Various - (8) Trace levels pg ml-1 levels AE; d.c.arc plasma; L Various - Lubricating oils Lubricating oils AE; d.c. arc; L 86/C1520; 87lC558 Various - (11) Various - Coal conversion products AE; GC - ICP; G AE; ICP; L AE; ICP; L 87/88 87lC2 12 871232 Various - (17) Lubricating oils Lubricating oils pg g-1 levels Various - ( 5 ) crucible heated between two electrodes, and the vapours passed into an ICP for determination of Ca, Cu, Fe, Mg and Mn enhanced by adding 1 part S to 5 parts sample and impregnating the graphite electrode with 1 M CaC1, Sensitivity for Co, Mo, Ni and V is 871577 Coal hydrogenation products AE; arc; S Various - (4) * Hy indicates hydride generation and S, L and G signify solid, liquid or gaseous sample introduction, respectively. Other abbreviations are listed elsewhere.ashing of the sample and dissolution of the residue. The discrepancy was ascribed to particle size fractionation in the spray chamber, where a substantial portion of the larger metal particles were deposited and hence not transferred into the plasma. In an attempt to reduce the effects of fractionation, these workers inverted the ICP geometry so that the spray chamber was located above the torch.This configuration produced good agreement between the Fe concentrations obtained by direct nebulisation and after dry ashing of the lubricating oils. An alternative approach (871232) proposed the use of a small graphite crucible heated between two graphite electrodes for electrothermal vaporisation of base oils into a high-power Ar - N2 ICP. No particle size effects were encountered in the determination of Fe in lubricating oil for samples containing particles up to 25 pm in diameter. In this respect the proposed method had advantages over direct nebulisation. The best results were obtained using organo- metallic standards in oil, but for some elements aqueous standard solutions could be used.It was suggested (86/C1518) that a graphite filament DCP could provide information about the size distribution of wear metal particles in used lubricating oils as the graphite fibres served as a depth filter. The largest particles were trapped near the surface of the fibre at the point of sample delivery, whereas particles of intermediate size flowed further along the filament before being trapped. Particles that were much smaller than the inter-fibre spacing spread along the fibre with the soluble species and became immobilised only when the sample was fully desolvated. A new technique for arc AES was proposed (86/C1520, 87/C558) which allowed the direct introduction and analysis of fuel oils and engine lubricants. The cathode of the new source consisted of a row of ten disc-shaped lobes, 0.5 cm wide, machined from a graphite rod 10 cm long by 1.2 cm diameter. Aliquots (30 p1) were pipetted on to each lobe and the rod rotated and resistively heated to ash the samples.These features prompted the authors to call the source an “ashing rotrode.” A second graphite rod 0.6 cm in diameter served as the anode. The volume of sample dispensed on to the rotating electrode was considered critical as emission intensity was a non-linear function of sample volume. The ashing rotrode seemed to exhibit particle size effects for some (but not all) elements according to the authors. Detection limits quoted for 11 wear metals measured simultaneously using a 14-channel polychromator were in the range 0.03-0.8 pg ml-1, although these values were derived from the analysis of an organometallic standard solution.1.1.3. Gasoline No significant developments in the analysis of gasoline were reported, but a number of modified atomic absorption spectrometry procedures were proposed for the determination of total Pb. Decomposition of tetraalkyllead species by extraction with a mixture of mercaptoacetic and nitrous acids in the presence of hydrochloric acid (87/9) allowed the analysis of motor spirit using aqueous standards. In an alternative approach (87/85), gasoline was treated with iodine and Aliquat 336 (tricaprylammonium chloride) prior to dilution with 4-methylpentan-2-one and injection into a flowingJOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, AUGUST 2987, VOL.2 137R acetone stream aspirated into an air - C2H2 flame. The formation of an aqueous gasoline emulsion was also proposed as a rapid method for the direct determination of total Pb by AAS (8612032). Of the five emulsions tested, the best results were obtained with a mixture of 1 ml of gasoline and 50 ml of propan-2-01 diluted to 100 ml with H20. Calibration standards were prepared either from organic lead compounds or a solution of lead-free gasoline and lead nitrate. Emulsions could also be prepared with ethanol and gasoline, but addition of a surfactant was required. The Pb detection limits of the Aliquat 336 and emulsion procedures were similar at about 0.1 pg ml-1. 1.2. Chemicals and Miscellaneous Materials There has also been a reduction in the number of papers received that described developments in general chemicals analysis.A summary is presented in Table 1.2. The most exciting innovation reported was the application of an air ICP that has advantages in the AES analysis of organic materials and can be deployed in on-line analysis. The general use of ICP-AES continues to expand and further examples of simultaneous and rapid sequential multi-element analyses were provided. Although sample preparation and pre-concen- tration procedures are still widely used, especially in the analysis of nuclear materials, advances in ETA-AAS technol- ogy have allowed the direct analysis of some solid samples. The need for speciation of the analyte in a variety of applications prompted the development of a number of hybrid procedures.1.2.1. Organic chemicals In the analysis of polymers and plastics, decomposition procedures are normally required to convert the sample into a form that will allow the accurate determination of trace metals. A variety of procedures have been reported that simplify the preliminary treatment of polymeric materials prior to analysis by atomic spectrometry. Alkaline earth and lead sulphates precipitated during the treatment of poly(viny1 chloride) (PVC) with H2SO4 and H202 were taken back into solution by treatment with EDTA in ammonia solution (87/406). The procedure was applied to the accurate determi- nation of Al, Ca and Sb in PVC by AAS. The determination of Sb in PVC was achieved (87/353) without destruction of the organic material by dissolving the sample in a solution of HCl- DMF.Treatment with NaBH4 in DMF resulted in the production of SbH3 which was decomposed in a quartz tube prior to AAS analysis. Although a combination of dry and wet ashing is suitable for the pre-analysis preparation of various polymers (86/1406) and surfactants (87/576), many organic samples require more rigorous treatment. A method was suggested for the determination of As and Se in polyethylene by Hy-AAS following semi-automated decomposition in an oxygen bomb (86/1056). High-pressure decomposition was also required for pharmaceutical samples of carboxymethyl- cellulose and ethylcellulose, prior to ICP-AES analysis (86/1419). However, ETA-AAS methods were reported that allowed direct analysis of polymers without chemical pre- treatment.A cup-in-tube procedure was used (871659) to measure the concentrations of Cu, Mn and Rb in mg amounts of polyesters and polyamides. The sample was placed in a pyrolytically coated graphite crucible that was positioned inside a modified ETA tube in place of a L’vov platform. The authors claimed that the results agreed well with concentra- tions obtained by FAAS. A similar method was used to determine Cr, Cu, Ni and Pb in polyethylene (86/1803) by depositing S1 mg of sample into a graphite boat that was placed inside a graphite oven. A series of methods for the determination of metals inpaints have been produced by the British Standards Institution; most are based on dry ashing or extraction procedures prior to analysis by FAAS. The methods include the determination of soluble Ba (87/282), Cd (87/283), Hg (87/285), Pb (87/280), Sb (87/281) and total Cr (87/284) and Pb (87/279).The formation of an emulsion was proposed as a simple method for the determination of Co and Pb in paints by FAAS following mineralisation of the organometallic driers with HN03 (871 83). It has also been suggested (87/C1086) that the stability of emulsions formed with hydrocarbon and halohydrocarbon solvents can be improved by addition of ethoxylated nonyl- phenols. Of course in many organic analyses, it is preferable not to decompose the sample, particularly if speciation of the metal containing compounds is required. A GC - ICP-AES system was developed for the determination of volatile organometal- lic compounds in complex mixtures (87/88).The main topic of interest was the identification of organoselenium compounds in coal gasification by-products. An ICP was also coupled to a gel chromatograph (87/407) for the separation and determina- tion of organosilicon compounds in anti-foaming agents, car polish and cosmetics. Eluate from the Sephadex LH-60 column was collected in 5-ml fractions that were aspirated into the ICP. The combination of GC with low-pressure and atmospheric pressure MIPS allowed the identification of various pesticides by measurement of nonmetal emission in a He plasma (86/C1150). The atmospheric pressure Beenakker detector was found to be somewhat more sensitive for C1 than the low-pressure Evenson system, but overall an electron- capture detector was more sensitive than either of the MIP systems by 2-3 orders of magnitude. There continues to be occasional interest in the use of atomic spectrometry for the indirect determination of organic species.The methods reported during the past year include the micro-determination of pilocarpine by the AAS analysis of a mercury-containing complex (87/317), the indirect determina- tion of streptomycin by the formation and detection of a Cu complex (87/245), the formation of Fe ion-pair complexes for the indirect determination of avacine, papaverine, diphen- hydramine and amylocaine by AAS (87K174) and the formation of Hg complexes of cinchona alkaloids with subsequent analysis by AAS (86/1393). Ion-pair formation has also been used for the indirect determination of bromhexine by AAS measurement of Co following reaction with the inorganic complex CO(SCN)~*- (8611465).1.2.2. Inorganic chemicals A considerable number of abstracts were received that described methods for the analysis of inorganic chemicals and materials. Unfortunately, very few of the papers were of any significance and it seems that there has been unnecessary publication of established arc and FAAS procedures on a major scale. Indeed, the only developments in this area worth mentioning involve modifications that improve the determina- tion of elements present at trace levels in catalysts and chemicals. The separation of Sb3+ from Sb5+ was achieved by complexation of Sb3+ with NaDDC at pH 9.5 and extraction into IBMK (87/487). For determination of trace total Sb concentrations, complexation with APDC into IBMK was proposed.It was claimed that the ICP-AES detection limits of 14 trace elements in nickel-plating electrolytes could be improved 5-10 fold by extraction of the impurities with trialkylbenzylammonium chloride in o-xylene in the presence of C1- and S042- (86/1786). An ion-exchange procedure was proposed (87/382) for the separation of Pb from major amounts of Ga, In, Zn and other elements in analytical- reagent grade chemicals. The Pb was retained on a short column of AG1-X4 anion-exchange resin in the bromide form while the other elements were eluted with 0.2 M HBr. The Pb was then eluted with 2 M HN03 for FAAS analysis. A procedure was reported (87/490) for the removal of trace amounts of Cd and Cu from solutions containing tartaric acid,138R JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, AUGUST 1987, VOL. 2 Table 1.2.SUMMARY OF ANALYSES OF CHEMICALS AND MISCELLANEOUS MATERIALS Technique ; atomisation; analyte form* air - C2H2; L AA; F, Matrix Concentration Sample treatmentlcomments Reference Element A1 3Jnm 309.3 871406 8611369 871476 871575 87/282 87tC783 871C791 871101 871406 86/1406 86/18 10 871283 871454 87t490 87lC79 1 8611456 8611465 87/83 8611650 871284 871608 871245 871490 Heat 0.1 g for 15 min with 2 ml concentrated H2S04, add dropwise 5 ml30% H202, boil to remove excess of H202 and cool; treat solution with 10 ml concentrated NH, and 10 ml4% EDTA; use method of standard additions for A1 only HC1 using a petroleum fraction (boiling range 150-220 "C), obtained from crude oil, that contains 0.2% S and 19% aromatic hydrocarbon Atomisation greatly improved (up to x 100) by addition of ascorbic acid and Ti; only slight interference from S10 mg ml-1 U Prepare sample as in BS 3900: Part B5 Extract Au from liquors adjusted to 0.1-3 M - Poly( vinyl - chloride) Au 242.8 Liquors AA; F, air - C2H2; L AA; ETA; L As Aqueous solutions S20 pg ml- * B Ba 249.8 553.5 Liquid fertilisers 0.1-1% Paints 0.05-5 YO mlm Gunshot residue Trace levels soluble Ba swabs AA; -; - AA; F, N20 - CZH2; L AA;-;L AE; ICP; L Extract analyte from swab or ash at low temperature followed by dissolution of the residue Samples injected directly into axial channel of ICP torch via a gas sampling valve and a low dead volume interface Add 10 ml H20, 2 drops 0.1 % p-nitrophenol to 1 g LiOH, followed by addition of 1 + 1 HNO, to slightly acidic and then 1 ml in excess; heat to dissolve, cool, add 2.5 ml 50 mg ml-l Sr and 10 ml10% NH4CI and dilute to 50 ml with H20 See Al.ref. 871406 Ba AE; ICP; G Br Freon-type gases >ng range and SF6 Ca Lithium hydroxide - AA; F, -; L Poly(viny1 chloride) - AA; F, air - C2H2; L AA;-;- AA. _ * - 9 , Ca 422.7 Cd Cd Plastics >mg kg-* levels Denture polymers - Dry ash and dissolve in 1 M HCI Concentration of Cd extracted by food simulants, saliva and gastric acid was measured Prepare sample as in BS 3900: Part B5 Paints 0.055% mlm soluble Cd Enamelled - Organic acids, Trace levels tableware inorganic chloride and sulphate salts Cd Cd Cd 228.8 AA; F, AA; ETA; L air - C2H2; L Leach analyte from enamel by boiling in 4% Adsorb analyte on to thin layers of ZnS and acetic acid dissolve in hot HNO, - HC1- H20 (1 + 1 + 2); method for preparation of ZnS given See Br, ref.871C791 AA; -; L AE; ICP; G c1 c o Freon-type gases and SF6 Solutions >ng range vg ml-1 levels AA; F, air - C,H2; L Form complex with acenaphthenequinone and adsorb at pH 6.5 on naphthalene; filter, dissolve in DMF - HN03 and aspirate bromohexine and CO(SCN),~- and measure Co in the 1,2-dichloroethane organic phase Extract the ion pair formed between AA;-;L Co(for 240.7 indirect bromo- hexine) c o - Bromo hexine Paint and varnish driers AA;-;L Emulsify solution formed after mineralisation of organo-analyte compounds with concentrated HNO, fragments <10 mg; weigh and place into the atomiser; ash to remove As and atomise at 2850 "C; used Smith - Hieftje background correction Etch slices of GeAs, wash and shatter into Prepare sample as in BS 3900: Part B5 - Cr Gallium arsenide AA; ETA; S Cr 357.9 Cr - Paints Catalysts 0.05-5% mtm total Cr AA; F, N20 - C2H2; L AA; F, -; L A catalyst used to convert ethylbenzene into styrene was dissolved in HNO, - HF, evaporated to dryness, dissolved in hot HC104 and 1 + 1 HCI, and analysed; 10% Na2S04 added to suppress interferences Indirect method for determination of streptomycin See Cd, ref.871490 - c u c u - Copper(I1) - streptomycin Organic acids, inorganic chloride and sulphate salts AA; F, -; L AA; -; L - Trace levelsJOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, AUGUST 1987, VOL. 2 139R Table 1.2. SUMMARY OF ANALYSES OF CHEMICALS AND MISCELLANEOUS MATERIALS-continued Element Unm c u - Fe 248.3 Hf - Hf - Hg(for 253.7 indirect alka- loids) - Hg Hg(for - indirect Br) Hg 253.7 - K 6Li 670.8 Technique; atomisation; Matrix Concentration analyte form* Sample treatmentlcomments Reference Plastics Trace levels AA; ETA; S Cup-in-tube procedure using a modified 871659 platform atomiser tube and a pyrolytic graphite coated graphite crucible papaverine, diphenhydramine and amylocaine through formation of ion pairs with Fe(SCN),3- and extraction into 1,2-dichloroe t hane 8-hydroxyquinoline - 5-sulphonic acid as a chelating agent; elute Zr with 2 M H2S04 and elute Hf with more concentrated H2S04 or oxalic acid determination by eliminating flame destabilisation effects quinine, quinidine, cinchonine and cinchonidine Organic solutions mg ml-1 levels AA; F, -; L Indirect method for determination of avacine, 87lC174 Zirconium salts - AE; ICP; L Separate on Dowex 50W-X8 using 8611699 Organic solutions >7.5 mg 1-1 AA; F, Addition of BuOH or PrOH assists the 871262 N20 - C2H2; L Alkaloids - AA; F, Formation of Hg complexes to determine 8611393 air - C2H2; L Industrial materials 0.01 p.p.m.-0.5% AA; vapour cell; G Pyrolyse samples containing organic C and Cu, Fe, Pb and S compounds, using Florisil - CaO (1 + 1) as a pyrolysis aid; collect Hg vapours on Au (for 0.01-1.0 p.p.m.Hg) or in 0.5% KMn04 in 0.5 M H2S04 (for 1 p.p.m.