摘要:

J ou r n a I of Ana I yt ica I Atomic Spectrometry (Including Atomic Spectrometry Updates - Formerly ARAAS) JAAS Editorial Board* Chairman: L. C. Ebdon (Plymouth, UK) J. Brew (London, UK) M. S. Cresser (Aberdeen, UK) D. L. Miles (Wallingford, UK) B. L. Sharp (Aberdeen, UK) M. Thompson (London, UK) A. M. Ure (Aberdeen, UK) *The JAAS Editorial Board reports t o the Analytical Editorial Board, Chairman J. D. R. Thomas (Cardiff, UK) JAAS Advisory Board F. C. Adams (Antwerp, Belgium) R. M. Barnes (Amherst, MA, USA) L. Bezur (Budapest, Hungary) R. F. Browner (Atlanta, GA, USA) S. Caroli (Rome, Italy) L. de Galan (Delft, The Netherlands) J. B. Dawson (Leeds, UK) K. Dittrich (Leipzig, GDR) W . Frech (UmeA, Sweden) K. Fuwa (Tokyo, Japan) A. L. Gray (Guildford, UK) F. Greenfield (Loughborough, UK) G.M. Hieftje (Bloomington, IN, USA) G. Horlick (Edmonton, Canada) B. V. L'vov (Leningrad, USSR) J. M. Mermet (Villeurbanne, France) Ni Zhe-ming (Beijing, China) N. Omenetto (Ispra, Italy) E. PlSko (Bratislava, Czechoslovakia) R. E. Sturgeon (Ottawa, Canada) R. Van Grieken (Antwerp, Belgium) A. Walsh,.<K. B. (Victoria, Australia) B. Welz (Uberlingen, FRG) T. S. West (Aberdeen, UK) Atomic Spectrometry Updates Editorial Board Chairman: *M. S. Cresser (Aberdeen, UK) R. M. Barnes (Amherst, MA, USA) N. W. Barnett (Plymouth, UK) *J. Brew (London, UK) *A. A. Brown (Cambridge, UK) J. C. Burridge (Aberdeen, UK) J. B. Dawson (Leeds, UK) J. R. Dean (Norwich, UK) *L. C. Ebdon (Plymouth, UK) H. J. Ellis (Ross-on-Wye, UK) J. Fijalkowski (Warsaw, Poland) D.J. Halls (Glasgow, UK) S. J. Haswell (London, UK) *D. A. Hickman (London, UK) G. M. Hieftje (Bloomington, lN, USA) S. J. Hill (Plymouth, UK) H. Hughes (Anglesey, UK) P. N. Keliher (Villanova, PA, USA) K. Kitagawa (Nagoya, Japan) *D. Littlejohn (Glasgow, UK) K. W. Jackson (Saskatoon, Canada) F. J. M. J. Maessen (Amsterdam, The Nether- lands) *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 Zealandl T. C. Rains (Washington, DC, USA) J. M. Rooke (Leeds, UK) G. Rossi (lspra, Italy) I. RubeSka (Prague, Czechoslovakia) A. Sanz-Medel (Uviedo, 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) *Members of the ASU Executive Committee Editor, JAAS: Judith Brew 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 by 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 €180.00, Rest of World f202.00, USA $356.00. Air freight and mailing in the USA by Publications Expediting Inc., 200 Meacham Avenue, Elmont, NY 11003. USA Postmaster: send address changes t o Journal of Analytical Atomic Spectrometry (JAAS), Publications Expediting Inc., 200 Meacham Avenue, Elmont, NY 11003. Second class postage pending at Jamaica, NY 11431. All other despatches outside the UK by Bulk Airmail within Europe, Accelerated Surface Post outside Europe.PRINTED IN THE UK. @ 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 (ARMS). 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 M S , AES and AFS, papers will be welcomed on atomic mass spectrometry and X-ray fluoresc- encelemission spectrometry. Papers describing the measurement of molecular species where these relate to the characterisation of sources normally used for the production of atoms, or are concerned, for example, with indirect methods of analysis, will also be acceptable for publication.Papers describing the development and applications of hybrid techniques (e.g., GC-coupled AAS and HPLC - ICP) will be parti- cularly welcome. Manuscripts on other subjects of direct interest to atomic spectroscopists, including sample preparation and dissolution and analyte preconcentration procedures, as well as the statistical interpretation and use of atomic spectrometric data will also be accept- able for publication. There is no page charge. The following types of papers will be con- sidered. Full papers, describing original work. Short papers: the criteria for originality are the same as for full papers, but short papers generally report less extensive investigations or are of limited breadth of subject matter.Communications, which must be on an urgent matter and be of obvious scientific i m portance. Corn m u n ications receive priority and are usually published within 2-3 months of receipt, They are intended for brief descriptions of work that has progressed to a stage a t 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 a t least two referees, by whose advice the Editorial Board of JAAS will be guided as to its acceptance or