-0.5% Hg), followed by cold vapour AAS Etch with 1 + 1 + 10 HF - HNO, - H20, dilute with H20, remove Cu on column of KU2 cation exchanger in H+ form, add H2S04, add Hgrr, pass through cation-exchange column and determine HgBr, in eluate using SnC12 reduction oxidise by KMnO, solution or O2 combustion and reduce Hg" to Hg with SnC12 - HCI pilocarpine; complex formed with Hg and HNO,; standard additions method used and interference effects studied standards; no interference from Al, Ca, Fe, Mg and Ti method for determination of the isotopic composition of Li by an ultimate absorbance-ratio procedure 8611743 Niobium germanide Trace levels films AA; vapour cell; G Paint 0.005-0.05% mlm AA; vapour cell; G Prepare solution as in BS 3900: Part B5; either 87/285 soluble Hg Pharmaceutical >2 mg AA;-;- Indirect method for the determination of 8713 17 Silicon - AE; F, -; L Remove matrix by treatment with HF, H2S04 8611327 formulations 871390 Molecular sieves - AA; F, Dissolve in 1 + 1 HCI; use acid matched air - liq .petroleum gas; L air - C2H2; L Lithium carbonate 0-99.3 % AA; F, Dissolve in dilute HCI and adjust to pH 1-3; 871378 and Li metal Lithium hydroxide - AA; F, -; L See Ca, ref. 871101 871101 Gallium arsenide - AA; ETA; - Matrix interferences are minimised by addition 87lC213 of orthophosphoric acid and use of platform atomisation; background absorption by GaO and GaCl are compensated for by deuterium correction See Cu, ref. 871659 871659 Characterisation of solids precipitated from 8611989 synthetic fuel reprocessing solutions in combination with EDXRF and Raman micro probe spectroscopy analyte intensities in the glow discharge plasma AE;-;- TIN plating was controlled by monitoring 8611411 AE; F,-; L See K, ref.8611327 8611327 AE; F,-; L 871277 Dry 1 g at 300 "C, fuse with Li2C03 - B203 or - H3B03 or - Li2B407, dissolve cooled melt in HCI and dilute with H20 AA; F, See K, ref. 871390 871390 air - liq. petroleum gas; L air - C,H,; L AA; F, Dry ash and dissolve in H 2 0 871576 Mn - Plastics Mo 202.03 Zirconium molybdate Trace levels - AA; ETA; S AE; ICP; L N 357.7 Deposition vapours - Na - Silicon - Na 589 Aluminium oxide 20.05% Na - Molecular sieves - Na 330.2, Na alkyl- and 8-11% 330.3 aryl-sulphonates 861 1952140R JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, AUGUST 1987, VOL. 2 Table 1.2. SUMMARY OF ANALYSES OF CHEMICALS AND MISCELLANEOUS MATERIALS-continued Technique; atomisation ; analyte form* AA; ETA; L Matrix Tungsten trioxide Concentration Trace levels Sample treatmentlcomments Reference Elemenl P P Pb Pb Pb Pb Pb Pb Pb Pd Unm 213.6 - - - 283.3 283.3 217.0 - - 244.7 8611038 87lC1008 8611406 87/83 871279 871280 871382 871454 87lc783 871333 871332 871470 871125 871332 871377 871659 87lC791 87/28 1 871353 871406 871454 Dissolve 0.4-0.7 gin 2 M NaOH, add0.5 M H3B03 and 2 M acetic acid and heat in a boiling-water bath for 15 min; cool to 20 "C, add 5 M HN03, 1 M Na2Mo04 and 0.4 M NH4V03, stand for 1 h, extract with IBMK, treat with Ni and analyse Dissolution prior to analysis See Cd, ref.8611406 See Co, ref. 87183 Niobium pentoxide Plastics Paint and varnish driers Paints Trace levels >mg kg-1 levels AE; MIP; L AA;-;- AA; -; L AA; F, air - C2H2; L 0.01-2% mlm total Pb Ash in presence of MgC03 at 475 "C; if no Sb, extract ash with HCI, filter, wash and dilute with H20; if Sb present, grind ash with Na2C03 + S (1 + l), heat till no more SOz, treat with H20, collect on filter, treat with HN03 then HCI, then filter as before; alternative method is H2S04 - H202 or - HN03 oxidation Prepare sample as in BS 3900: Part B5 Paints 0.0>5% mlm soluble Pb 10 pg-10 mg AA; F, AA; F, air - C2Hz; L air - C2H2 or N20 - C2H2 ; L Dissolve in 0.2 M HBr, pass through a short column of AG1-X4 anion-exchange resin in the bromide form to retain Pb and separate from gram amounts of Ba", CaII, CoII, CuII,FeIII, GaIII, In"', Mn", UvI and Zn"; elute Pb with 2 M HN03 See Cd, ref.871454 Analytical grade chemicals Enamelled tableware Gunshot residue swabs Solutions AA; ETA; L - Trace levels B0.14 pg ml-1 AA; -; L See Ba, ref.87/C783 AA; F, air - C2H2; L Mix with 2 mlO.1% nioxime solution, adjust to pH 3.5 with 2 ml acetate buffer, shake and leave for 5 min; add 2 ml20% naphthalene solution in acetone, shake for 30 s, filter and dissolve in 10 ml1 + 9 butylamine - dimethylformamide off silica, co-precipitate analyte with Te in 2 M HCI at 90 "C for 5 h; dissolve precipitate in aqua regia and evaporate to dryness; dissolve and make to 100 ml with 2 M HCI Decompose <2.5 mg with 10 ml aqua regia, cool, treat with 10 ml5% Ca(N03)2 solution in 10% HN03 and dilute to 25 ml with H20; suitable for catalysts based on alumina, silica gel or molecular sieve Use of high resolution ICP-AES to determine various isotopes of Pu including 242Pu and 240Pu Fuse with Na202 and dissolve in HCI; filter See Pt , ref.871332 Pt 214.423 Alumina- based 0.01-3% catalysts AE; ICP; L Pt 265.9 Platinum catalysts - AA; F, air - C2Hz; L Pu 453.61 4 Solutions ng ml- levels AE; ICP; L 0.01-0.58Yo 0.05-5 pg ml-1 AE; ICP; L Rh Ru 342.5 349.9 Alumina-based Nitrosylruthenium catalysts complex AA; F, air - C2H2; L Decompose nitrosylruthenium complex by addition of 0.5 ml30% H202, heat for 1 h in a water bath at 100 "C, add 2-3 mg Fe(N03)3 and heat for 30 min; cool and add 0.5 M CeIV solution to form ruthenium tetroxide from RuIII See Cu, ref. 871659 See Br, ref. 87lC791 Ru S Plastics Freon-type gases Paints and SF6 Trace levels >ng range AA; ETA; S AE; ICP; G Sb 217.6 0.05-5% mlm soluble Sb - AA; F, AA; Hy; G air - C,H,; L Prepare sample as in BS 3900: Part B5 Sb Plastics Dissolve in HC1 - DMF solution; evolve hydride using NaBH4 in DMF and atomise in a heated quartz cell See Al, ref.871406 AA; F, AA; ETA; L air - C2H2; L Sb Sb 217.6 PoIy(viny1 chloride) - Enamelled - tableware See Cd, ref. 871454JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, AUGUST 1987, VOL. 2 141R Table 1.2. SUMMARY OF ANALYSES OF CHEMICALS AND MISCELLANEOUS MATERIALkontinued Technique; atomisation; Matrix Concentration analyte form* Element hlnm Sb - Sample treatmentkomments Various extractiodpre-concentration procedures for determination of a range of Sb"' and SbV concentrations; Pb electrodes decomposed by oxidation with NaOCl and dissolution in HN03 - tartaric acid See Ba, ref.87lC783 Reference 871487 871C783 871407 87lC1008 861141 1 86lC1268 8611406 87lC213 871278 871326 8611699 8611989 871262 8611062 86lC1150 86lC1161 86lC1165 86lC1172 86K1173 86lC1174; 86/C 1573 86lC1198 86lC1237 86lC1256; 871C848 8611 3 14 86/14 18 Electrodes and - solutions AA;-;L - Sb Si - Gunshot residue Trace levels Antifoaming agent, 1300- swabs car polish and cosmetics 47 000 p.p.m. AA;-;L AE; ICP; L Separate organo-Si compounds by gel chromatography using Sephadex LH-60, IBMK + MeOH (10 + 3) eluent and 0.7 ml min-' flow-rate; aspirate every 5-ml portion into ICP Dissolution prior to analysis (also see P, ref. 87/C1008) See N, ref. 86/1411 Comparison with fluorimetric and See Cd, ref. 8611406 See Mg, ref. 87lC213 Prepare solution as in BS 4140: Part 13; radiochemical methods operating range is up to 0.5 mg (as ZnO) in 100 ml Selectively dissolve trace Zn in 1 ml2 M HCI by shaking for 1 min; operate atomiser at slightly higher than normal char temperature to eliminate interferences from small amount of Ga dissolved See Hf, ref.8611699 See Mo, ref. 8611989 - Si Niobium pentoxide Trace levels AE; MIP; L AE; -; - AE; ICP; L AA;-;- AA;ETA;- AA; F, air - C2H2; L AA; ETA; L Ti 364.3 U - Deposition vapours - ~ndustria~ effluents - Zn Zn Zn 213.8 - Plastics Gallium arsenide Aluminium oxide >mg kg-1 levels - - Zn Gallium 1 0 - 8-1 0- 4% - Zr Zr 343.82 Hafnium salts Zirconium molybdate Organic solutions Catalysts AE; ICP; L AE; ICP; L - Zr AA; F, N 2 0 - CZH,; L AA; F, -; L AE; ICP; L See Hf, ref. 871262 Various - (8) Treat with HF to remove Si, digest with 10% HCI and analyse for Al, Fe, Na, Ni, Sb, Sn, Ti and V; good agreement between techniques of C1, N, P and S emission using a simultaneous multi-element detector ICP at 40 MHz and ICP analysis Characterisation of pesticides by measurement Description of operating conditions for an air Automated decomposition, pre-concentration Various - (4) Pesticides AE; GC - MIP; L Various - Organic solvents AE; ICP; L AE; 1CP;- Various - Organic and inorganic materials Plant chemicals Discussion of the potential of ICP analysis in automatic process control On-line analysis employing an air ICP at 40 MHz On-line analysis employing an air ICP at 40 MHz Separate impurities using column partition chromatography with trifluorochloro- ethylene polymer coated with tri(2-ethylhexy1)phosphate or di-n-hexyl- N, N-diethylcarbamoylmethylene- phosphonate; elute with HN03 - Various - AE; ICP; L AE; ICP; L AE; ICP; L AE; ICP; L Various - Various - Industrial plant streams Brine stream Various - Uranium compounds p.p.m.levels Various - Various - (19) (12) Chinese herbal medicines Engine cleaning fluids Major and trace levels AE; ICP; L AAS used to determine Ca, Cu, Fe, K, Mg, Mn, Na, Pb, Si and V; ICP-AES used for P and S Dissolve in HN03, extract U with Ba3P04 solution and aspirate aqueous phase AA;-;- AE; 1CP;- Various - (17) Nuclear grade uranium compounds Selenium p.p.m. level AA; F, air - C2H2 or N2O - C2H2; L AA; F, -; L Dissolve in concentrated HNO,, add HC1, evaporate to dryness and dissolve residue in either S l % HNO, or HCI, or water saturated butanol; for the latter, separate the aqueous phase for analysis; SeOz remains in the butanol, but so also do Ag, Bi, Sb and Te Various - Trace levels142R JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, AUGUST 1987, VOL.2 Table 1.2. SUMMARY OF ANALYSES OF CHEMICALS AND MISCELLANEOUS MATERIALS-continued Technique; atomisation; analyte form* AE; ICP; L Sample treatmentlcomments Reference 8611 41 9 86lC1559; 87/C55 1 ; 87lC884 86lC1560 86lC1571 8611 7 13 8611716 8611746 Element Vnm Various - Matrix Concentration Pharmaceutical and Trace levels High-pressure decomposition cellulose compounds Organic solvents Various - Trace levels AE; ICP; L Direct method using standards prepared in organic solvents AF; ICP; L Addition of 50 cm3 min- 0, to the nebuliser flow reduces carbon deposits Dissolve in 3 + 1 HC1- HN03 and dilute with de-ionised H,O; use high solids nebuliser to introduce concentrated solutions elements, Cd or Zn, on analyte intensities; both buffers were equally good, giving improved detection limits for B, Be, Ga, In, Mn, Mo, P, Pt and V From 27 solvents studied, decane, pseudo- cumene, xylene, dodecane and a petroleum fraction (boiling-point range 15Ck200 "C) were recommended for Ag, Al, Cr, Cu, Fe, Ni, Pb, Si, Sn, V and Zn residue in warm 1 + 1 HCI - H20 and adjust to 20 ml for As, Cd, Cr, Cu, Fe, Mn, Ni, Pb and Zn trialkylbenzylammonium chloride in o-xylene, in the presence of ca.240 g 1-1 NaC1,l M HC1 and 120 g 1-1 SO,,-; a 5-10 fold pre-concentration is achieved Sample placed in graphite boat and analysed directly using Zeeman-effect background correction for Cr, Cu, Fe and Ni Electrodeposition from aqueous solutions on to a hanging drop Hg electrode coupled with spectrographic analysis Separate Eu, Dy, Gd and Sm from U matrix by solvent extraction with Alamine 336 in xylene or diethyl ether followed by cation exchange using Bio-Rad AG 50W-X8 observation height to aqueous solution conditions for simultaneous determination of Au, Ba, Ca, Cd, Cr, Cu, Fe, K, Li, Mn, Na, Pt and Zn Determine non-volatile impurities (Al, Cu, Fe and Mg) in an aqueous solution of decomposed trimethylgallium; measure volatile Si impurities in vapours swept from an exponential dilution flask containing same sample Fuse with Li tetraborate and dissolve melt in HNO,; use air - C2H2 for Ca, Mg, Zn and N20 - C2H2 for Al, Ba.Si and Ti; equivalent concentrations obtained by FAAS, ICP and wet chemical methods Bromide salts increased the spectral line intensities of rare earth elements when mixed with the sample; the order of the effects were LiBr.2H20 < NaBr, KBr, CsBr and MgBr2.6H20 < CaBr, < SrBr,, BaBr, conditions for simultaneous determination of Cr, Cu, Fe, Mn, Mo, Ni and Zr without matrix interferences from up to 70% VIV CH,COOH Study of the use of non-easily ionised Evaporate with Na,SO, and HNO,, dissolve Extract with an equal volume of 0.6 M No significant difference in power and Simplex optimisation used to obtain best Various - Various - Organic solvents Ga and GaAs p .p. b.-p.p.m. levels AE; ICP; L Various - (9) Graphite ng levels AE; d.c.arc; S Various - (11) Organometallic compounds ng ml- 1 levels AE; ICP; L Various - (9) Sulphuric acid mg levels AE; ICP; L 8611786 Various - (14) Nickel-plating electrolytes Trace levels AE; ICP; L 0.03-0.2% Trace levels AA; ETA; S AE; arc; S Various - (4) Polyethylene 8611 803 8612022 8711 1 Various - (13) NaCl and KCI Various - (4) Uranium compounds 0.017-0.31 p.p.m. AE; DCP; L Various - (13) Chloroform mg 1-1 levels pg g-1 levels AE; ICP; L 87124 Various - (5) Trimethylgallium AE; ICP; G or L 87/59 Various - (7) Pigments AA; F, air - C2H2 or N20 - C2H2; L AE; ICP; L AE; d.c. arc; S 87/84 Various - Carbon powder Trace levels 50 pg ml- * 87/99 Various - Acetic acid solutions AE; ICP; L 871127JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, AUGUST 1987, VOL.2 143R Table 1.2. SUMMARY OF ANALYSES OF CHEMICALS AND MISCELLANEOUS MATERIALhontinued Element Unm Matrix Concentration Various - Organic solutions - Various - (15) Various - Various - (4) Various - Various - (4) Various - (7) Various - Various - Various - (9) Lead telluride 10 - 8-10 -5 yo Nuclear industry - Diving gas mixtures YO levels materials Organic solvents Nuclear grade uranium oxide Calcium phosphate Polyacrylamide polymers Organic samples High-purity acids and organic solvents Trace levels Trace levels 1 0 - 5- 1 0 -2% Trace levels - 0.01-0.1 mgl-1 level Technique; atomisation; analyte form* MS; ICP; L AE; d.c. arc; S MS; 1CP;- AE; MIP; G AE; ICP; L AE; ICP; L AE; d.c. arc; S AA; F, -; L AE; F, -; L AA; F, -; L AA; ETA; L AE; ICP; L Sample treatmentlcomments Reference Addition of a small amount of O2 to the nebuliser gas was effective in removing carbon particulate from the sampling cone; detection limits for a variety of elements were similar to those for aqueous solutions Dissolve, remove most of Pb and Te matrix by precipitation, then mix with graphite powder and NaCl Comparison with spectroscopic techniques He-based gases analysed using 314-wave cavity at 15 torr for measurement of Ar, He, 0 and N CH30H and (CH&CO analysed Method developed for extraction of U from solutions followed by simultaneous determination of Dy, Eu, Gd and Sm carrier for determination of As, Ba, Cu, Mg, Ni, Pb and Zn Acidic decomposition in presence of NaOCl as an oxidative matrix modifying agent to minimise polymer matrix effects caused by partially hydrolysed polyacrylamides Either dissolve sample with a suitable organic solvent and use discrete sampling by micro-injection, or form an organic - aqueous emulsion and continuously nebulise; ethoxylated nonyl-phenols are recommended as emulsifying agents (10 g dm-3) Direct analysis using platform atomisation for ETA-AAS; evaporate 40 ml to 2 ml prior to analysis by ICP-AES; both methods give comparable results for Ag, Au, Co, Cu, Fe, K, Li, Na and Ni Mix with graphite powder and a spectroscopic 87lC188 871269 871321 871612 871614 871692 871C1027 87lC1081 87lC 1086 87lClO9 1 * Hy indicates hydride generation and S, L and G signify solid, liquid or gaseous sample introduction, respectively.Other abbreviations are listed elsewhere.citric acid, sulphates and alkali and alkaline earth chlorides and sulphates. The Cd and Cu were adsorbed on to a layer of ZnS which was subsequently dissolved in hot HN03 - HCl - H20 (1 + 1 + 2) for analysis by AAS. The recoveries of Cd and Cu were 73-120 and 9&102%, respectively. The determi- nation of Pt and Rh in alumina-based catalysts by ICP-AES (87/332) was performed by co-precipitation of the analytes with Te after fusion of the sample with Na20z and dissolution in HCl. The precipitate was redissolved and aspirated directly into the ICP. It was claimed that the recovery of the co-precipitation process was 98.5-100%. No interferences from commonly co-existing metals were reported. Controlled- potential electrolysis at a hanging mercury drop electrode was used to concentrate and separate trace amounts of reducible metals from concentrated salt solutions (86/2022).The reagent-free procedure allowed the simultaneous multi-ele- ment analysis of NaCl, KC1, rock salt and natural brine solutions without matrix interference from the major constitu- ents. In yet another approach to improve analytical sensitiv- ity, Ce4+ was added to sample solutions to convert Ru3+ quantitatively into volatile Ru04 (87/377). This resulted in a 60-fold improvement in the sensitivity for the determination of Ru by FAAS. Preliminary decomposition of Ru complexes could be achieved by treatment with H202. Not all the procedures reported for the analysis of catalysts required the pre-concen tration of analyte elements.Direct acid digestion was proposed for the FAAS analysis of platinum catalysts (87/470) and the determination of Cr in catalysts used to convert ethylbenzene into styrene (87/608), The determination of Al, Fe, Na, Sb, Sn, Ti and V in fresh and regenerated fluid catalytic cracking catalysts by ICP-AES and FAAS was also achieved following conventional acid diges- tion (86/1062). 1.2.3. Microelectronic components As expected, ICP-AES and ETA-AAS continue to be the most important techniques for the determination of trace elements in microelectronic components. In comparison with last year, however, relatively few new developments were reported and most of the papers concerned the analysis of gallium and gallium arsenide. In the preparation of semicon- ductor materials by chemical vapour deposition, metal alkyls of Groups 11, I11 and IV are reacted with hydrides or alkyls of Groups V and VI.The purity of the highly reactive organome- tallic compounds is of critical importance as trace levels of impurity elements may completely alter the properties of the semiconductors produced. Two procedures were reported (87159) for the analysis of trimethylgallium (TMG) by ICP-AES. As TMG is pyrophoric and volatile and the nature of the impurities was not known, separate methods were devised for the determination of non-volatile and volatile components. The non-volatile impurities (Al, Cu, Fe and Mg) were measured by conventional ICP-AES after decomposi- tion of TMG in aqueous solution. The volatile silicon containing impurity was determined by placing a known144R JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, AUGUST 1987, VOL.2 amount of TMG in an exponential dilution flask and the vapour was flushed from the flask into the ICP by an Ar gas stream. The detection limits for the above elements were in the range 0.08-2 pg g-1. The concentrations of several impurity elements in gallium and gallium arsenide were measured by ICP-AES through use of a high-solids nebuliser or a V-groove Babington-type nebuliser which allowed the aspiration of solutions containing up to 10% dissolved solids (86/C1571). It was suggested that the speed of ICP-AES analysis allowed impurity levels and dopant concentrations to be monitored throughout the fabrication of a device, from raw materials through to the final product.A variety of procedures were devised to minimise matrix interferences and other sources of error in the determination of trace elements in semiconductor materials by electrothermal atomisation atomic absorption spectrometry. The use of platform atomisation and orthophosphoric acid as a matrix modifier allowed the determination of Mg and Zn in gallium arsenide by ETA-AAS (87/C213) without the need for pre-concentration. The authors reported that molecular absorption by GaCl and GaO could be adequately compen- sated for by use of deuterium-arc background correction. Trace concentrations of Zn in high-purity gallium were measured by ETA-AAS (87/326) following selective dissolu- tion of the analyte in 1 ml of 2 M HC1. A higher than normal char temperature was used to eliminate the interference of the small amount of gallium dissolved with the analyte.A procedure for the direct determination of Cr in gallium arsenide was proposed (8611650) which involved the analysis of semiconductor fragments placed inside a graphite furnace atomiser. The temperature programme was designed to remove the arsenic during the char stage and release the Cr from the gallium matrix during atomisation at 2850 "C. Effective background correction was achieved by the Smith - Hieftje method and aqueous synthetic standard solutions could be used for calibration. Matrix interferences were avoided in a d.c. arc AES procedure for the determination of trace impurities in lead telluride (87/269) through removal of the lead and tellurium by precipitation of the nitrate and oxide salts, respectively. Trace amounts of P and Si in electronics grade niobium pentoxide were determined successfully by microwave induced plasma atomic emission spectrometry after dissolution of the sample (87/ClOO8).Unfortunately, no details of the spectral wavelengths and detection limits were given. 1.2.4. Gases, acids and solvents A gas sampling valve and a low dead-volume interface were constructed (87/C791) for the direct injection of SF6, Freon 13B1 and Freon 12 into the axial channel of an ICP. The detection of Br, C1 and S atomic emission at VUV wavelengths was achieved by inserting an optical sampling orifice directly into a horizontal ICP so that the plasma flowed around the tip of the water-cooled copper cone that supported the circular orifice (see Houk, R.S., Fassel, V. A., and La Freniere, B. R., Appl. Spectrosc., 1986,40,94). The sampling cone was mounted on the optical axis of a vacuum monochro- mator and no lenses or optical windows were used to collect the analyte radiation. The entire optical path was purged by a He gas stream that flowed out of the sampling orifice into the ICP. Further information was provided (87/612) on a previ- ously reported method for the analysis of diving gas mixtures by microwave induced plasma atomic emission spectrometry (see JAAS, 1986,1,97R). Superior performance was achieved in the determination of Ar, N and 0 when the He MIP was operated at 15 torr in a 3/4-wave cavity rather than at atmospheric pressure with a Beenakker cavity. Analyte atomic emission lines in the region 700-900 nm were detected with good sensitivity by a small silicon diode.An interesting procedure was reported that allowed the oil consumption in a diesel engine to be measured by monitoring the composition of the exhaust gases (86/1064). Chlorinated paraffin was added to the oil and the C1 component of the exhaust gas was scavenged with Ag+ to obtain silver chloride which was collected and analysed by ICP-AES. Few reports on the analysis of acids were received during the period under review. Matrix evaporation procedures were used (86/1746, 87/C1091) to improve the ICP-AES detection of trace element contaminants in high-purity acids. A 40-ml sample of acid or organic solvent was reduced to a volume of 2 ml by sub-boiling distillation prior to simultaneous determina- tion of Ag, Au, Co, Cu, Fe, K, Li, Na and Ni by ICP-AES (87/C1091).The concentrations obtained were in good agree- ment with ETA-AAS results. In the determination of As, Cd, Cr, Cu, Fe, Mn, Ni, Pb and Zn by ICP-AES, a sample of sulphuric acid was evaporated with Na2S04 and HN03 and the residue was dissolved in warm 50% V/V HC1 for analysis (86/1746). A modified Simplex method of optimisation was applied successfully to remove matrix interferences in the determination of Cr, Cu, Fe, Mn, Mo, Ni and Zr in acetic acid by ICP-AES (87/127). The optimum conditions for applied power and the three gas flows were achieved within 25 experiments. The main developments in the analysis of organic solvents concerned the operation of ICPs with either AES, AFS or MS.The use of air or other molecular gases as a partial or total substitute for the three main gas flows of an Ar ICP has been considered by various groups in recent years. The formation of a total molecular gas inductively coupled plasma requires the application of 2 4 kW applied power and the start-up procedure normally involves the gradual transition from a pure Ar plasma to a pure molecular gas plasma. A recent investigation (86/C1161) has shown that a pure air ICP can be sustained when a simple one-step gas flow conversion pro- cedure is applied after initiation of an Ar plasma. Computer calculations indicated that molecular gas ICPs should be more efficient at sample decomposition than a pure Ar ICP (see also Kovacic, N., Meyer, G.A., Ke-Ling, L., and Barnes, R. M., Spectrochim. Acta, Part B, 1985, 40, 943) and this was evaluated for the determination of trace metals in organic solvents. The preliminary results indicated that injection of organic aerosols into the air ICP does not yield the same visible zones as observed when using a pure Ar plasma. Unfortunately, no details of the detection limits obtained for the analysis of organic solvents with an air ICP were available for inclusion in this review (see also section 1.2.6). A detailed study was undertaken (87124) to investigate and control the solvent load of an Ar ICP when aspirating chloroform solutions. The chloroform plasma load was regulated by the use of a condenser, the temperature of which was varied in the range -50 to +20 "C.Analyte and background intensities were obtained for various chloroform loads and two sets of experimental conditions were selected for simultaneous multi- element analysis of chloroform solvent solutions, one with and one without aerosol cooling. When aerosol cooling was applied, the detection limits for elements in chloroform were similar to those obtained when aspirating aqueous solutions. Without aerosol cooling, the detection limits were up to an order of magnitude poorer. An attempt was made to characterise organic solvents on the basis of both volatility and their behaviour in ICP systems. The authors suggested that the volatility effects of organic solvents depended on the evapora- tion rate, which influences the rate at which the analyte is delivered to the plasma, and saturation vapour pressure effects, which influence the excitation conditions through the solvent load of the plasma.The chemical and physical problems encountered when analysing organic solvents by ICP-AES were also considered in a series of presentations given by researchers from Allied Analytical Systems (86/C1559, 87/C551, 87/614, 87/C884), and in a discussion of the analysis of engine cleaning solvents (86/C1256, 87/C848). Vapour-loading effects were also considered in the opti-JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, AUGUST 1987, VOL. 2 145R misation of inductively coupled plasma atomic fluorescence spectrometry for the determination of metals in organic solvents (86/C1560). Solvents with a volatility similar to that of water required no change from normal operating conditions and no deterioration in plasma stability was encountered. The well established procedure of adding a small percentage of O2 to the nebuliser carrier gas flow assisted in the complete combustion of carbon compounds in the plasma, and analy- tical figures of merit were achieved similar to those obtained for aqueous solutions.When selecting solvents for the dissolution of organic materials, kerosene was recommended for most non-polar compounds whereas DMF was found to be suitable for most polar materials. The addition of a small amount of 02, mixed with the nebuliser gas, was also shown to be effective (87/C188) in eliminating the build up of carbon particles on the cone of the sampler orifice in the analysis of organic solutions by inductively coupled plasma mass spec- trometry.Background spectra and detection limits obtained when analysing organic solvents were similar to those ob- served under aqueous conditions. 1.2.5. Nuclear fuels and related materials Further developments were reported on the separation and determination of impurity levels in nuclear fuels. To avoid the spectral interference by uranium lines, a method was developed that allowed the quantitative separation of about 40 impurities from uranium prior to ICP-AES analysis (86/ C1198). Column partition chromatography was used with neutral organophosphorous compounds as extractants. The columns were prepared from tri (2-ethyl hex yl) phosphate or di-n-hexyl-hr,N-diethylcarbamoylmethylenephosphonate coated trifluorochloroethylene polymer.Uranium was ad- sorbed by the organic phase and the impurities were eluted by HN03. After evaporation and volume adjustment, the trace metals were determined by ICP-AES. Excellent recoveries were claimed for this procedure. An extraction procedure was used (87/11) prior to the determination of Dy, Eu, Gd and Sm in uranium(1V) and urariium(V1) oxides by DCP-AES. Uranium and some anionic species were extracted with o-xylene - petroleum ether (b.pt. 8&100 "C) - Alamine 336 (50 + 100 + 65); the aqueous phase was then passed through a Bio-Rad AG50W-X8 cation-exchange column to remove residual levels of uranium. When the last traces of uranium had been flushed from the column, the lanthanide elements were eluted and determined by DCP-AES.A similar proced- ure was also reported for the removal of uranium prior to the determination of Dy, Eu, Gd and Sm by ICP-AES (87/692). A method for the ion-exchange chromatographic separation of Hf and Zr was reported (86/1699) that employed 8-hydroxy- quinoline-5-sulphonic acid as a chelating agent. Separation was based on the difference in the stability of the sulphoxinate and sulphate complexes of the metals. By using 2 M H2SO4 as the eluent, only Zr was eluted while Hf was retained on the ion exchanger (Dowex 50W-X8) which could be eluted with more concentrated H2S04 or oxalic acid. Analysis of eluate solutions by ICP-AES indicated that it was possible to obtain reactor-pure Zr in a single separation step and remove nearly all Zr impurities from Hf salts.The removal of Zr from acidic solutions by precipitation with Mo was described (8611989) and it was suggested that the application of this procedure in the nuclear fuel cycle could be extended to include other fission products, such as Pu and U. A variety of techniques including ICP-AES, XRFS and Raman microprobe spectros- copy were recommended for characterisation of the precipi- tates. The determination of 17 impurity elements in nuclear quality uranium compounds by flame atomic absorption spectrometry was achieved (86/1314) by extracting the uran- ium with tributyl phosphate solution. The aqueous phase was then aspirated directly into either an air - C2H2 or an N20 - C2H2 flame. The authors reported recoveries of between 90% (for K) and 100% (for Cr).Other analytical studies in the area of nuclear fuels included the application of high resolution ICP-AES for the character- isation of the 242Pu spectrum in the 200-700 nm region (87/125), the addition of ascorbic acid to improve the ETA-AAS sensitivity for the determination of B (87/476), the development of an ultimate absorbance ratio technique for the AAS determination of the isotopic composition of Li (87/378) and an evaluation of ICP-MS for the determination of impurities in Zircaloy and other materials (871321). 1.2.6. On-line process control The application of atomic spectrometry to the continuous monitoring of industrial processes has proved more difficult than the use of electroanalytical and chromatographic pro- cedures. However, the use of an air ICP (see section 1.2.4) for on-line process analysis was discussed in conference presenta- tions by representatives of the Dow Chemical Company (861C1173) and the Baird Corporation (86/C1174,86/C1573).The plasma, operated at 40 MHz, was designed for 24-h operation in a production environment without operator control. It was suggested that by identifying the individual requirements of a particular analysis, a certain amount of miniaturisation and rearrangement of the instrument com- ponents was possible. No specific information was provided regarding industrial applications of the air ICP system, but the determination of three elements in a brine stream was mentioned in one of the abstracts (86/C1174). Atomic emission spectroscopy was used to monitor the conditions of a vapour deposition process used in triode ion plating (86/1411).In the deposition of TIN, the intensities of the N and Ti emissions were measured at 357.7 and 364.3 nm, respectively. Variations in the relative emission intensities of N and Ti were indicative of changes in the vapour composition that would alter the stoicheiometry of the film deposited. The AES measurements were attractive as they provided a method of controlling the deposition process without disturbing the glow discharge plasma itself. Other topics of relevance to on-line process control included the application of chemometrics and plasma spec- trometry in process analytical chemistry (86/C1172) and the use of automated sample preparation in conjunction with ICP-AES (861C1158, 86/C1165).2. IRON AND STEEL The total number of papers on iron and steel analysis received during the review period was 47 (Table 2). No significant new developments were reported and many of the papers de- scribed modifications of well established principles to solve some of the analytical problems encountered in the modern iron and steel industry. This was particularly true for the trace element analysis of high-technology steels (clean steels) where ultra-low levels of Some elements have a significant influence on the properties of the material. Many of the papers, however, reported only routine applications of atomic spec- trometry. 2. 1. Atomic Emission Methods The application of plasma atomic emission spectrometry techniques accounted for almost half of the papers reviewed with the ICP outnumbering the DCP as an excitation source in the ratio of 5 : 1.Two papers on the determination of P were146R JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, AUGUST 1987, VOL. 2 Table 2. SUMMARY OF ANALYSES OF IRON AND STEELS Element As As As B B Bi Ca Cd Cr Cr Cr c u c u Fe Hf Mn Mn Mn P P P Pb Sb Sb Se Se Si Si Si Ta Ti Unm - 193.76 - 249.68 249.77 223.06 422.7 229.5 - - - - 324.7 - 286.64, 307.29 403.45 403.45 - Matrix Iron and steel Steel Steel, Cu alloys Steel Steel Steel Steel Steel Iron and steel Steel Steel Steel and Cu ores Steel Coated steels Steel Steel Steel Steel 281.6 (Mo) Steel Concentration Trace levels O.O1-O.O9% O.OO3-O.05 Yo 10-100 pg g- 0.7-13 pg g-l 4-24 pg g-1 2-25 pg g-l 0.35-8 pg ml-l s17% &30°/o - - 0-0.670 - 10-50 pg g-1 - - - Trace levels 214.91, Steel and Cu alloys Trace levels 253.56 - Steel Trace levels 217.0 Steel 0.5-10 pg ml-1 206.83 Steel O.OO2-O.O34% - Steel 0.01 44.096% - Steel and Cu alloys 0.003-0.05% - - Steel - Iron and steel 0.2-1 .O% 251.6 Ferrosilicon - - Steel - 240.07 Steel and - 323.45, Steel - ferroniobium 323.66 Technique ; atomisation; analyte form* AA; ICP, Hy; L AE; ICP, Hy; L AE; ICP, Hy; L AE; ICP; L AE; ICP; L AE; ICP, Hy; L AA; ETA; L AE; ETA; L AA; F, air - C2H2; L AA; F, air - C2H2; L AA; F, -; L AE; laser; S AE; DCP; S AE; DCP; S AE; GDL; S AE; d.c.arc; S AE; arc; S AE; arc; S AE; laser; S AE; ICP; L AE; DCP; L AE; ICP; L AA; F, air - C2H2; L AE; ICP, Hy; L AE; ICP, Hy; L AA;F,-;L AE; ICP, Hy; L AE; ICP; G AA; F, N2O - C2H2; L AE; laser; S AE; ICP; L AE; ICP; L Sample treatmentlcomments Reference Hydride generation following dissolution in Analysis by ICP following hydride generation Analysis by ICP following hydride generation Soluble and insoluble B determined after Samples dissolved in H2S04 - HN03 - HC104 mixture from a HN03 - HCI steel solution separation of iron with Et,O H3P04 - HN03 acid mixture; methanol added and methyl borate distilled into 4% NaOH solution See As, ref.8611635 Both AA and AE applied using standard and pyrolytically coated graphite tubes as atomisers Analysis followed the separation of the element by precipitation as xanthate, adsorption on to naphthalene and dissolution in DMF A mixture of NH4C104 and ZnC1, used as interference suppressor for Cr"1 Flow injection system developed for sample introduction Photodiode array used to resolve radiation from a laser generated high temperature plasma (LIBS) Application of DCP following generation of aerosol from solid by laser ablation; see also Cu, ref.8611841 See Cu, ref. 8611464 Application of GDL to elemental depth profiling in coated steels Hf separated by passing test solution through column packed with 0.3 g of silica gel grafted with 0.2 mmol g-1 sulphophenyl groups; after drying, residue mixed 1 + 1 with graphite Study of conditions to produce stable intensity output using flat and dimpled samples and a pointed tungsten counter electrode Study of conditions to produce stable intensity output using a tungsten pin electrode; see also Mn, ref. 8611391 See Cr , ref.871480 Determination of P indirectly by its combination with Mo as a complex heteropolyacid and measuring Mo line intensities Study of interference effects and application to four standard steels and three standard Cu alloys Extraction of P associated with molybdic acid using IBMK and determination indirectly from Mo; see also P, ref. 86lC1252 See Cd, ref. 8611646 See As, ref. 8611635 See As, ref. 87lC991 Conditions optimised to minimise Fe See As, ref. 87lC991 Application of ICP to analysis of aerosol Fusion with Na2C03 - Na2B407 and interference produced from liquid metal by Ar bubbling Na2C03 - Na202 followed by dissolution in dilute HCI with or without HBF4 See Cr , ref. 871480 Study of interference by other elements and comparison of different line performance Interference by Mn and Ni investigated 8611453 8611635 87lC991 8611 36 1 871291 8611635 861 162 1 8611646 8611703 871438 871480 8611464, 8611841 8611841, 8611464 86lC1496 8611376 8611391 871129, 8611391 871480 86lC1252 8611923 871610, 86lC1252 8611646 8611635 87lC991 871690 87lC991 86lC 149 1 871102 871480 8611933 8611884JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, AUGUST 1987, VOL.2 147R Table 2. SUMMARY OF ANALYSES OF IRON AND STEELS--continued Technique; atomisation; Concentration analyte form* 0.01-4Yo AA; F, 0,-sheathed air - C2H2; L Element Unm V - Matrix Steel Sample treatmentlcomments Effect of various acidic media (HN03, HCl, HC104, H2S04 and H3P04) examined and 8-hydroxyquinoline and TiC13 employed as interference suppressor and sensitiser See Fe, ref.861C1496 See Hf, ref. 8611376 Optimisation of operating conditions presented to achieve maximum sensitivity and precision aerosol by laser ablation ionisation by ICP technique using normalisation of results to 100% using Fe as the internal standard to simplify ICP analysis of steels Description of closed PTFE digestion vessel using microwave oven to dissolve steel samples in 80 s with HN03 - HCl - HF acid mixture Acid dissolution in HCl after fusion in Na2C03 - K2S2O7 (3 + 1) (Al, Ca, Cr, Fe, Mg, Mn, Ni and Si) Investigation of different fluxes to expedite dissolution of samples using automatic solution preparation equipment (PLASMASOL) Analysis following the production of an Analysis by MS following laser ablation and Development of single calibration curve Application of an internal standard method Reference 8716 861C1496 8611376 8611444 8611452 86lC1480 861C1504 8611698 8611781 8611789 87/42 Zn - Zr 327.31 Various - Coated steels Steel Steel, Cu and A1 alloys Steel Steel Steel - AE; GDL; S 3-15 pg g-1 Major and AA; F, AE; d.c.arc; S intermediate air - C2H2 or - AE; ICP; G levels NzO - GH, ; L Various - Various - - MS; ICP; S Various - (22) Major levels AE; GDL; S Various - S tee1 - AE; ICP; L Various - (12) Steel - AE; DCP; L Steel-making slags - AA; F, -; L AE;F,-;L Various - (8) Various - Steel products - AE; ICP; L AA;-;L Various - (6) Steels and A1 alloys Major, minor and AE; ICP; L Application of generalised internal reference procedure using major matrix elements to 87143 trace levels improve analytical performance by ICP (Cr , Cu , Mn , Mo , Ni and V) - MS; ICP; S Analysis by MS following intermittent arc vaporisation and ionisation by ICP Major levels AE; ICP; L Development of procedures to dissolve nine types of ferroalloys and select optimum lines (B, Cr, Mn, Mo, Nb, Si, Ti, V and W) Application of MS using the GDL as an ion source Trace levels MS; GDL; S Various - Solids Ferroalloys 87/60 87169 87lC189 87/426 87/604 871606 871680 871681 871C878 871925 871C1007 Various - (9) Various - Steels and high-purity metals Steel Various - ( 5 ) Trace and major