rejection.Papers that are accepted must not be published else. where except by permission. Submission of a manuscript will be regarded as an undertaking that the same material is not being considered for publication by another journal. Manuscripts (three copies typed in double spac- ing) should be addressed to: Judith Brew, Editor, JAAS The Royal Society of Chemistry, Burlington House, Piccadilly, London W1V 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. Brew (London, UK) M. S. Cresser (Aberdeen, UK) D. L. Miles (Wallingford, UK) B. L. Sharp (Aberdeen, UK) M. Thompson (London, UK) A. M. Ure (Aberdeen, UK) *The JAAS Editorial Board reports to the Analytical Editorial Board, Chairman J. D. R. Thomas (Cardiff, UK) JAAS Advisory Board F. C. Adams (Antwerp, Belgium) R.M. Barnes (Amherst, MA, USA) L. Bezur (Budapest, Hungary) R. F. Browner (Atlanta, GA, USA) S. Caroli (Rome, Italy) L. de Galan (Delft, The Netherlands) J. B. Dawson (Leeds, UK) K. Dittrich (Leipzig, GDR) W. Frech (UrneB, Sweden) K. Fuwa (Tokyo, Japan) A. L. Gray (Guildford, UK) S . Greenfield (Loughborough, UK) G. M. Hieftje (Bloomington, IN, USA) G. Horlick (Edmonton, Canada) B. V. L'vov (Leningrad, USSR) J. M. Mermet (Villeurbanne, France) Ni Zhe-ming (Beijing, China) N. Omenetto (lspra, Italy) E. PlSko (Bratislava, Czechoslovakia) R. E. Sturgeon (Ottawa, Canada) R. Van Grieken (Antwerp, Belgium) A. Walsh,.K. B. (Victoria, Australia) B. Welz (Uberlingen, FRG) T. S. West (Aberdeen, UK) Atomic Spectrometry Updates Editorial Board Chairman: "M. S. Cresser (Aberdeen, UK) R.M. Barnes (Amherst, MA, USA) N. W. Barnett (Plymouth, UK) *J. Brew (London, UK) *A. A. Brown (Cambridge, UK) J. C. Burridge (Aberdeen, UK) J. B. Dawson (Leeds, UK) J. R. Dean (Norwich, UK) *L. C. Ebdon (Plymouth, UK) H. J. Ellis (Ross-on-Wye, UK) J. Fijalkowski (Warsaw, Poland) D. J. Halls (Glasgow, UK) S. J. Haswell (London, UK) *D. A. Hickman (London, UK) G. M. Hieftje (Bloomington, IN, USA) S. J. Hill (Plymouth, UK) H. Hughes (Anglesey, UK) P. N. Keliher (Villanova, PA, USA) K. Kitagawa (Nagoya, Japan) *D. Littlejohn (Glasgow, UK) K. W. Jackson (Saskatoon, Canada) F. J. M. J. Maessen (Amsterdam, The Nether- *J. Marshall (Middlesbrough, UK) *D. L. Miles (Wallingford, UK) J. M. Mermet (Villeurbanne, France) E. Norval (Pretoria, South Africa) I. Novotny (Brno, Czechoslovakia) P.E. Paus (Oslo, Norway) P. R. Poole (Hamilton, New Zealand) T. C. Rains (Washington, DC, USA) J. M. Rooke (Leeds, UK) G. Rossi (lspra, Italy) I. RubeSka (Prague, Czechoslovakia) A. Sanz-Medel (Oviedo, Spain) *B. L. Sharp (Aberdeen, UK) W. Slavin (Norwalk, CT, USA) R. Stephens (Halifax, Canada) J. Stupar (Ljubljana, Yugoslavia) A. Taylor (Guildford, UK) M. Thompson (London, UM J. F. Tyson (Loughborough, UK) *A. M. Ure (Aberdeen, UK) B. Welz (Uberlingen, FRG) J. B. Willis (Victoria, Australia) lands) *Members of the ASU Executive Committee Editor, JAAS: Judith Brew The Royal Society of Chemistry, Burlington House, Piccadilly, London W1V OBN, UK. Telephone 01-734 9864. Telex No. 268001 US Associate Editor, JAAS: Dr. J. M. Harnly US Department of Agriculture, Beltsville Human Nutrition Research Center, BLDG 161, BARC-EAST, Beltsville, MD 20705, USA.Telephone 301 -344-2569 Advertisements: Advertisement Department, The Royal Society of Chemistry, Burlington House, Piccadilly, London WIV OBN. Telephone 01-437 8656. Telex No. 268001 Journal ofAnalytical Atomic Spectrometry fJAAS) (ISSN 0267-9477) is published eight times a year by The Royal Society of Chemistry, Burlington House, London WIVOBN, UK. All orders accompanied with payment should be sent directly t o The Royal Society of Chemistry, The Distribution Centre, Blackhorse Road, Letchworth, Herts. SG6 IHN, UK. 1987 Annual subscription rate UK f180.00, Rest of World f202.00, USA $356.00. Air freight and mailing in the USA by Publications Expediting Inc., 200 Meacham Avenue, Elmont, NY 11003.USA Postmaster: send address changes to Journal of Analytical Atomic Spectrometry (JAAS), Publications Expediting Inc., 200 Meacham Avenue, Elmont, NY 11003. Second class postage paid at Jamaica, NY 11431. All other despatches outside the UK by Bulk Airmail within Europe, Accelerated Surface Post outside Europe. PRINTED IN THE UK. 0 The Royal Society of Chemistry, 1987. All rights reserved. No part of this publication may be reproduced, stored in a retrieval system, or transmitted in any form, or by any means, electronic, mechanical, photographic, recording, or