AE; spark; S levels AE; arc; S Application of multi-system emission spectrometer using light guides and spark and arc excitation to cover wide concentration ranges (B, Ca, Cr, Te and Ti) Determination of trace levels of rare earth elements in steel following addition of 13% C and 1.3% NaF (La, Nd, Y and Pr) Nine CRMs analysed using spectrometric techniques; results of round-robin tests by 16 different laboratories Dissolution of samples in HN03 or a mixture of HN03 - HCl following mineral acid interference studies (Bi, Cd, Pb, Sb, Sn and Zn) of steels and complex intermetallic compounds Methodology developed to produce a gp,neral scheme for application to a broad range of steels Review with five references on AES analysis of metals Description of data handling system for AES spectrometer including background correction, calibration and transmission of results Dissolution procedures developed for a variety Various - (4) Steel Trace levels AE; d.c.arc; S Various - Steel Various - (6) Steel Trace levels AA; ETA; L Various - Steels and white metal - AE; ICP; L Various - Steel Trace levels AE; ICP; L Various - Various - Metals - - AE; spark; S - AE; spark or ICP; S * Hy indicates hydride generation and S, L and G signify solid, liquid or gaseous sample introduction, respectively.Other abbreviations are listed elsewhere.148R JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, AUGUST 1987, VOL. 2 typical examples of the problems encountered in the trace element analysis of high-quality steel. Ever since the inception of the ICP, papers on P line selection have been numerous. During the past year, two papers (86/C1252,87/610) suggested that no line was really satisfactory to determine P at the levels present in clean steels (<lo pg g-1).Both methods used the same novel procedure to overcome the problem, which involved chemical combination of P with Mo to form a complex molybdic acid. Following extraction into IBMK, the concentration of P was determined indirectly by ICP-AES through measurement of Mo atomic emission. The organic solution could be analysed directly or as an aqueous ammonia extract. Wittman (86/C1252) reported an RSD of 17% at the 0.001% m/m P level using the Mo wavelength at 286.1 nm and claimed that the method gave an order of magnitude better sensitivity than the direct determination of P. Analysis of the organic solution rather than an aqueous solution gave further improvements in sensitivity, which was also confirmed by Ichioka et al. (87/610) who reported a 2-3 fold improvement in the P detection limit when the organic solution was aspirated into the ICP.In contrast, other workers (86/1923) reported the determination of P in steel using DCP-AES and the 214.9-nm P wavelength, but the concentration levels were higher than for the ICP-AES methods. The spectrophotometric determi- nation of B in steel also presents problems and improved methods using ICP-AES have regularly been suggested. Typical of these covered by the present review period were by Spanish and Japanese workers. In the first (86/1361) Fe was removed by extraction with Et20 and both soluble and insoluble B were determined using the 249.68-11111 wavelength. Acceptable accuracy was reported for concentrations in the range 10-100 pg g-1 B. Hosoya et al. (87/291) proposed a method that involved rapid distillation and evaporation with methanol following dissolution of the steel sample in acid. A detection limit of <0.1 pg 8-1 B was claimed, although a determination limit of 1 pg g-1 B is more realistic because of relatively high reagent blank concentrations.Iron and steels containing 0.7-13 pg g-1 B were successfully analysed by this procedure using the 249.77-nm B wavelength. A method was reported for the determination of As, Bi and Sb in steel by ICP-AES following hydride generation (86/ 1635). Detection limits of 0.3,1 and 1 pg g-1 were reported for As, Bi and Sb, respectively. Two papers described the benefits of using the main matrix element (e.g., iron) as an internal standard in the ICP-AES analysis of steel. Ohls and Loepp (86/1698) measured intensity ratios simultaneously and after background correction, the analytical data were calculated iteratively. The method therefore required only two working steps, sample dissolution and nebulisation.Israeli workers (87/43) employed the generalised internal reference method to improve precision and accuracy in steel and aluminium alloy analysis. Two-point calibration was employed for steel using a blank and a standard solution, equivalent to the composition of BCS-SS410, and an RSD of better than 0.3% was achieved for elements in low-alloy steels. The direct analysis of solid samples remained the province of arc and spark AES and XRFS for over 25 years, but this situation has changed substantially over the past five years, mainly due to the combination of various methods of vaporisation (arc, spark, laser, etc.) with a variety of excitatioddetection systems (e.g., ICP, DCP and MS).The application of a number of combined systems was reported during the period under review. Work by Cremers et al. has been reported previously (JAAS, 1986,1,10lR) and a further paper (86/1452) gave details of the calibration graphs, accuracy and precision obtained for the determination of several elements in steel by laser ablation of solid samples. A Nd : YAG laser was used to vaporise the sample and the metal aerosol was flushed by a gas stream into an ICP for AES analysis. Other work by Cremers and Romero (87/480) reported a combination of laser ablation and spectral resolu- tion of the plasma radiation by a photodiode array (LIBS).Effects due to changes in laser pulse energy and the optical system were minimised by ratioing absolute elemental intens- ities to those of adjacent iron lines. Calibration graphs for Cr, Mn and Si in steel were presented together with accuracy and precision data. Mitchell and co-workers (86l1464, 86/1841) reported a combination of laser ablation and DCP-AES to determine Cu in steel. A linear calibration graph up to 0.6% mlm Cu was reported with a detection limit of 100 pg g-1. An alternative detection system in the form of mass spec- trometry was introduced in two papers. Arrowsmith et al. (86/C1480) reported the analysis of a variety of samples, including NBS steels, by laser ablation - ICP-MS. They reported detection limits of 0.1-1 pg g-1 for most elements in preliminary results.Jiang and Houk (87160) employed an intermittent arc - ICP-MS combination. Detection limits in the pg g-1 range were claimed with linear calibration graphs up to approximately 0.1% mlm. Finally, a paper on glow discharge mass spectrometry illustrated the application of a GDL as an ion source (87/C189). Results were reported for the analysis of steels and the determination of trace impurities in high-purity metals and high-temperature alloys. A dynamic range of ten decades was claimed and most detection limits were at the ng g-1 level. In last year’s Update, six papers were referred to that described the direct analysis of molten metal, but only one paper on this topic has been identified in the present review. Ono et al.(86/C1491) used a spark chamber to generate ultrafine particles (UFP) of iron which were swept into an ICP torch for analysis. A total of 15 elements (including C, P and S) were determined simultaneously and the analytical figures of merit achieved were equivalent to conventional spark AES. For example, an RSD of 0.7% was obtained at 0.21% m/m Si with a determination limit (not defined) of 0.003% mlm Si. Difficulties were encountered with the spark discharge when the procedure was applied to the analysis of molten iron. The problem was thought to be caused by carbon on the surface of the molten metal and Ar bubbling was successfully applied as an alternative method of producing UFP. A prototype unit tested on a production site gave good correlation between Fe to Si intensity ratios and the concentrations of Si in the range 0.34.8% mlrn.The analytical cycle time was 80 s for simultaneous multi-element analysis and the measuring device could be located up to 40 m from the sampling point. It was claimed that fluctuations in the surface level of the molten steel (sic) did not cause problems during the analysis, which was an advantage of the proposed method. 2.2. Atomic Absorption Methods All the papers reviewed described development work based on relatively well established FAAS and ETA-AAS prin- ciples. Again, the development of methods for the analysis of high-technology steels was of particular interest. Vanloo et al. (86/1453) employed flame atomic absorption spectrometry following hydride generation to determine As in steel and cast iron.A detection limit of 1 pg g-1 was reported with an RSD better than 4% for concentrations exceeding 10 pg g-1. These results are comparable to those obtained using Hy - ICP-AES procedures referred to previously (see section 2.1, 86l1635). Two papers reported the determination of other trace elements in steel. Following a separation step, FAAS was used to determine Cd and Pb in steels. The elements were precipitated as xanthates, which were adsorbed on to naphtha- lane and dissolved in DMF. Concentrations in the range 0.35-8 and 0.5-10 pg ml-1 were determined for Cd and Pb, respectively. Other workers (87/680) employed electrothermal atomisation atomic absorption spectrometry to determine Bi , Cd, Pb, Sb, Sn and Zn in alloy steels. Matrix interferences caused by the alloy elements and mineral acids were studied prior to the development of an HN03 or HN03 + HCIJOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, AUGUST 1987, VOL.2 149R dissolution procedure that allowed the determination of trace elements down to 0.1-1 pg g-1. The determination of trace amounts of Ca in steel was also investigated using ETA-AAS and electrothermal atomisation atomic emission spectrometry (8611621). This element is added in small amounts to modify sulphide inclusions in high performance pipeline steels. Reproducibility was slightly poorer with ETA-AES, but concentrations in the range 2-20 pg g-1 were successfully determined and, with detection limits better than 9 ng ml-1 in solution for both techniques, detection limits in the steel were in the region of 1 pg g-1.Other FAAS papers reported the determination of V in steel for between 0.01 and 4% mlm (87l6) and Se in steel down to 0.01% mlm with RSD values of 5.12 and 1.03% at 0.014 and 0.096% rnlm Se, respectively (87/690). In the former method, an 02-sheathed air - C2H2 flame was employed with 8-hydroxyquinoline as the interference suppressor and TiC13 as the sensitiser. The determination of major elements by FAAS was the subject of two papers. Chromium was measured in steel over the range 5-1770 rnlm, using NH4C104 and ZnClz as interference suppressors (86l1703). The concen- tration of Si in ferrosilicon was determined (87l102) following fusion of the sample in Na2C03 - Na2B407 or Na2C03 - Naz02 with subsequent dissolution in dilute HCl with or without the presence of HBF4.3. NON-FERROUS METALS The drop noted in the 1985 review of the numbers of papers on iron and steel analysis (JAAS, 1986, 1, 98R) has been mirrored by a similar trend in the non-ferrous field, the number of table entries for the review years 1982-1986 being 153,185,165,115 and 85, respectively. The previous review of the non-ferrous field drew attention to the increasing prom- inence of procedures involving dissolution of samples. This pattern is repeated in the current review where many of the papers essentially described chemical topics such as matrix removal and pre-concentration of analytes. The review period has revealed very few papers dealing with simple arc and spark sources, but there have been a number of publications relating to newer sources such as glow discharge lamps, atomic fluorescence and special sampling techniques (Table 3).3.1. Atomic Emission Methods 3.1.1. Arc methods Reported applications of arc atomic emission spectrometry came mainly from Russian and Chinese workers, as had been noted in the previous review year. Portnaya and Rychkova (86/1043) used a 12 A a.c. arc to determine Ru in tungsten metal in the range 0.03-2% mlm, where the sample in the form of the oxide was mixed with a flux - buffer of graphite containing gallium oxide or lead oxide. The flux - buffer procedure, using a graphite - sodium chloride mixture, was also employed by Chanysheva and Yudelevich (87l936) to determine trace elements in high-purity tin following removal of the matrix as tin bromide.Thirty-four elements were determined down to levels of 10-5-2 x 10-8% mlm. Wang and Zhou (86l2021) used a form of the carrier distillation method to determine impurities in magnesium - yttrium alloy at levels between 0.05 and 1.6% mlm. They used a graphite powder containing 0.2% mlm Co304 as an internal standard and 6% mlm AgCl as the carrier. Sodium was determined in aluminium (86/1044) using a 2 A a.c. arc established between the sample and a graphite counter electrode. Measurements down to 0.0005% mlm were reported. An unusual application was described by Suranov et al. (86l1701) who used an arc source and a photodiode array detection system for qualitative and semi-quantitative analysis of nickel-based alloys and high-purity magnesium. A combined recording and data processing time of <5 min was reported.3.1.2. Spark methods The direct use of spark atomic emission spectrometry was reported by only group, in two papers by Millard and co-workers (87l35, 87l481). A detection limit of 2 p.p.m. for Be in beryllium - copper alloys was obtained using a laser to induce breakdown in the spark gap. It was suggested that the procedure could be used for alloy sorting “where only discrimination between discrete concentrations is required.” 3.1.3. Plasma methods Major interest in this field remains with ICP-AES applica- tions, DCP-AES and MIP-AES procedures being in the minority. Inductively coupled plasma atomic emission spectrometry methods which involved dissolution, ion-exchange and extrac- tion processes suffer from limitations in the speed of sample turn-round. It is not surprising therefore that faster, direct insertion techniques which allow solid samples to be intro- duced to plasmas continue to attract attention. Clark et al.(86l1651) used an ETA technique to vaporise specimens of nickel-based alloys into an ICP for the determination of As, Cd, Mg, Pb, Se and Zn at p.p.m. levels. This group also described (87l41) the use of a special probe for insertion of weighed metal chips into an ICP in a similar application, which gave detection limits down to p.p.b. levels. An ICP sampling system that consisted of a heated graphite crucible positioned immediately below the inlet tube of a modified Meinhard nebuliser was described by Ohls et al. (87l231). The system permitted controlled heating of the sample to allow selective vaporisation of metals and it was possible to determine Bi, Pb, Te and Zn at p.p.b. levels in reference materials.Spark erosion of a solid metal sample was employed by Prell and Koirtyohann (87/C815) to produce a vapour for introduction into an ICP torch. Using a sequential spectrometer they determined Cr, Cu, Fe, Mg, Mn, Ni and Zn in aluminium alloys at typical alloying concentrations. Sainz et al. (86l C1533) described a development in the sampling of liquid metal for analysis by ICP-AES. A high-voltage spark was used to sample molten lead or lead - tin solder and a stream of Ar flushed the resulting metal vapour into the ICP torch. Precisions of 0.14.3% were claimed (87l43) for a general- ised internal reference method that was applied to theICP-AES determination of eight elements in aluminium alloys.Major, minor and trace elements were determined simultaneously on a direct-reading spectrometer and the spectral lines of the major elements and argon were used as the internal refer- ences. The procedure was successfully applied through a single-point calibration to determine concentrations which varied by up to two orders of magnitude. A method was described (86/1289) for the multi-element determination of major and minor constituents of “sub-micro” samples by ICP-AES. The same amounts of an internal standard were added to the sample and standard solutions so that accurate weighing and dilution were not necessary. The procedure was applied to the analysis of Co - Cr thin films and Co - Cu - Fe - Sm - Sr magnetic alloy.The results obtained were in good agreement with those achieved by analysis of macro-samples. Publications which described the use of direct current plasma atomic emission spectrometry for the analysis of non-ferrous metals showed no particular novelty. Ching and Chan (86lC1255) compared DCP-AES and ICP-AES for the150R JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, AUGUST 1987, VOL. 2 Table 3. SUMMARY OF ANALYSES OF NON-FERROUS METALS Element Ag Ag As As Au Au Ba Be Bi Cd Ce c o c o Cr c u Fe Ga H In Li Mo Na Ni 0 Pb Pt Ru Sb Se Se Si Sn Sn Te Th Ti Unm - - - - - 242.8, 267.6 553.6 234.9 - - - 304.4 - - 324.7 - - 656.3 303.9 - - - - 777.2 - 214.4, 265.9 - - - - - 224.6 - - - - Matrix Concentration Pd alloys - Cu metal p.p.m.levels Cu and Ni powders Trace level Cu alloys, steels Pt alloys Ag - Au alloys Metallurgical products Be - Cu alloys Cu metal Ultra-pure Al, water, hair Fe - Si alloys Pure Sn, glass, vegetation High-purity Ni Pre-treated A1 Standard alloys metal Co alloy Ni-based heat-resisting alloys Titanium Pb and Zn metals Metallurgical products Co alloy 0 .OO9-O .24% - - - 0.001-0.22% 0.2-10 pg g-1 - - ng g-1 levels - - - - p.p.m. levels - 10-1000 ng g-1 pg g-1 level - Technical grade A1 5-100 pg g-1 Co alloy - Titanium - Pb - Sn alloys Major Ag - Au alloys - cons ti tuen ts W metal 0.03-2% Cu alloys, steels 0.00%0.24% Cu and Ni powders Trace level Cu alloys, steels - Technique ; atomisation; analyte form* air - C2H2; L F, AA; -; - AA; Hy; L AE; ICP, Hy; - AA; ETA; L AE; ICP; L AA; F, AE; F, AE; spark; S N20 - CZHZ; L N2O - CZHZ; L AA; Hy; L AA; F; L AE; 1CP;- AF; ETA; S AE; ICP; L AA; ETA;- AE; KP;- AA; F, AA; F, AA; ETA; L air - C,H,; L air - C2Hz; L AE; MIP; G AA; ETA; L AA; F, -; L AE; F, -; L AA; F, L AE; a.c.arc; S AA; F, air - C2H2; L AE; MIP; G AA; F, AE; ICP; L N20 - GH2; air - C2H,; L AE; a.c. arc; S AE; ICP, Hy;- AE; ICP, Hy;- AA; Hy; L High-purity In Sub-p.p.m. levels AA;-; - Al-based alloys, 0.5% level AA; Hy; L foodstuffs Pb - Sn alloys Major AA; F, Ni-based p.p.m. levels AA; ETA; L constituents air - C,H,; L heat-resisting alloys A1 metal 10 ng g-1 level AE; ICP; L A1 metal 1-50 pg g-1 AE; ICP; L Sample treatment/comments Reference 8611826 Prepare sample solution containing 1% V/V acid and 0.1% m/V thiourea; addition of Fe removes interference by Pd Deposit Ag from solution on to H,-activated Pt gauze Separate analyte using Chelex 100 resin; a masking agent is needed with Cu matrix Hydride generation equipment made in-house; 8612026 871376 87lC991 masking agents needed when analysing Cu alloys Separate Au using ion-exchange procedure with Cellex D and Cellex T Extract ion pairs formed from iodo- compounds and tetradecyldimethylbenzyl- ammonium (Zephiramine) Compares performance of the two techniques Uses time-resolved laser-induced breakdown (LIBS) and long spark technique (LST) Uses AlzO,-coated silica tube as atom trap - Fluorescence is excited by tunable laser with furnace system under vacuum Treatment involves ion-exchange operations Complex extraction procedures involving organic reagents in molten naphthalene Dissolve in HC1 - HN03 - H3P04, buffer with A1 - H3P04 solution Dissolve in HF - HNO,; use furnace with L'vov platform Heat for 30 min, in He atmosphere; sweep Separate In using Amberlyst A-26 resin evolved gas into plasma loaded with Na salt of Xylenol Orange - See Fe, ref. 87/934 - See Fe , ref.871934 See H, ref. 8611441 Electrolytic dissolution in 3.5% V/VHCI See Au, ref. 8611788 Oxidise to WO,; mix 2 + 1 with graphite containing 6% mlm G+03 or 10% mlm PbO, See As, ref. 87lC991 See As, ref. 871376 See As, ref. 871C991 Attack by chlorination with CuCI2 at 470 "C Extract organic complex into CHCI, and generate hydride in non-aqueous medium See Pb, ref. 86/1370 See Ga, ref. 8611077 Various extraction and collection procedures Dissolve in HC1; collect analytes on La(OH), are described 87/C181 86/1788 87/C1068 87/35, 871481 871443 871104 8611066 871126 8611832 87/C549 8611325 871934 8611077 8611441 871644 871C1071 87/934 86/1044 871934 8611441 8611370 8611788 8611043 87lC991 871376 871C991 8611886 87112 8611370 8611077 8611833 8611033JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, AUGUST 1987, VOL.2 151R Table 3. SUMMARY OF ANALYSES OF NON-FERROUS METALS-continued Technique; atomisation; Concentration analyte form* 10 ng g-1 level 1-50 pg g-1 - AA; F, AE; ICP; L AE; ICP; L N 2 0 - CzH2; L ng g-1 level AA; ETA; L 1-50 pg g-1 AE; ICP; L - AE; ICP; L Element h/nm U V W 400.9 - - Matrix A1 metal A1 metal Alloys, ores Sample treatment/comments See Th, ref.8611833 See Ti, ref. 86/1033 Use alkaline medium with K2S208 as releasing agent Reference 8611 833 8611 033 87/40 871528 8611033 871049 8611042 8611075 861C1253 861C1254 861C1255 8611278 8611289 8611373 8611444 86lC1495 86lC1553 86lC 1554 86lC1562 8611622 8611623 8611651 86/1700 86/1701 8611876 8612021 87141 87167 871131, 87/C156 87/23 1 Zn - Zr - Zr - Ga metal A1 metal Pre-treated A1 metal B alloys Inject sample as liquid at 40-50 "C SeeTi, ref. 8611033 See Cr , ref. 87/C549 Various - Various - ( 5 ) Strip off 2000 pm layer for analysis Use electrochemical treatment to recover Describes application of commercial (B, Cr , Fe, Mn and Si) surface layers instrument (VG 9000) to a range of matrices and trace elements against ICP with other methods Describes evaluation of GDL technique Compares the techniques with each other and (Hf, Nb, Sc andTa) High-temperature Al, B, Ni, gallium alloys arsenide - AE; 1CP;- Various - Sub-p.p.m.levels MS; GDL; S Various - Various - Various - Various - (4) Pb and Pb alloys - AE; GDL; S Precious metals AE; DCP; - AE; ICP; - - 0.0 1-2% AE; ICP; L Mo and V metals Co - Cr and Sm - Co - Fe - Cu- Zr alloys High-purity A1 Major and minor AE; ICP; L constituents Describes various sample treatments for different matrices Various - ( 10) Trace levels AA; F, -; - Concentrate analytes using chelating ion-exchanger (Cellulose Hyphan); introduce sample to flame by injection technique (Bi, Ca, Cd, Cu, Fe, Mg, Mn, Ni, Sr and Zn) Describes the evaluation of the technique Various - Alloys Cu metal Major and minor AA; F, --; - constituents - AF; GDL; S Various - (4) Describes evaluation of optimum conditions using laser-excited fluorescence (Fe, Hg, In and Pb) Dissolve samples in nitro-tartaric acid Various - Pb alloys Major AE; DCP; L - AE; ICP; L - AE; ICP; L constituents Various - Various - A1 - Zn coatings Cu and Ni products, ores Precious metals Strip coatings using HCI containing As03 Gives details of attack on samples by fused Details use of copper sulphide to collect sodium peroxide analytes in assay process (Ag, Au, Ir, Pd, Pt, Rh and Ru) Dissolve in HBr - Br solution, fume with H,SO,; use HC1 to dissolve PbS04 (Ag, Bi, Cd, Cu, Fe, Ni and Zn) Method for direct analysis of metal samples (As, Cd, Mg, Pb, Se and Zn) Dissolution procedure uses mixed acids - AA;-;- AE; DCP; - AE; 1CP;- 10 pg g-1 level AA; F, air - C,H2; L Various - (7) Various - (7) Pb- and Sn-based alloys Ni-based alloys Cr - Si - W alloys Mn metal Ni-based alloys Various - Various - (6) 50 Pg g-' AE; ETA-ICP; S Major AA; F,-; L constituents - AE; arc; - Uses automated instrument with linear charge-coupled photodiode array detector for qualitative and semi-quantitative analyses Uses second derivative wavelength modulated technique (Co, Cu, Fe, Mn, Ni, Pb and Zn) Various - Various - (7) - AE; -; - AF; F, AE; d.c.arc; S air - C2Hz; - 0.05-1.5 % Cu alloys Various - ( 5 ) Mg - Y alloy Ignite nitrate residue to oxides, mix with C powder buffer containing Co304 internal standard and AgCl ascarrier (Cu, Fe, Mo, Ni and Si) Uses a direct insertion procedure (Cd, Mg, Pb and Zn) Attack with 50% V/VHCI and complete solution with HF - HN03.Discusses the effect of oxide formation on results (Ag, As, Cd, Ga, Se and Te) Samples turned from rods or pressed powders with 3 mm deep x 3 mm diameter cavity; ICP technique used for calibration Describes a modified torch and crucible for direct sample introduction (Bi, Pb, Te and Zn) Various - Various - (4) (6) Ni-based alloys Ni-based alloys Sub-p.p.m. level AE; ICP; S 1-100 pg g-1 MS; ICP; L Brass, steel CRMs Various - Major AE; HCL; S constituents Various - (4) 10 pg g-1 level AE; ICP; S152R JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, AUGUST 1987, VOL. 2 ~~ Table 3. SUMMARY OF ANALYSES OF NON-FERROUS METALS-continued Element Unm Various - (6) Various - (9) Various - Various - (7) Various - Various - Various - (34) Various - Various - (13) Various - Various - (8) Various - (11) Technique; atomisation; Matrix Concentration analyte form* Mo and W powders pg g-1 level AA;-;L Rare earth - Co Major and minor AE; ICP; L magnet alloys constituents Precious metals ng g-1 levels AF; ICP; L A1 alloys Alloying level AE; ICP; S Mg-based alloys - AE; 1CP;- Pyro-metallurgical - products AE; ICP; L High-purity Sn Trace levels AE; d.c.arc; S Alloys O.I-5OYo AE; ICP; - Co,CuandNi - AA; -; - alloys High-purity Pt - AA;F,-;L Ag,CuandPb - AA; -; - Hard metals 0.001-2% AA; F,-; L alloys Sample treatmentlcomments Reference Pre-concentrate analytes using styrene polymer with functional groups (Co, Cu, Fe, Mn, Ni and Zn) Be as internal standard (Ce, Co, Cu, Fe, Hf, Mn, Sm, Y and Zr) Dissolve in aqua regia, dilute with HC1; add - Uses a spark sampling technique, sweeping vapour into the plasma (Cr, Cu, Fe, Mg, Mn, Ni and Zn) Study of performance of low-power torch (ARL Minitorch) Mix finely powdered sample 4 + 1 with flux (Li2B407 containing 1 % mlm Sc2O,); suspend 0.5 g sample in 25 ml glycerol - water mix (2 + 3) residue with graphite containing 0.5% mlm NaCl Describes the use of a sequential spectrometer Remove Sn by bromination in CCl,; mix 871322 87l479 871C550 87/C815 87/C883 871935 871936 87lC 10 19 - 87/C1064 Extract Pt with IBMK - isoamyl alcohol 87/C 1069 (Al, Ca, Cr, Cu, Mg, Mn, Ni and Pb) - 871C1070 8711 166, 8711167, 8711168, 87/1169 British Standard BS 5600; sub-section 4.17.1986 gives full details (Ca, Co, Fe, K, Mg, Mn, Mo, Na, Ni, Ti and V) * Hy indicates hydride generation and S , L and G signify solid, liquid or gaseous sample introduction, respectively.Other abbreviations are listed elsewhere. determination of trace impurities in high-purity gold, pallad- ium and platinum. No specific results were mentioned in the abstract, but the parameters compared included instrument stability and reproducibility, the extent of stray light and spectral interferences, matrix enhancement and depression, line resolution and selection, and over-all ease of operation. Kallmann (86/1622) used DCP-AES as an alternative tech- nique to AAS or ICP-AES for the analysis of precious metal residues collected on copper sulphide. No interferences of copper on Au, Ir, Pd, Pt and Rh were reported, but there was a slight effect on the determination of Ru.In the DCP-AES determination of As, Cu, Pb, Sb and Sn in antimonial lead alloys used in lead - acid batteries (86/C1553), matrix matching was required to obtain a consistent background emission signal. Although use of nitro-tartaric acid to dissolve the samples resulted in precipitation of metastannic acid, this presented no problem to the system. The sole reported application of microwave induced plasma atomic emission spectrometry was by Hanamura et al. (86/ 1441) who used a He plasma to determine H and 0 liberated from titanium by heat treatment. Water was used to provide calibration signals. The application of inductively coupled mass spectrometry for the determination of Ag, As, Cd, Ga, Se and Te in nickel-based alloys was found to be severely limited (87/67) by the formation of matrix metal oxide ions of the same nominal mass as the trace metaI ions of interest.The spectral interferences were most significant in the middle mass range (69-140 u) and a resolution capability of between 5000 and 50 000 was considered necessary for adequate separation of the metal oxide and metal ion peaks. 3.1.4. Discharge lamp methods The versatility of the glow discharge lamp was illustrated in three conference presentations that discussed combinations of this source with different detection systems. Schmitt (86/ C1254) described the use of GDL-AES as a faster alternative to solution ICP-AES for production analyses in the lead battery industry. The main characteristics of a GDL as an atomisation source in laser-excited AFS were evaluated by Pate1 and Winefordner (86/C1495) for the determination of Fe, Hg, In and Pb in copper.The composition of the copper rod was found to affect sputtering rates and the release of Pb from the sample. This and other matrix effects resulted in poor correlation and non-linearity of the analytical curve for the measurement of Pb in SRM copper. Hutton et al. (86lC1253) gave a comprehensive description of the use of a commercially available GDL-MS system for the determination of trace impurities in a variety of matrices. Trace levels of Cu, Fe, Mg, Si, Ti and Zn were measured in ultrapure aluminium by a semi-quantitative procedure which gave results within a factor of three of the true value.A 15-30 min pre-analysis period was required to remove surface contaminants and the 2040 pm oxide layer on the aluminium surface. The GDL-MS system was also used for the semi-quantitative analysis of an electro-refined nickel sample and the sub-p.p.m. concentra- tions of 16 elements were obtained in approximately 25 min. Two modes of use were reported for the hollow-cathode lamp source. De Marco et al. (87/131) used cathodes prepared from samples either in the solid form or as pressed powder, to determine the major constituents of brass and steel. Use of pressed powder samples permitted the incorporation of aJOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, AUGUST 1987, VOL. 2 153R known amount of internal standard. Marcus and Harrison (8611821) continued their investigation of the HCL plume as an emission source (see JAAS, 1986, 1, 106R; 861259, 86lC622).3.2. Atomic Absorption Methods A variety of extraction and pre-concentration procedures were used prior to the analysis of a range of non-ferrous metals by atomic absorption spectrometry. Ion-exchange procedures were used in the FAAS determination of ten trace impurities in aluminium at sub-p.p.m. levels (8611373) and for six impurities in molybdenum and tungsten (871322) at levels below 10-2% mlm. Solvent extraction in n-butanol (8611418) was used for matrix removal of selenium prior to the determination of 13 trace elements. Tin at the p.p.m. level was extracted from aluminium (87/12) using a chloroform solution of the ammonium salt of N-nitrosophenylhydroxamic acid.A somewhat unusual procedure was proposed by Nagahiro et al. (8611325) in which a copper complex of 2,4,6,-tri(2- pyridyl)-l,3,5-triazine was extracted into molten naphthalene followed by dissolution in DMF. This rather involved proce- dure is an extension of the work of Lin et al. noted in the previous review (see JAAS, 1986, 1, 102R; 86/972) which proposed the use of naphthalene in solution. Precious metals have been determined (8611643) at p.p.m. and sub-p.p.m. levels by collection in silver beads followed by dissolution in alkaline cyanide. Vanadium was used to suppress the interfer- ences. Another unusual application of AAS was described (8611700) for the determination of major constituents in Cr - Si - W materials. The flame conditions were optimised so that Cr, Si and W could be measured in one solution.Huang and Luo (87/104) investigated the use of an alumina-coated silica tube as an atom trap for the determina- tion of Cd in aluminium using a fuel-lean flame in the collection phase and a fuel-rich flame for the release phase. Detection limits down to p.p.b. levels in solution were achieved. The effect of various buffers on sensitivity was investigated (871934) in the determination of Fe, Mo and Ni in cobalt alloys. A solution containing aluminium and H3P04 enhanced the sensitivity when Mo was determined with a N20 - C2H2 flame. An air - CzHz flame was used for the determination of Fe and Ni. Chinese workers (871528) described an interesting method where molten gallium at 40-50 "C was injected directly into a graphite furnace for the determination of Zn at p.p.b.levels. Interference by gallium was eliminated by not allowing the atomisation temperature to exceed 1300 "C, and a detection limit of 1 p.p.b. Zn was achieved with an'dSD of <lo% for 5 p.p.b. Zn. 3.3 Atomic Fluorescence Methods A laser-excited atomic fluorescence spectrometry (LEAFS) system based on a Nd : YAG laser, a dye laser and a graphite cup electrothermal atomiser (871126) was used €or the determination of Co in pure tin at the p.p.b. level. The sample was placed in a graphite cup positioned inside a metallic cell that could be evacuated to 10-2 torr prior to electrothermal vaporisation (VETA). Although atomisation in vacuum produced a solution detection limit of 0.2 ng ml-1 Co which was two orders of magnitude poorer than for vaporisation at atmospheric pressure, the authors suggested that the LEAFS- VETA method provided opportunities for direct solids analysis with reduced matrix interferences.LOCATION OF REFERENCES The full references cited in this Update have been published as follows: 8611031-8611460, J . Anal. At. Spectrom., 1986, 1(4), 107R-120R. 8611461-86/1834, 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. 871396871637, J. Anal. At. Spectrom., 1987, 2(3), 69R-77R. 871638-8711169, J . Anal. At. Spectrom., 1987, 2(4), 115R-131R. 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 86J1033. Fukuoka-ken Kitakyushu Kogyo Shikenjo Kenkyu Hokoku, 1985, 39. 8611038. Fresenius Z . Anal. Chem., 1985, 321, 677. 8611042. Zavod. Lab., 1985, 51(8), 33. 8611043. Zavod. Lab., 1985, 51(8), 34. 8611044. Zavod. Lab., 1985, S1(8), 36. 8611056. Anal. Chem., 1985, 57, 2481. 8611062. At. Spectrosc., 1985, 6(4), 81. 8611063. Bunseki Kagaku, 1985, 34(7), T85.8611064. JSAE Rev., 1985,16,28.8611065. Goriva Maziva, 1985,24,27. 8611066. Imono, 1985,57,534. 8611075. Ber. Kernforschungsanlage Jiilich, 1985, Jul-1975, 131 pp.8611077. Nippon Kinzoku Gakkaishi, 1985, 49, 656. 8611278. Bunseki Kagaku, 1985, 34, T77. 86/1289. Guangpuxue Yu Guangpu Fenxi, 1985,5(4), 37.8611314. Nucleotecnica, 1985, 4(8), 28. 8611325. Zh. Anal. Khim., 1985, 40, 1601. 8611327. Zavod. Lab., 1985, 51(9), 29. 8611361. Rev. Metal. (Madrid), 1985, 21(2), 87. 8611369. Anal. Chim. Acta, 1985, 173, 97. 8611370. Galvanotechnik, 1985, 76, 1428. 8611373. Fresenius 2. Anal. Chem., 1985, 322, 166. 8611376. Zh. Anal. Khim., 1985,40, 1833. 8611391. Spectrochim. Acta, Part B , 1985,40, 1167. 86J1393. Spectrochim. Acta, Part B , 1985, 40, 1205. 8611406. Rocz. Panstw. Zakl. Hig., 1985,36(3), 197. 8611411. J . Vac. Sci. Technol., A , 1985, 3, 2364. 86J1418. Fresenius Z . Anal. Chem., 1985,322,404. 8611419. ATOMKI Kozl., 1985, 27, 373. 8611441.Can. J. Spectrosc., 1985,30(2), 46.8611444. Fresenius 2. Anal. Chem., 1985,322, 11. 8611452. Proc. SPIE-lnt. SOC. Opt. Eng., 1985, 540(Proc. Southwest Conf., Opt.). 86/1453. Anal. Chim. Acta, 1985, 175, 325. 8611456. Fresenius Z . Anal. Chem., 1985,322, 514. 8611463. Spectrochim. Acta, Part B , 1985, 40, 1447. 8611464. Anal. Lett., 1985, 18 (A14), 1723. 86J1465. Anal. Lett., 1985, 18 (B15), 1887. 8611621. Talanta, 1986, 33, 61. 8611622. Talanta, 1986, 33, 75. 8611623. Talanta, 1986,33,91. 8611629. Anal. Chem., 1986, 58, 658. 86J1635. Analyst, 1986,111,225. 8611643. Analyst, 1986, 111, 291. 8611646. In?. Lab., 1985, Nov./Dec., 60. 8611650. Anal. Proc., 1986, 23, 8. 8611651. Anal. Proc., 1986,23, 15. 8611698. Fresenius Z. Anal. Chem., 1985,322,371.8611699. Fresenius Z . Anal. Chem., 1985,322,154R JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, AUGUST 1987, VOL. 2 495. 8611700. Fresenius Z . Anal. Chem., 1985, 322, 401. 8611701. Zh. Prikl. Spektrosk., 1985, 43, 377. 8611703. Guangpuxue Yu Guangpu Fenxi, 1985, 5(5), 47. 8611713. Fresenius Z . Anal. Chem., 1985,322,383.8611716. Zh. Anal. Khim., 1985,40, 1563. 8611722. Khim. Tekhnol. Topl. Masel, 1986, (l), 35. 8611743. Anal. Chim. Acta, 1985, 175, 211. 8611746. Ryusan to Kogyo, 1985, 38(9), 159. 8611781. Anal. Chem., 1986, 58, 511. 8611786. Zh. Anal. Khim., 1985,40,2025.86/1788. Bunseki Kagaku, 1985,34,671.86/1789. Kung Yeh ChiShu, 1985,137, 75. 8611803. Fresenius Z. Anal. Chem., 1985, 322, 713. 8611810. Dtsch. Zahnaerztl. Z . , 1985,40,1187.86/1821.Anal. Chem., 1986, 58, 797. 8611826. Guangpuxue Yu Guangpu Fenxi, 1985, 5(5), 64. 8611832. Anal. Lett., 1985, 18(A19), 2477. 8611833. Mikrochim. Acta, 1985, 2, 85. 8611841. Appl. Spectrosc., 1986, 40, 274. 8611876. Spectrosc. Lett., 1985, 18, 781. 8611884. Hutn. Listy, 1985, 40,812. 8611886. Zh. Anal. Khim., 1986, 41, 80. 8611923. Finn. Chem. Lett., 1985, ( 5 ) , 186. 8611933. Hutn. Listy, 1985, 40, 882. 8611952. Zavod. Lab., 1986, 52(2), 38. 8611989. Appl. Spectrosc., 1986, 40, 330. 8612021. Fenxi Huaxue, 1985, 13, 879. 8612022. Analyst, 1985, 110, 1481. 8612026. Talanta, 1986, 33, 155. 8612032. Talanta, 1986, 33, 279. 8716. Fenxi Huaxue, 1986, 14, 119. 8719. Talanta, 1986, 33, 358. 87111. Talanta, 1986, 33, 445. 87/12. Talanta, 1986, 33, 458. 87124. Spectrochim. Acta, Part B , 1986, 41, 3. 87/35. Appl. Spectrosc., 1986,40,491.87/40. Analyst, 1986,111,115. 87/41. Spectrochim. Acta, Part B , 1986, 41, 63. 87/42. Spectrochim. Acta, Part B , 1986, 41, 73. 87143. Spectrochim. Acta, Part B , 1986, 41, 105. 87/59. Anal. Chem., 1986, 58, 1734.87160. Anal. Chem., 1986,58,1739.87/67. Spectrochim. Acta, Part B , 1986,41,169. 87/69. Spectrochim. Acta, Part B , 1986,41, 193. 87/83. Analusis, 1986, 14, 158. 87/84. Analusis, 1986, 14, 139. 87/85. Anal. Chim. Acta, 1986,179,491. 87/86, Erdoel Kohle, Erdgas, Petrochem., 1986, 39, 193. 87/87. Spectrochim. Acta, Part B , 1986, 41, 303. 87/88. J. Chromatogr., 1986, 351, 465. 87199. Guangpuxue Yu Guangpu Fenxi, 1985, 5(3), 23. 871101. Guangpuxue Yu Guangpu Fenxi, 1985, 5(3), 59. 871102. Zh. Anal. Khim., 1986, 41, 675. 871104. Fenxi Huaxue, 1986, 14, 198. 871125. Spectrochim. Acta, Part B , 1986,41,475.87/126. Spectrochim. Acta, Part B , 1986,41,487.87/127. Spectrochim. 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ISSN:0267-9477    

DOI:10.1039/JA987020133R

出版商:RSC    

年代:1987

数据来源: RSC

摘要:

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Thijssen, T., Janssens, E., VandenBussche, P., Vonk, W., A flexible software approach for optical emission spec- trometers, (Philips Export, Lelyweg 1, 7602 EA Almelo, The Netherlands). Henry, R., Grote, B., Advantages of using optimised plasma conditions in a sequential scanning ICP, (Bodenseewerk Perkin-Elmer and Co. GmbH, Berliner StraBe 312, 6050 Offenbach, Main, FRG).Horlick, G., Lepla, K., Measurement characteristics and capabilities of a Hamamatsu PDA image sensor for ICP-AES, (Dept. Chem., Univ. Alberta, Edmonton, Alberta T6G 2G2, Canada). Muszynski, M., JY 38 PLUS, a new generation of ICP sequential spectrometers, (Instruments SA, Division Jobin-Yvon, 16 rue du Canal, 91160 Longjumeau, France). Thijssen, T., Jonkers, A., VandenBussche, P., Janssens, E., Performance of a programmable scanner in a simul- taneous ICP spectrometer, (Philips Export, Lelyweg 1, 7602 EA Almelo, The Netherlands). Horlick, G., Todd, B., King, G., A Fourier transform spectrometer system for ICP-AES, (Dept. Chem., Univ.Alberta, Edmonton, Alberta T6G 2G2, Canada). Johnson, T. J., A low power, low flow excitation system for ICP-AES, (ARL Applied Research Laboratories SA, En Vallaire, 1024 Ecublens, Switzerland). van der Plas, P. S. C., de Galan, L., Investigation into ceramic materials for externally cooled ICP torches, (Lab. Anal. Chem., Delft Univ. Technol., De Vries van Heystplantsoen 2, 2628 RZ Delft, The Netherlands). De Win, A. P. M., Evaluation of the silicon blank value in inductively coupled plasma, (Philips Elcoma, Complex Beatrix, Bldg BL, room 70, Hurksestraat, Eindhoven, The Netherlands). Dubois, D., Soudikre, J., The use of a Babington type nebuliser with d.c. plasma emission spectrometry, (ARL Applied Research Laboratories SA, En Vallaire, 1024 Ecublens, Switzerland).Klok, A., Jansen, E. B. M., Sensitivity enhancement by the use of a special designed nebuliser for ICP-AFS, (Baird Europe B.V., Produktieweg 30, 2382 PC Zoeterwoude, The Netherlands). Steffan, I., Vujicic, G., A new nebuliser for ICP analysis of solutions with high salt contents, (Analytical Institute, University of Vienna, A-1090 Vienna, Wahringerstrasse 38, Austria). Stahl, R. G., Timmins, K. J., Experiences with a glass frit nebuliser, (Directorate of Quality Assurance, Technical Support, Materials Centre, Royal Arsenal East, Wool- wich, London SE18 6TD, UK). Foetisch, M., Olle, M., Imbert, J. L., Trassy, C., Comparison of several sample introduction systems in ICP-AES, (ARL Applied Research Laboratories SA, En Vallaire, 1040 Ecublens, Switzerland). 87/C1358.87/C 1359. 87x1360, 87/C1361. 87/C1362. 87/C1363. 87/C1364. 87/C1365. 87/C1366. 87lC1367. 87lC1368. 87/C1369. 871C1370. 87/C1371. 87/C 1372. 87K1373. 87/C 1374. Kreuning, G., Maessen, F. J. M. J., Experimental control of the solvent plasma load of argon ICPs, (Laboratorium voor Analytische Scheikunde, Univ. Amsterdam, Nieuwe Achtergracht 166, 1018 WV Amsterdam, The Nether- lands). Ebdon, L., Dean, J. R., Stockwell, P. B., Recent advances in hydride generation plasma spectrometry, (Dept . Envi- ron. Sci., Plymouth Polytechnic, Drake Circus, Plymouth, Devon PL4 SAA, UK). Steffan, I., Vujicic, G., “Off-line”, hydride generator for ICP-AES, (Anal. Inst., Univ. Vienna, A-1090, Wahrin- gerstrasse 38, Austria). Vermeiren, K. A., Taylor, P. D, P., The appraisal of thermospray as a method for sample introduction into an inductively coupled plasma, (Inst.of Nucl. Sci., State Univ. Ghent, Proeftuinstraat 86, B-9000 Ghent, Belgium). Disam, J., Schaack, S., Steiner, J.-D., Analyse your solid directly with ICP, (Schott Glaswerke, Dept. TSM, Hatten- bergstr. 10, D-6500 Mainz 1, FRG). Jansen, E. B. M., Klok, A,, Multi-element determination of microlitre samples with an electrothermal sample introduction device and rapid data aquisition for ICP- OES, (Baird Europe B.V., Produktieweg 30, 2382 PC Zoeterwoude, The Netherlands). Lemarchand, A., Labarraque, G., Masson, P., Broekaert, J. A. C., The analysis of ferrous alloys by spark ablation coupled to ICP optical emission spectrometry, (Instru- ments S.A., Division Jobin-Yvon, rue du Canal 16-18, F 91 163 Longjumeau-Cedex, France).Zaray, G., Broekaert, J. A. C., Leis, F., Burba, P., Analysis of high-purity aluminium by direct sample insertion ICP-OES combined with trace element pre- concentration, (Institut fur Spektrochemie und ange- wandte Spektroskopie, P.O. Box 778, D-4600 Dortmund 1, FRG). Cox, A. G., McLeod, C. W., Miles, D. L., Cook, J. M., Trace enrichment and determination of sulphate by flow injection - inductively coupled plasma emission spec- trometry, (Dept. Chem., Sheffield City Polytechnic, Sheffield S1 lWB, UK). Mathe, D., Herbeiin, P., Sample preparation microwave digester - laboratory robotics, (SociCtC Prolabo, 12 rue PelCe, 75011 Paris, France). Lernarchand, A., Obadia, J. M., Role of the frequency and the technology of generators in ICP-AES, (Jobin-Yvon, Instruments S.A., 16-18 rue du Canal, 91163 Longjumeau Cedex, France).Garavaglia, R., Interference from easily ionisable ele- ments in ICP emission spectroscopy: analytical aspects, (CISE, P.O. Box 12081, Milano, Italy). Tang, Y. Q., Diemiaszonek, R., Trassy, C., Charge transfer in analytical ICPs, (Lab. Physicochim. Indus- trielle, INSA, Bat. 401, 69621 Villeurbanne Cedex, France). Marichy, M., Mermet, M., Mermet, J. M., Relation between limits of detection and mechanisms in ICP-AES, (Lab. Sci. Anal., Bat. 308, Univ. Claude Bernard-Lyon I, 69622 Villeurbanne, Cedex, France), Tang, Y. Q., Diemiaszonek, R., Trassy, C., Thermal and collisional processes in ICP, (Lab. Physicochim. Indus- trielle, INSA, Bat. 401, 69621 Villeurbanne Cedex, France).Murillo, M., Mermet, J. M., Relation between operating parameters and line energy in ICP-AES, (Lab. Sci. Anal., Bat. 308, Univ. Claude Bernard-Lyon I, 69622 Villeur- banne Cedex, France). Turk, G. C., Axner, O., *Omenetto, N., Optical detection of laser induced ionisation in the inductively coupled plasma for the study of ion - electron recombination and ionisation equilibrium, (Joint Res. Cent. Ispra, Chem. Div., Ispra, Varese, Italy).162R JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, AUGUST 1987, VOL. 2 871C1375. Yang, P., Barnes, R. M., Experimental and theoretical evaluation of a low-power oxygen inductively coupled plasma discharge for spectrochemical analysis, (Dept . Chem. , Univ. Massachusetts, GRC Towers, Amherst, 87/C1376. Erlich, S., Brenner, I.B., Goldbart, Z., Characteristics of a low-power nitrogen - argon ICP for multi-element analytical emission spectrometry, (Geol. Surv. of Israel, 30 Malke Israel St., Jerusalem 95501, Israel). 871C1377. Meyer, G. A., Total consumption sample introduction into an air ICP using a direct injection nebuliser, (The Dow Chemical Company, Michigan Appl. Sci. Technol. Labs. , 1602 Building, Midland, MI 48674, USA). 87/C1378. Durr, R. C., Mermet, J. M., Trassy, C., Determination of trace elements in air using argon and air ICPs, (ESI Durr, Rue J. Porraz, 73201 Altberville, France). 87/C1379. Bergey, C., Birolleau, J. C., Thouzeau, F., Durr, R. C., Air ICP uses for instantaneous monitoring of airborne pollutants, (CEA, Service CQ, BP 12, 91680 Bruyeres le Chatel, France).87/C1380. Williams, J. G., Polyatomic, oxide and doubly charged ions on a VG PlasmaQuad ICP-MS system, (Dept. Chem., Univ. Surrey, Guildford, Surrey GU2 5XH, UK). 871C1381. Hutton, R. C., Cantle, J. E., Eaton, A. N., Practical figures of merit in ICP-MS, (VG Isotopes Ltd., Ion Path, Road Three, Winsford, Cheshire CW7 3BX, UK). 87/C1382. Gray, A. L., Williams, J. G., Optimisation of a commer- cial ICP-MS instrument for routine multi-element analysis, (Dept. Chem., Univ. Surrey, Guildford, Surrey GU2 5XH, UK). 871C1383. Boorn, A., Fulford, J., Gillson, G., Complete elemental analysis by ICP-MS, (SCIEX, 55 Glen Cameron Rd., Thornhill, Ontario L3T 1P2, Canada). 871C1384. Hulmston, P., Recent applications of inductively coupled plasma mass spectrometry, (Chemistry and Explosives Division, Atomic Weapons Research Establishment, Aldermaston, Berkshire, UK).871C1385. Long, S. E., Isotope dilution determinations by ICP-MS, (Environ. and Medical Sci. Div., Harwell Lab., Oxford- shire OX11 ORA, UK). 871C1386. Boorn, A., Gillson, G., Fulford, J., Douglas, D., Quan, E., Analysis of complex samples by ICP-MS, (SCIEX, 55 Glen Cameron Rd., Thornhill, Ontario L3T 1P2, Canada). 87/C1387. Brown, R. M., Pickford, C. J., ICP-MS as a detector for environmental levels of low specific activity radionuclides, (Environ. and Medical Sci. Div., Harwell Lab., Oxford- shire OX11 ORA, UK). 871C1388. Taylor, P. D. P., McLaren, J. W., The determination of trace elements in biological and environmental reference materials using ICP-MS, (Inst.Nucl. Sci., State Univ. Ghent, Proeftuinstraat 86, B-9000 Ghent, Belgium). 87/C1389. Luck, J., Determination of low REE concentrations in iron formating samples by ICP-MS, (Hahn-Meitner-Insti- tut Berlin GmbH (HMI), AG Geochemie, Glienicker- straae 100, D-1000 Berlin 39, FRG). 871C1390. Date, A. R., Cheung, Y. Y., Stuart, M. E., The application of ICP-MS to the analysis of iron-rich samples, (British Geol. Surv., 64 Gray’s Inn Road, London WClX 8NG, UK). 87/C1391. Jackson, S. E., Fryer, B. J., Gosse, W., Healey, D. C., Longerich, H. P., Strong, D. F., Determination of the precious metals in geological materials by inductively coupled plasma mass spectrometry, (Dept. Earth Sci., Memorial Univ. Newfoundland, St. John’s, Newfound- land A1B 3x5, Canada). 871C1392.Date, A. R., Stuart, M. E., The application of ICP-MS to the determination of halides in urban dust, (British Geol. Surv., 64 Gray’s Inn Road, London WClX 8NG, UK). MA 01003-0035, USA). 871C1393. Dean, J. R., Crews, H. M., Ebdon, L., Massey, R., Speciation of trace metals in foodstuffs by HPLC - ICP-MS, (Dept. Environ. Sci., Plymouth Polytechnic, Drake Circus, Plymouth, Devon PL4 8AA, UK). 871C1394. Brenner, I. B., Lemarchand, A., Gatel, G., Lang, Y., Grosdaillon, P., A critical evaluation of the analytical performance of the Grimm discharge lamp (GDL), inductively coupled plasma (ICP) and spark generator (SG) ICP atomic emission spectrometries (AES) for multi-element analysis of geological samples and related materials using sequential and simultaneous spectromet- ers, (Geol.Surv. of Israel, 30 Malke Israel St., Jerusalem 95501, Israel). 871C1395. Vandenhssche, P., Thi-issen, T., Evaluation of GDL as an 87/C 871C 871C analytical technique for the .metal industry, (Philips Export, Lelyweg 1, 7602 EA Almelo, The Netherlands). 396. Hall, D., Charalambous, P. M., Sanderson, N. E., GDMS for material analysis, (VG Isotopes Ltd., Ion Path, Road Three, Winsford, Cheshire CW7 3BX, UK). 397. Bengtson, A., Lundholm, M., Surface analysis with the GDL-some aspects of the quantification problem, (Swedish Inst. for Metals Res., Drottning Kristinas vag 48, A-114 28 Stockholm, Sweden). 398. Ohannessian, L., Hocquaux, H., Tousset, J., Surface analysis by glow discharge. Target sputtering yield: com- parison of theory - experiments, (Cent.Recherches d’Uni- eux, BP. 34, 42701 Firminy, France). 87/C1399. Paski, E., Blades, M. W., Laser excited time-wavelength resolved spectroscopy of solid state mixtures, (Dept. of Chem., 2036 Main Mall, Univ. British Columbia, Van- couver, BC V6T 1Y6, Canada). 87/C1400. Bador, R., Morin, M., Dechaud, H., Desuzinges, C., Laharotte, C., Laser-induced luminescence of lanthanide chelates: application to fluorescent labelling of biomole- cules, (Lab. Biophys., Fac. Pharm., Univ. Claude Ber- nard-Lyon I, 8 avenue Rockefeller, 69373 Lyon Cedex 08, France). 87/C1401. Favarger, P.-Y., ICP and fresh water sediment poly- metallic pollution: how to optimise trace determination in varying matrices, (Institut F.-A. Forel, Univ. Gentwe, Switzerland). 87/C1402. Muszynski, M., New approach to the fast analysis of Na, Li, K by ICP method, (Instruments S.A., Division Jobin-Yvon, 16 rue du Canal, 91160 Longjumeau, France).87/C1403. de Gelis, P., Berneron, R., Surface analysis of steel by ICP-OES, (IRSID, St. Germain en Laye, France). 87/C1404. Gomez Coedo, A., Dorado Lopez, M. T., Vindel Maeso, A., ICP analysis of Co-base superalloys, (CENIM, Gre- gorio del Amo, 8, 28040-Madrid, Spain). 871C1405. Brenner, I. B., Erlich, S., Grosdaillon, P., Trace element analysis of refractory metallurgical materials: a critical evaluation of internal references and high resolution spectrometers, (Geol. Surv. Israel, 30 Malkhe Israel St., Jerusalem 95501, Israel). 87/C1406. Ibar, A., Berisha, M., Djeli, A., Krijestorac, Z., The application of ICP to the production control analysis of lead and zinc flotation and metallurgy, (Fac.Sci., Chem. Dept., Univ. Kosova, 38000 Prishtina, Yugoslavia). 871C1407. Baucells, M., Lacort, G., Roura, M., Pd, Fe and Cu determination in gold by inductively coupled plasma emission spectrometry (ICP) technique , (Servei d’Espec- troscbpia, Univ. Barcelona, Gran Via 585, 08007 Barce- lona, Spain). 871C1408. Grote, B., Henry, R., Analysis of precious metals using ICP-AES, (Bodenseewerk Perkin-Elmer and Co. GmbH, Berliner StraJ3e 312, 6050 Offenbach, Main, FRG). 87/C1409. Reynolds, B. J., Notton, J. H. F., Whitehead, P., Charac- terisation of trace element in platinum standard, (Johnson Matthey Technology Centre, Sonning Common, Reading, UK).JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, AUGUST 1987, VOL.2 163R 87/C1410. Whitehead, P., The use of internal standards for precious metal analysis by inductively coupled plasma emission spectrometry, (Johnson Matthey Technology Centre, Son- ning Common, Reading, UK). 87lC1411. Barbaro, M., Passariello, B., Determination of precious metals by atomic spectroscopy, (Istituto peril Trattamento dei Minerali, Via Bolognola, 7 Rome, Italy). 87K1412. Thouzeau, F., Birolleau, J. C., Lavergne, M., Bergey, C., Simultaneous determination of U, Np, Pu, Am by ICP-AES, (CEA, Service CQ, BP 12, 91680 Bruykres-le- Chiitel, France). 87/C1413. Kocken, J. W. M., Analyses of very concentrated geo- chemical samples with ICP-ES, (Dept. of Geochem., Inst. Earth Sci., Univ. Utrecht, PO Box 80.021, 3508 TA Utrecht, The Netherlands).87/C1414. Castillo, J. R., Molinero, A. L., Marco, E., Element determination at macro-, micro- and trace level in geolog- ical samples by ICP emission spectroscopy, (Dept. Anal. Chem., Univ. Zaragoza, Zaragoza, Spain). 871C1415. Noras, P., Wansen, G., On the use of solution-insert capability of ICAP spectrometry in geochemical mapping, (Geol. Surv. Finland (GSF), SF-02150 ESPOO, Finland). 87/C1416. Vujicic, G., Flury, W., Bermanec, V., ICP-AES determi- 87/C 14 87/C14 nation of plagioclase feldspars Brutto formulae, (IWM Zurich, Industriestrasse 59, CH-8152 Glattbrugg, Switzer- land). 7. Walsh, J. N., Barker, J. E., Direct determination of the rare earth elements by ICP-OES in geological samples: testing the limits of detection in routine analysis, (Dept.Geol., R. H. B. New College, University of London, Egham Hill, Egham, Surrey TW20 OEX, UK). 8. Guecheva, M., Analysis of acidic ammonium acetate - EDTA soil extracts by ICP spectrometry, (Swiss Federal Inst. of Forestry Res., CH-8952 Birmensdorf, Switzer- land). 871C1419. Dubois, D., Soudiere, J., Determination of various trace elements in high purity BGO crystals using d.c. plasma emission spectrometry, (Analub SA, 138 Rue du Centre, 1025 St. Sulpice, Switzerland). 87/C1420. David, P., Anzola, M,, Thouzeau, F., Bergey, C., Precise determination of major components in barium titanates by ICP-AES, (CEA, Service CQ, BP 12, 91680 Bruykres le Chiitel, France). 87/C1421. Fodor, P., Bertknyi, I., Analysis of agriculture sample using ICP-AES, (Univ. of Horticulture, Villhnyi u.31, 11 14 Budapest , Hungary). 871C1422. Leblondel, G., Mauras, Y., Allain, P., Interest of a simultaneous ICP-OES instrument (JY 48) for the study of elements in animals, (Lab. de Pharmacol., C.H.U., 49033 Angers, France). 87/C1423. Allain, P., Mauras, Y., Interest of a simultaneous ICP- OES spectrometer in clinical chemistry (JY 48), (Lab. de Pharmacol. , C.H.U., 49033 Angers, France). 87K1424. Foetisch, M., One, M., Imbert, J. L., Analysis of trace elements in dairy products by ICP-AES technique, (ARL Applied Research Laboratories S.A., En ValIaine, 1024 Ecublens, Switzerland). 87lC1425. Brescianini, C., Valerio, F., Mazzucotelli, A., Frache, R., Determination of trace amounts of zirconium in airborne particulates by ICP, (Istituto Nazionale per la Ricerca sul Cancro, Viale Benedetto XV, 10 Genoa, Italy), 87/C1426. Bezur, L., Ernyei, L., Cui, X., Pungor, E., Simultaneous multi-element analysis of blood serum with ICP injection technique, (Dept.for General and Anal. Chem., Tech. Univ. Budapest, 1521 Budapest, Gellert ter 4, Hungary). 87K1427. Horlick, G., Mixed gas inductively coupled plasmas, (Dept. Chem., Univ. Alberta, Edmonton, Alberta, T6G 2G2, Canada). 87/C1428. Montaser, A., Chan, S.-K., A helium inductively coupled plasma: background spectra emitted in the red and near-infrared spectral regions, (Dept. Chem. , George Washington Univ., Washington, DC 20052, USA). 87/C1429. Meyer, G. A., Air ICP analytical spectrometry, (Dow Chemical Company Analytical Labs, 1602 Bldg., Midland, MI 48674, USA). 8711430.87/1431. 87/ 1 43 2. 87/1433. 87/1434. 8711435. 871 87/ 871 871 436. 437. 438. 439. 8711440. 8711441. 87/1442. Taylor, A., Usefulness of measurements of trace elements in hair, Ann. Clin. Biochem., 1986, 23, 364. (Supra- Regional Trace Element Laboratory, Robens Inst. of Indust. and Environ. Health and Safety, Univ. Surrey, Guildford, Surrey GU2 5XH, UK). Toyoda, H., Uchida, H., Takahashi, J., Simultaneous multi-element analysis of human hair by ICP-AES, Bun- seki Kagaku, 1986,35, T.80. (Japan Med. Prev. Syst. Inc., Chiba 271, Japan). Kim, E. P., Kim, Y. S., Studies on atomic absorption spectrophotometric analysis of hexavalent chromium in wastewater by solvent extraction, Taehan Hwahakhoe Chi, 1986,30,423. (Dept. Chem., Korea Univ., Choong- Narn 320, South Korea). Miyazaki, A., Bansho, K., Determination of trace boron in natural waters by inductively coupled plasma emission spectrometry combined with solvent extraction, Anal.Sci., 1986,2,451. (Natl. Res. Inst. Pollut. Resour., Yatabe 305, Japan). Nagourney, S. J., Heit, M., Bogen, D. C., Electrothermal atomic absorption spectroscopic analysis of trace metals in Adirondack Mountain lakes, Spectroscopy (springfield, Oreg.), 1986, 1(11), 41. (Argus Div., Witco Corp., Brooklyn, NY 11231-2193 USA). Kato, K., Application of inductively coupled plasma atomic emission spectrometry to analysis of radioactive materials: a review, At. Spectrosc., 1986, 7 , 129. (Dept. Chem., Japan At. Energy Res. Inst., Tokai 319-11, Japan). Taylor, H. 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ISSN:0267-9477    

DOI:10.1039/JA987020155R

出版商:RSC    

年代:1987

数据来源: RSC

摘要:

166R JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, AUGUST 1987, VOL. 2 Glossary of Abbreviations Whenever suitable, elements may be referred to by their chemical symbols and compounds by their formulae. The following abbreviations are used extensively in the Atomic Spectrometry Updates. a.c. 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 ED-XRF alternating current atomic absorption atomic absorption spectrometry atomic emission atomic emission spectrometry atomic fluorescence atomic fluorescence spectrometry ammonium pyrrolidinedithiocarbamate (ammonium tetramethylenedithio- carbamate) anodic-stripping voltammetry capacitively coupled microwave plasma certified reference material continuous wave direct current d.c.plasma N, N-dimethylformamide deoxyribonucleic acid electrodeless discharge lamp ethylenediaminetetraacetic acid energy dispersive X-ray fluorescence electrothermal atomisation flame AAS flame AES flame AFS flow injection gas chromatography glow discharge lamp hollow-cathode lamp high-frequency 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 WD-XRF 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 radio frequency 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 wavelength dispersive X-ray fluorescence X-ray fluorescence

ISSN:0267-9477    

DOI:10.1039/JA987020166R

出版商:RSC    

年代:1987

数据来源: RSC

摘要:

JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, AUGUST 1987, VOL. 2 417 Atomic Spectrometry Viewpoint Roger Stephens Department of Chemistry, Dalhousie University, Halifax, Nova Scotia B3H 4J3, Canada Professor Roger Stephens is a member of the Atomic Spectrometry Updates Editorial Board and was an invited speaker at the Annual ASU Symposium held in London on 8th April 1987. During the meeting Dr. Neil Barnett (Plymouth Polytechnic) and Dr. Barry Sharp (Macaulay Land Use Research Institute) took the opportunity to interview Professor Stephens. B.S. Would you like to tell us something about the work you did for your PhD at Imperial College? R.S. Briefly, the work involved the devel- opment of a system to operate low-pres- sure flames and to introduce the sample into such systems, which presented a rather tricky problem.However the thing turned out to be an extremely useful training exercise, and gave an introduc- tion to the basics of applied spectroscopy, electronic design, computer program- ming, etc., which proved subsequently to have been invaluable. N.B. Who was your supervisor? R.S. Tom West, and Graham Nickless during my MSc at Bristol before going to Imperial. N.B. Did you employ a number of differ- ent sample introduction techniques with these low-pressure flames? R.S. We started off using a conventional nebuliser, which had to be pretty well blocked off or the aspiration rate was tremendous because of the pressure dif- ferential. That was never terribly satisfac- tory, largely because of the combination of a glass pressure vessel and a flame running inside.The glass got very hot, and if the nebuliser misbehaved water sprayed everywhere. The risk of this thing cracking with an oxyacetylene flame run- ning inside of it filled me with horror, In fact one vessel did crack, luckily without imploding, or even releasing the pressure too fast, but things got quite exciting for a few moments. B.S. I think it filled everyone in the laboratory with horror. Speaking as someone who worked just behind you, I think you did have one or two memorable explosions with it. R.S. There were one or two. You have got to remember that at low pressures the stable burner diameter increases so we are talking about pre-mixed oxyacetylene burning on maybe a one inch diameter burner head, which is OK at low pressure, but if you get it wrong the consequences are rat her cat as trophic.B.S. I seem to remember that the primary reaction zone was about three feet long. R.S. Yes, that was certainly one visual effect! N.B. Did you leave and go to Canada of your own volition, or were you pushed after these temporary excursions into pyrotechnics? B .S. Or did you just decide to get out whilst you were still alive? R.S. Well to be quite honest, I finished in 1971, which was the same year as Fred Alder; other contempories of that period being Malcolm Cresser, Barry [Sharp], Les Ebdon, Terry Risby all working for Tom West, Gordon Kirkbright, Roy Dag- nall or Bernard Fleet. It was quite a productive period. N.B. Often referred to in spectroscopic terms as the golden years at Imperial College, the early to mid-1970s.B . S. It just never seemed like it at the time. N.B. These things are often easier to look back on in retrospect as being golden, because at the time they are just like any other time. R.S. There is no question I think, the combination of that group was beneficial to everyone who was in it. N.B. It was beneficial to the science in general, wouldn’t you say? R.S. True enough; it’s a tremendous experience for anyone who is lucky enough to be part of a team like that one was. B.S. Yes there was friendly competition, and it was great fun. N.B. At that time I was in Australia working as a chemist, but one knew of the work of the groups such as that at Imperial College. How did you find going from such a nucleus to. . ., I cannot think of the term? R.S.The colonies! N.B. Well not quite the colonies! But you went to somewhere where presumably you were the major spectroscopist and you had to set up things. Was that difficult? R.S. Yes. In terms of the availability of the physical plant it was initially very difficult indeed. When I first moved to Dalhousie there was nothing in the way of atomic spectroscopy going on. There wasn’t much money either, and my job was to start a spectroscopy operation. N.B. A familiar story. R.S. You have to sort of pull yourself up by your own boot straps. B.S. What was your prime motivation for going off to Canada rather than staying in the UK? R.S. It was a job. I hadn’t any job opportunities in the UK, lots of rejec- tions though. I thought at the time, well, here is a tremendous opportunity to see another part of the world.I could travel for a few years, come back with a bit of418 JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, AUGUST 1987, VOL. 2 money, set myself up. In fact I found I liked it so much I have stayed there ever since. N.B. That was in 1971. So your group has gone from Roger Stephens on his own, pulling himself up by his boot straps, to what now? What is the state of your group? R.S. The actual history at Dalhousie is quite interesting. It all started with a chap called Doug Ryan, who is an analytical chemist of Tom West's generation, and in the late 1960s early 1970s he foresaw that the time was right to develop a strong analytical group at Dalhousie. He put forward arguments to raise enough money, initially approaching the Pre: sident of the University for permission to go ahead with the scheme and for guaran- tees that the University would support it in the long term.He then went to the National Research Council and said look, there is the possibility of setting up a group here, that is what we might do. The National Research Council at that time felt that there was a need to strengthen analytical chemistry in the country, and they bought the idea. Essentially the money became available initially from the National Research Council to bring in new people, of whom I was one. Gradu- ally these people were absorbed by the University and taken on as faculty mem- bers. So the analytical division has been built up to its present strength really because of the efforts and foresight of Doug Ryan some 15 or 20 years ago.B.S. What is the mix in the group now? R.S. Well, Doug Ryan started out as an organic chemist who began his analytical career during the war years, looking for methods to determine the fission products of uranium. Since then he has pursued various interests, though always keeping a strong foothold in the chemical part of analytical chemistry. Then we have Walter Aue, specialising in GC methods, column coatings, and particularly in the development new detectors; Chatt, a radiochemist who covers activation analy- sis and who has become quite involved with the problems of nuclear waste management; Robert Guy, speciation and model systems; and Lou Ramaley, electrochemistry and computer controlled instrumentation.The facilities available to the group are quite good; we even have a SLOWPOKE nuclear reactor centre whose operations are controlled by Chatt and Ryan. B.S. You haven't had a mini-Chernobyl or anything like that? R.S. No, but we did take the precaution of building it under the Psychology Department! B.S. A wise place, they could do with a little activation. R.S. They did get a bit upset about it. So there is a fair span of interests in the Department. N.B. Your interests are obviously the atomic spectroscopy, but do you have broader interests than that or do you confine yourself basically to atomic spec- troscopy? R.S. My major interests really are concer- ned with finding out the limitations of the apparatus that we are using. For instance, by the time I left Imperial I was all too aware of the highly irritating fact that noise eventually limits the useful gain of a spectrometer, and correspondingly limits the available sensitivity.I went down various roads to follow this up, and eventually formed the opinion that those instrumental artifacts which lead to flicker noise could always be corrected if one was sufficiently ingenious and was prepared to go to enough trouble. That left photon noise, and over the years I have become increasinglv interested in the Question of N.B. From a diagnostic point of view or from an analytical one? R.S. Both. For instance this afternoon one of the things I shall be talking about is the spectroscopic analysis of isotopes. By conventional AA this is really not a very satisfactory thing to do because you wind up using isotopic sources, generally with severe spectral overlaps, and it is difficult to deconvolute the signals.It turns out that with magneto-rotation many of these difficulties can be resolved and you can carry out isotopic analysis, in principle at least. N.B. L'vov published a paper years ago where he said, as far as he was concerned, there were ten elements that it was possible to do isotopic atomic absorption, and some of those were of course noble gases. Are you saying that the magneto-optic effects will increase this number of ele- ments or just make it easier to do the ten that he has suggested? whether ;hoton noise is a findamental R.S. The one that I have concentrated on llmlt on any measurement system which is lead, and so far as I'm aware no-one has involves extracting information from tried to do that one by AA at all at light, Or whether it is merely f~~damental atmospheric pressure.Magneto-rotation to the types of spectrometer systems we allows this to be done, better yet with an use at the 11-10ment. The Pursuit of that ordinary hollow-cathode source. The question has Played a big Part in shaping three natural isotopes show up quite the direction of my research. It even clearly, and with clearly distinct response begins to look as if the question may have curves. So I think there is a lot of potential an answer! there. You don't have the same levels of sensitivity you would have if you were just looking for lead, the reason being you are with spectroscopy as a measurement not simply looking for a signal; you are science as well as its analytical application. looking for information on that signal worked a lot On the mag- and you have to have a correspondingl; netic atomic spectroscopic techniques and, higher signal to noise ratio.so it will Zeeman AA magneto-rotation is used only as a method machines. But there are a whole variety of of detection, However, it is an option about at the to present capabilities. Whether it will curiosities or do you think any of them will techniques, for example, remains to be application? it is also more finicky to calibrate, and will N . B. Because when we listen to John probably never have the same sensitivity. Dawson, one is tempted very much to start arguing for coherent forward scattering in N.B* With the advent O f the many new all possible ways and forms.B~~ no one is techniques we are talking about in the Asu doing it. Mind you it has taken a very long reviews, things like Fourier transform the effect has been known for a long while. how these may magneto-optic rota- tion. With FT you get vastly improved have been very much have One Of these has ' O w become commer- never be as sensitive a technique as when with the advent Others, Some Of which You are going to which J think may offer a useful extension remaining as lab actually successfully compete with MS ever come through for routine analytical seen. Although it could be a lot cheaper, Symposium today* You see them time to get a Zeeman instrument, although sPectroscoPY 7 One wonders R.S. Zeeman correction was first sugges- resolution; is this going to help the isotopic ted in 1969, by Pearl and Parker if iSSUe, because YOU Can ?YleaSUre the iS0- memory serves.Yes, I believe coherent topic shifts in the hyperfine structure, With forward scattering has a tremendous FT- UVfor example which has been deve- future but then I am biased. loped in the UK. B.S. so it will be the year 2000 before R.S. Again with non-magnetic techniques coherent scattering will become the problem is in the atomiser itself. If you are using a conventional atmospheric commercially available. atomiser pressure broadening is quite R.S. Remember though-that technique enough for the majority of elements to can do things which I think nothing else cause more or less severe overlap of the can touch.isotopic lines.JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, AUGUST 1987, VOL. 2 419 N.B. So you are saying you have to go back to low pressure to get rid of some of this broadening, to increase the resolution? R.S. If you are relying on a technique that has to separate the resonance lines, you may have no choice but to go to low pressure. Magneto-rotation can work by sensing changes in the line profile, so if you have two overlapping lines you still have the distorted line profile coming through even in a mixture. N.B. With FT spectrometry you can measure very accurately the line profile, all of the lines, all of the time, that is the point I was making. I don’t know whether that would make any advancement in magneto- rotation. R.S. It is certainly a reasonable sugges- tion. There might be problems with the signal to noise ratio if additional strong emission lines were present apart from those of isotopic interest.N.B. Once again, if we are talking about costs, it is expensive, B .S. Do you detect differences between the way research is carried out in academic institutions in the UK and in Canada? We have had some comments on this before in JAAS in the interview with Gary Hieftje, who compared the differences in funding. R.S. Yes there certainly are differences in funding. I am personally responsible for almost everything required for my research, from solder and hook-up wire through to a good part of graduate students stipends, but at the same time it gives me a lot of freedom in how the money is spent.I can choose to put it into apparatus, if it suddenly seems necessary to open a new research area, or into stipends if some good students suddenly appear, or PDFs, or whatever mix seems appropriate. This allows a very quick and flexible response to be made as circum- stances change. It is a very nice system I think, in that it gives you responsibility for your own performance as it were. You stand or fall by how effectively, and imaginatively, the money is used. There are other types of grants and awards of course whose uses are much more rigidly defined, but the operating grants I have been talking about, and their flexibility, are a cornerstone of NSERC’s present policy. B.S. Do you think it is a lot more competitive? R.S. It is competitive in that I have a feeling the tenure decisions are probably more savage over there in the end.B.S. So to surmount the tenure barrier you have really got to prove your worth at that early stage? R.S. Pretty much. We have something like a 50% success rate in obtaining tenure. I am not sure what a comparable figure would be in the UK. B.S. Where do most of your funds come from? Do they come in from industry, do you have to go out and compete for them, do they come from the equivalent of our Science and Engineering Research Coun- cil, or does the University itselfprovide the bulk of them? R.S. Industry first. By and large our local industries are not too bothered about higher education. We are talking of tim- ber, pulp and paper, fishing, tourism in the summer. They don’t have much need for our research, and it is difficult to convince them (or our politicians!) that research is important, not only for the long-term health of the country, but also for support of undergraduate education. So most of my money comes from the Natural Sciences and Engineering Research Council. Some direct support comes from the University, mainly in the form of graduate funding.N.B. It is interesting to hear your break- down of funds, the fact that you are in control as it were from the burettes upwards, who spends what, who goes where, whereas in this country we get a grant, and it will be for a project, some of which will be for travel. However, we cannot shift the money around. I think that makes a great deal of difference, and as you say, if you want to have a lot of students, fine, or if perhaps you want one or two good ones and some more kit, or a larger piece of equipment then the flexibil- ity would make a great deal of difference.We find in the UK, I am sure Barry will agree with me, that the Government fun- ded institutes often have equipment but no people to run them. Certainly in the Polytechnics we can get people, but getting money for equipment is the problem because we can get grants for studentships (in Polytechnics) from the Local Author- ity, but it is pointless having a student with only test-tubes, as these days we are dealing with instrumental advances that cost money. B.S. Your system of total funding appears to be similar to that in the USA. I have always felt that it does give you a lot more flexibility.The grants awarded seem astro- nomical in UK terms but they have to pay for absolutely everything including the typist. However, the emphasis can be changed to suit current requirements. N.B. Can I ask you about the association with ARAAS and now ASU, and when it started? R.S. It started off with a suggestion by John Dawson, about three years ago. N.B. In many cases it is preaching to the converted about things I am going to say, but how do you think the journal goes down in its present format compared with the ARAAS format in North America? R.S. Certainly in Dalhousie it was received very enthusiastically. Just to give you an example, at the moment our library budget is frozen, but at the same time they are having to face the problem of the spiralling increases in journal subscriptions, in effect cutting back on coverage.When the first issue of JAAS came out I showed it to my colleagues, who were enthusiastic enough to help squeeze enough money out of the budget to take it on as a new subscription, in spite of the cut-backs in other areas. I think that shows how the journal is regarded. N.B. It does and we are obviously very pleased with the way the journal has gone. It is a credit to people like Barry and the late John Ottaway that they came up with the idea. R.S. I think you had a good foundation to begin with. B.S. Yes the book had given us the experience of how to do it, but we had to relearn how slightly in order to change from producing an annual book into a bimonthly journal. I think in getting JAAS, with the ASU content, off the ground we were lucky in the sense that the community of analytical atomic spectro- scopists in the UK is very close knit.It is a small country so we meet each other often and we were in a unique position therefore to call on lots of people to give their time freely to make it work. It had a very strong home constituency. I suspect that there aren’t many other places where it would have been possible to get that degree of co-operation. R.S. Certainly not in Canada as people are geographically spaced much wider. N.B. Do you have a similar professional association? We are all within the Royal Society of Chemistry, Do you have an analytical division of Canadian Chemical Society? R.S. It is nothing like as strong as over here. Part of the problem is that of geographical isolation, it being such an enormous country.The Canadian Insti- tute of Chemistry does have an annual meeting, This year it happens to be in Quebec City, which isn’t too far away. If it was in, say, Saskatoon, that would be almost as far as to come over here. That really is a very difficult barrier to over- come. B .S. My fond memories of you at Imperial College were as a squash partner who hit420 JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, AUGUST 1987, VOL. 2 anything that moved including me, and as a driver of exotic cars, such as Triumph roadsters. Have you managed to export some of these aspects of English life to the co Lon ies ? R.S. Right now I drive a Renault, which is a much more practical vehicle, given our winter climate, than any sports car.And I gave up squash as old age began to catch up with me. I don’t know that one should be too keen to export too many traditions to a new country, though I must confess to feeling much more comfortable with English influences than those of the USA. N.B. Further to our discussion about the Canadian Chemical Society, one doesn’t tend to hear much about it, which perhaps emphasises your point that they are not quite as strong as perhaps the RSC. The thing we do hear about is the NRCC, which almost seems to represent Canadian Chemistry. We hear a lot about people from the National Research Council of Canada, and for example, people from there appear to be organising this year’s CSI. They seem to be a very strong body. R.S. Yes the NRC labs have a very good reputation, and have an excellent group of staff.N.B. Do you think there is a time limit for groups such as these or not? It would seem that Imperial College had that wonderful time, but Tom West went to the Macaulay and Gordon Kirkbright went to Manches- ter. Things seem to have a finite length of time. R.S. That is exactly right. Nothing is written in tablets of stone. Such groups provide an inspiration to the people connected with them, but it’s a two way street. The individuals must generate vitality for the group as a whole, and must in turn receive some external support for their efforts. Often it is one individual who acts as a focus for both these aspects and when that individual moves away, or encounters sufficient opposition, the group dies back. B.S. You need the right combination of people for a start, that is what it boils down to. But then the circumstances have to be right and if the two come together and there is some money around things begin to happen. However, situations change and the right “chemistry” occurs somewhere else and other groups become the torch bearers. Thank you for spending some time remembering the past and discussing the future for magneto-rotation. It was cer- tainly good to see you again in the UK and we wish you well for the rest of your trip. Edited by L. Bretherick Safety Consultant Society of Chemistry, Mem London WClB SDT, UK. Non to: The Royal Society of Che Road, Letchworth, Herts SG6 Hazards in the Chemical Laborat06 has become established as an essential handbook of safety practices, measures and toxic effects for laboratories handling dangerous chemicals. Since the last edition was published in 1981 there have been many changes in legislation, regulations, precautionary safety methods and toxicity assessments which warrant publication of this new 4th edition. In addition coverage has been expanded to include material relating to legislation and safety practices in the USA. Protective PVC Binding 618pp Price €2950 ($54.00) ISBN 0 85186 489 9 RSC Members Price €18.00 ORDERING RSC Members should send their orders to: The Royal /A. ROYAL

ISSN:0267-9477    

DOI:10.1039/JA9870200417

出版商:RSC    

年代:1987

数据来源: RSC

摘要:

JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, AUGUST 1987, VOL. 2 421 Conference Reports 1986 Eastern Analytical Symposium: October 19th=24th, 1986, New York, USA (plus details of the 1987 programme) This report will discuss the 1986 and 1987 Eastern Analytical Symposia (EAS) with respect to papers presented in the general area of atomic spectrometry. The 1986 meeting was held in New York City from October 19th through 24th and was unique in several important ways. Firstly, it was the 25th “Silver Jubilee” meeting; secondly, it was the first meeting held in the New York City Hilton Hotel, a vastly improved physical location as compared with previous meeting sites and; thirdly, it was the first full five-day meeting in EAS history. Previous meetings had been three- or, more recently, four-day meet- ings.An important symposium at the 1986 EAS was “Laser excitation in analytical spectroscopy” organised and chaired by J. D. Winefordner (Florida) with an introductory talk by Winefordner, a dis- cussion of laser induced ionisation spec- troscopy of small biological precursors in supersonic beam mass spectrometry by Lubman (Michigan), laser excited AFS by Michel (Connecticut), laser induced molecular fluorescence by Sepaniak (Tennessee) and a concluding paper by Ramsey (Oak Ridge) on analytical appli- cations of non-linear optics including phase conjugation. Browner (Georgia Tech) organised an interesting sympo- sium on the important problem of sample introduction in AES. He opened the symposium with a talk on the problems and this was followed by a discussion of advanced nebulisation techniques by Bonner Denton (Arizona), chromato- graphic sample introduction with plasma emission detection by Caruso (Cincin- nati) and a survey of solid-sample intro- duction for ICP-AES by Routh (ARL).Hieftje (Indiana) organised and chaired an ICP-MS symposium that began with a philosophical paper by Horlick (Alberta) followed by a talk on applica- tions of ICP-MS to biological and envi- ronmental samples by Barnes (Massa- chusetts). Douglas (Sciex) discussed sam- pling ions from the ICP for quadrupole MS and Hieftje concluded the session with a description of his laboratory-built ICP-MS system that allowed optical scan- ning of the ICP while performing the MS. Zander (Perkin-Elmer) organised a ses- sion on current events in AAS that began with a keynote address by Slavin (Perkin- Elmer) on state-of-the-art graphite fur- nace AAS.Hadeishi (Lawrence Berkeley Laboratory) described a simultaneous, multi-element, Zeeman AAS utilising phase sensitive detection and encoding techniques, and de Loos-Vollebregt and de Galan (Delft, The Netherlands) com- mented on the possibilities of totally pyrolytic graphite as a tube material in electrothermal atomisation AAS. Monnig and Hieftje (Indiana) described coherent forward scattering as a possible alterna- tive to AAS. Finally, Holcombe (Texas) presented some additional chemical infor- mation from time and spatial data from graphite furnace AAS. Keliher (Villanova) organised and Barnes (Massachusetts) chaired a sympo- sium on recent advances in plasma emis- sion spectrometry.Ebdon (Plymouth) discussed solid-sample analysis by slurry atomisation and Griffin (Texas Instru- ments) used a DCP technique for ultra- trace metal determination in effluent waters. Brenner (Geological Survey of Israel) critically evaluated internal refer- ences and high-resolution spectrometers for refractory metallurgical materials and Montaser (George Washington Univer- sity) discussed potentials and limitations of helium ICPs. Routh (ARL) concluded the session with a report on practical ICP - Fourier transform spectrometry. In addi- tion to the above mentioned symposia, there were many submitted papers dis- cussing atomic spectroscopic techniques. For 1987, the meeting will again be held at the New York City Hilton and the 1987 dates are September 13th through 18th.A most important symposium will be held honouring Velmer A. Fassel (Iowa State), the 1987 recipient of the newly established EAS award. Professor Fassel will present his award address entitled “Successful New Analytical Techniques: What are the Magical Ingredients?” In addition, Xi-en Shen (Shanghai Institute of Ceramics) will report on the utility of ICP-AES in the analysis of ceramics and related materials and Zander (Perkin- Elmer) will compare performances of various inert gas plasma excitation sources, Browner (Georgia Tech) will report on sample introduction problems in the ICP and Barnes (Massachusetts) will present a somewhat philosophical talk entitled “ICP-AES, What Comes Next?” Qinhan Jin (Jilin University, China) will describe the development of a microwave plasma ionisation detector for GC and Houk (Iowa State) will report on recent sampling experiments for ICP- AES and ICP-MS.Finally, Routh will report on recent developments in ICP- FT. Krull (Northeastern) has organised a symposium on trace metal speciation with talks on interfacing by Uden (Massa- chusetts), Caruso (Cincinnati), Irgolic (Texas A & M) and Houk (Iowa State). In addition, Bonner Denton (Arizona) will discuss the future of intelligent spec- trometers in chemical analysis. Michel (Connecticut) has organised a symposium on lasers with papers by himself on laser excited AFS in graphite furnaces, Lub- man (Michigan) on pulsed laser desorp- tion and Yeung (Iowa State) on combin- ing laser spectroscopy and chromato- graphy in chemical analysis.Finally, Bial- kowski (Utah State) will describe real time correlation filters applied to pulsed laser excited photothermal spectroscopy. Montaser (George Washington Univer- sity) has organised a symposium on AFS with ICPs and furnaces that opens with a discussion of pulsed lasers and hollow- cathode source AFS in the ICP by Wine- fordner (Florida) and continues with a comparison of excitation sources and sample introduction for HCL excited ICP-AES by Demers (Baird). Zhu (Vil- lanova) will be describing the effects of various organic solvents on signal-to- noise and detection limits on an ICP-AFS system, Montaser (George Washington University) will describe diagnostic stu- dies of ICP discharges in AFS and Michel (Connecticut) a background correction system for AFS.In addition to the above mentioned symposia, there are many submitted papers on atomic spectroscopy for the 1987 EAS meeting as well as an important keynote lecture by Brenner (Geological Survey of Israel) describing analytical performance of glow discharge, conventional ICP and spark ablation - ICP atomic emission spectrometers for analysis of geological and related materials. The EAS continues to be an important meeting in many areas includ- ing atomic spectroscopy. Peter N. Keliher Villanova University, Villanova, PA, USA422 JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, AUGUST 1987, VOL. 2 Anwendertreffen: Plasmaspektrometrie: March 26th and 27th, 1987, Dortmund, FRG A meeting of users and manufacturers of plasma emission spectrometric in- strumentation was held at the Institut fur Spektrochemie und angewandte Spek- troskopie in Dortmund on March 26th and 27th in cooperation with the “Deutsche Arbeitskreis fur Angewandte Spektroskopie.” Eighty-seven partici- pants from Germany, Austria, Switzer- land and The Netherlands gave short presentations and took part in lively discussions covering current topics in ICP, DCP, CMP and MIP optical emission spectrometry as well as in ICP mass spectrometry.Dr. Boumans gave an introductory talk on figures of merit in ICP spectrometry and reported on the latest results of work on interferences at Philips Research Lab- oratories. A series of contributions dealt with achievements in sample introduction for ICP spectrometry.The performance of various commercially available pneu- matic nebulisers, such as cross-flow, CGN, and also Babington types, was discussed. Work with organic solvents was covered and practical aids for such things as tubing and optimisation led to lively discussions. The possibilities of using the carbon rod atomiser from PS Analytical in combination with ICP spec- trometry were presented. An interesting report on work in agro-chemical labora- tories highlighted the particular problems of ICP-OES for plant nutrient studies and for residue analysis. Further contribu- tions dealt with sampling and automatic dilution with commercial equipment, on- and off-line background correction and the low-consumption ICP as well as an kchelle - ICP system. Another contribu- tion concentrated on the risks of system- atic errors which may arise from the use of software-controlled data treatment.The latter was also discussed in a presentation on correction for drift offered in commer- cial software packages. In addition, preci- sion measurements for noble metals were reported. Dr. Ohls presented data on a comparison study carried out by a work- ing group on ICP-OES in the “Verein Deutscher Eisenhuttenleute” (VDEh). The results of a study on low- and high-alloy steels showed that ICP-OES and AAS can make use of the same sample preparation procedure when deal- ing with a number of problems in a steel analysis laboratory. A recommendation resulting from this work will be adopted in the “Handbuch fur das Eisenhiittenlabor- atorium.” A further contribution dealt with problems encountered in the analysis of ceramics; in particular grinding and the contamination involved were impres- sively dealt with.This suggests that increased research efforts are required, because of the importance of ceramics as new working materials. In connection with these themes, methods for the direct analysis of non-conducting powders, such as direct sample insertion into the ICP for volatile elements, spark ablation after mixing with copper and briquetting into pellets and particularly slurry atomisa- tion, were discussed. Also, the need for systematic work on laser ablation for bulk and micro-distribution analyses in non- conducting solids was clearly demon- strated. A presentation on DCP-OES showed how problems in the analysis of refractory metals such as tungsten can be readily solved with this technique. The discussion showed that good compromise conditions for a DCP - kchelle spectrometer are not easy to realise.Therefore, the high re- solving power of the system enabled freedom of interferences in many of the examples studied. Contributions on MIP- OES concentrated on the coupling of the Beenakker-type MIP with gas and liquid chromatography. Of special interest was the use of a compact filter photometer, which even enabled background correc- tion. By coupling three such units with suitable light-guides three elements could be detected simultaneously and on-line with the gas chromatograph. A further MIP contribution dealt with the determi- nation of chlorine in liquids of low volatil- ity by HPLC - MIP-OES.Figures of merit of ICP mass spec- trometry were treated in a joint contribu- tion. In particular, the interferences and how they have to be dealt with for real samples, such as geological standards, were discussed. The capabilities of laser ablation for direct solids sampling were given using metal analyses as an example. The use of ICP-MS in the aluminium indvstry was discussed. The technique was shown to be an impressive, powerful tool for the characterisation of standard samples of various alloys as well as of high-purity aluminium. An additional contribution dealt with the use of ICP-MS for the analysis of waste water. Relevant interferences in water analysis were treated and the accuracy for ultratrace determinations in water samples also demonstrated.It could be concluded that as ICP mass spectrometry becomes more widely used the number of instruments in Germany will be expected to grow. This “Anwendertreffen” was the fourth held in Dortmund. The fact that all manufacturers offering equipment for plasma spectrometry on the German mar- ket participated and that many users accepted our invitation to come to Dort- mund, has encouraged us to organise another meeting of this kind in two years time. J. A. C . Broekaert Institut fur Spektrochemie und angewandte Spektroskopie, Dortmund, FRG 12th Norwegian Workshop on Atomic Spectroscopy: April 6th-8th, 1987, Raros, Norway The 12th Norwegian workshop on atomic spectroscopy was arranged by the Divi- sion of Analytical Chemistry of the Nor- wegian Chemical Society, April 6th-8th, 1987.The venue was Roros Turisthotell, which is situated in the outskirts of the old copper-mining town of Rmos. The programme contained the tradi- tional mixture of plenary lectures by invited speakers, short lectures, posters and an instrument exhibition. The invited speakers this year were: Professor Les Ebdon, Plymouth Poly- technic, UK (Slurry atomisation in plasma spectroscopy, and Combined atomic absorption spectroscopy and chro- matography for metal speciation); Dr. Olle Lindsjg, Outokumpu oy, Finland (Third generation instruments for atomic absorption spectroscopy); Dr. Walter Lund, Department of Chemistry, Univer- sity of Oslo, Norway (Sampling and sample preparation, a neglected science?); and Dr. Kire Julshamn, Insti- tute of Nutrition, Directorate of Fisheries, Bergen, Norway (Problems adhering to trace element analysis of samples of marine origin). About 80 people attended the workshop. F. J. Langmyhr University of Oslo, Oslo, NorwayJOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, AUGUST 1987, VOL. 2 423 L to R: Dr. G. Lundgren, Professor L. Ebdon and Mr. S. Omang L to R: Dr. W. Lund, Professor F. Langmyhr and Dr. R. Bye Photographs by courtesy of Dr. 0. Lindsjei Postscript sun growing daily stronger. The organ- the early hours of the morning, with A notably friendly atmosphere per- isers, ably led by Dr. Ragnor Bye, are to especial interest being shown in the rneated the meeting, helped doubtless by be congratulated on a meeting which once the first signs of the Norwegian spring in again brought together practitioners from the mountain town of Roros. The gently the analytical laboratory with leading melting snow, a memorial to a hard winter researchers and instrument manufactur- even by Roros’ standards, glistened in a ers. Discussions often continued on into capabilities of ICP-AESand the prospects for ICP-MS, as well as of course the success of JAAS. Les Ebdon Plymouth Polytechnic, Uk

ISSN:0267-9477    

DOI:10.1039/JA9870200421

出版商:RSC    

年代:1987

数据来源: RSC

摘要:

JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, AUGUST 1987, VOL. 2 423 Book Review Analytical Applications of Lasers. Edited by Edward H. Piepmeier. Chemical Analysis, Volume 87. Pp. xvi + 703. Wiley-Interscience. 1986. Price f85.95. Twenty-two well known scientists from all over the world contributed to this addi- tion to the established Wiley series on Chemical Analysis. This new and inter- esting book is on an area of science that is developing strongly. The contents are organised into six parts: Introduction; Selected Methods that Use Various Detection Schemes; Methods with Improved Spectral Resolu- tion; Selected Multi-photon and Multi- wavelength Methods; Methods Based on Special Characteristics of Lasers; and Lasers with Other Methods. These six parts contain 19 chapters altogether.The Editor prepared the Introduction on the basic principles of lasers. This chapter gives an excellent readily under- standable survey on the theoretical aspects of lasers and the apparatus used. However some of the examples used could be better explained, e.g., the exact energy levels. ISBN 0-471-87023-4 Part I1 contains five chapters on: Laser- excited atomic and ionic fluorescence (LEAFS); Laser enhanced ionisation (LEI); Detection of small numbers of atoms and molecules; Optoacoustic spec- troscopy; and Infrared absorption spec- troscopy. Winefordner and Omenetto, the best known scientists in this field, contributed an informed and realistic critical section on LEAFS, with numerous diagrams, schemes and tables and 239 references. This gives an excellent account of the state-of-the-art and for the future of this most sensitive method of analytical atomic spectrometry in the field of inorganic analysis. It may even be that the future is even more optimistic as examples of extreme trace analysis are increasingly being reported.Green repor- ted on the use of LEI in organic analysis. The content of this chapter gives precise and up-to-date information about this new technique. The main advantages of this method are that it is easy to distinguish between the signal being detected and the optical excitation, there are no stray light effects and its simplicity. These advan- tages are, without any doubt, the basis for further development of this optogalvanic procedure. Sixty-two references support this progressive opinion. The more theoretical aspects rather than the practical analytical methodology is described by Alkemade, one of the senior researchers in the field, in Chapter 4, which is on the detection of small numbers of atoms and molecules, par- ticularly single atom detection.This chapter is very impressive, because it shows from a theoretical and practical point of view what is actually possible with “laser” techniques. Particularly, the recommendations of this author for spec- troanalytical chemists are a valuable guide for the future. The importance of the chapter is underlined with 121 refer- ences. The chapter on optoacoustic spec- trometry, written by Tam, is short. The theoretical part is informative and detailed but there are too few analytical examples (92 references). The chapter on IR absorption spec- trometry written by Yeung is also short, but there is some interesting information on new laser types (wave mixing, diode424 JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, AUGUST 1987, VOL.2 lasers, spin-flip Raman laser, etc.). In accordance with the practicality of this method, some experimental techniques are briefly described (long-path absorp- tion, modulation spectroscopy, etc.); 54 references are included. Part I11 contains two chapters: Cryogenic molecular fluorescence spec- trometry (by Wehry) and Linear and non-linear site-selective laser spectro- scopy (by Wright et d). The major developments in laser-excited molecular fluorescence based on the Shpolski- effect is the main subject of the first chapter.Numerous analytical applica- tions are described and it is concluded that other methods of transition-energy selection will arise with improvements in lasers and decreasing costs of the instrumentation (209 references). The chapter on site-selective spectroscopy is much more theoretical (26 references), but shows that complex compounds, REEs, proteins etc. can be studied. Part IV also contains two chapters: Two-photon excited fluorescence (by Kostulo and Wirth) and Raman related methods in chemical analysis (by Yeung). The first stages of two-photon excitation for qualitative and quantitative analysis of organics are described (27 references). In accordance with its importance, the chapter on Raman spectroscopy is long, with conventional Raman spectroscopy, Raman remote sensing, inverse Raman scattering, Kerr-effect spectroscopy, photoacoustic Raman spectroscopy, coherent anti-Stoke’s Raman spectro- scopy, resonance Raman, Raman spectro- electrochemistry being descirbed from theoretical and practical points of view (130 references).Six chapters on different topics are included in Part V. Remote sensing with lasers, written by Measures, is an interest- ing area from the theoretical and particu- larly from the practical point of view in environmental sciences. The author shows that it is possible to determine both major and minor constituents and to measure thermal properties of the atmo- sphere by absorption and scattering processes using lasers; 190 references underline the importance of this field. The Editor contributed the next chapter on Intracavity-enhanced spec- troscopy.This gives rise to the possibility of measuring very small absorption coeffi- cients. In spite of the fact that the method is still in its early stages of development, it is evident that this technique could be the most sensitive of all (52 references). Harris describes the thermal lens effect, which is also a new technique for trace analysis. Because the lens is only a semi- selective detector, combinations with chromatography and FIA are specifically mentioned (56 references). Wirth and Blanchard present informa- tion on pico-second spectroscopy (21 references). Ware describes electro- phoretic light scattering with a brief dis- cussion of the theoretical background and of the applications (43 references).The importance of laser flow cytometry for biological, biochemical and medical research is described by Hein and Thomas, where single cells can be detec- ted in flow streams. An area where this technique could be of interest in the future should be in colloid chemistry (131 references). The last part contains three chapters on areas where lasers have been combined with other techniques. Yeung describes the application of lasers as detectors in chromatography. Because many of the principles of lasers in other areas can also be applied to chromatography much of this chapter repeats what has already been described in earlier chapters (26 refer- ences). The last two chapters discuss the use of lasers for the generation of ions for mass spectrometry (written by Houk) and for the generation of atoms and ions from solids (laser ablation) for atomic spectro- scopy (written by the Editor). The analy- sis of solids by laser desorption is des- cribed by Houk, who underlines the practical use of this very expensive tech- nique with 174 references. In the last chapter the Editor tries to deal with the wide area of laser ablation for direct solid analysis.He combines some theoretical proposals with a summary of applications. Because this is one of the oldest fields of application of lasers in analytical chem- istry there are many references (177). Summarising, it can be concluded that the book will be of interest to specialists and as well as non-specialists and students. Of course it is always a problem to produce a work with contributions from many authors, because this can lead to inhomogeneity and repetitions cannot be avoided. Another critical note is the literature. There are obviously a large number of references, but the most recent ones cited are from 1982-1983. A parti- cular example is the last chapter on laser ablation, where from 177 references only seven are from the 1980s (three being by the author). For such a strongly developing field of analytical chemistry, if the 22 authors could have worked in parallel the up-to- date character of the book would have been improved. However, this note does not diminish the value of the book too severely, so it is highly recommended for reading and studying. Klaus Dittrich Karl- Marx- Universitat, Leipzig, GDR

ISSN:0267-9477    

DOI:10.1039/JA9870200423

出版商:RSC    

年代:1987

数据来源: RSC