otherwise, without the prior permission of the publishers. Information for Authors Full details of how to submit material for publication in JAASare given in the Instructions to Authors in Issue 1.Separate copies are available on request. The Journal of Analytical Atomic Spectrometry (JAAS) is an international journal for the publi- cation of original research papers, short papers, communications and letters concerned with the development and analytical application of atomic spectrometric techniques. The journal is published eight times a year, includes com- prehensive reviews of specific topics of interest to practising atomic spectroscopists and incor- porates the literature reviews which were pre- viously published in Annual Reports on Analy- tical Atomic Spectroscopy (ARAAS). Manuscripts intended for publication must describe original work related to atomic spec- trometric analysis. Papers on all aspects of the subject will be accepted, including fundamental studies, novel instrument developments and practical analytical applications.As well as AAS, AES and AFS, papers will be welcomed on atomic mass spectrometry and X-ray fluoresc- ence/emission spectrometry. Papers describing the measurement of molecular species where these relate to the characterisation of sources normally used for the production of atoms, or are concerned, for example, with indirect methods of analysis, will also be acceptable for publication. Papers describing the development and applications of hybrid techniques (e.g., GC-coupled AAS and HPLC - ICP) will be parti- cularly welcome. Manuscripts on other subjects of direct interest to atomic spectroscopists, including sample preparation and dissolution and analyte preconcentration procedures, as well as the statistical interpretation and use of atomic spectrometric data will also be accept- able for publication.There is no page charge. The following types of papers will be con- sidered. Full papers, describing original work. Short papers: the criteria for originality are the same as for full papers, but short papers generally report less extensive investigations or are of limited breadth of subject matter. Communications, which must be on an urgent matter and be of obvious scientific i m porta nce. Co m m u n icat ions receive priority and are usually published within 2-3 months of receipt. They are intended for brief descriptions of work that has progressed to a stage at which it is likely to be valuable to workers faced with similar problems. Reviews, which must be a critical evaluation of the existing state of knowledge on a parti- cular facet of analytical atomic spectrometry. Every paper (except Communications) will be submitted to at least two referees, by whose advice the Editorial Board of JAAS will be guided as to its acceptance or rejection. Papers that are accepted must not be published else- where except by permission. Submission of a manuscript will be regarded as an undertaking that the same material is not being considered for publication by another journal. Manuscripts (three copies typed in double spac- ing) should be addressed to: Judith Brew, Editor, JAAS The Royal Society of Chemistry, Burlington House, Piccadilly, London WIV OBN, UK Dr. J. M. Harnly US Associate Editor, JAAS US Department of Agriculture, Beltsville Human Nutrition Research Center, BLDG 161, BARC-EAST, Beltsville, MD 20705, USA or All queries relating to the presentation and submission of papers, and any correspondence regarding accepted papers and proofs, should be directed to the Editor or US Editor (addresses as above). Members of the JAASEditorial Board (who may be contacted directly or via the Editorial Office) would welcome comments, suggestions and advice on general policy mat- ters concerning JAAS. Fifty reprints are supplied free of charge.

ISSN:0267-9477    

DOI:10.1039/JA98702FX009

出版商:RSC    

年代:1987

数据来源: RSC

摘要:

JASPE 2(3) 263-342,43R-78R (1 987) April 1987 Journal of Analytical Atomic Spectrometry Including Atomic Spectrometry Updates CONTENTS NEWS AND VIEWS 263 Atomic Spectrometry Viewpoint-Richard F. Browner 264 Conference Reports 267 ASU Highlights-Alistair A. Brown 267 Conferences and Meetings 268 Papers in Future Issues PAPERS 269 277 283 287 293 299 305 31 1 317 32 1 325 329 333 339 Determination of Rare Earth Elements in Geological Samples by Inductively Coupled Plasma Source Mass Spectrometry-Alan R. Date, Dawn Hutchison Determination of Trace Metals in Marine Sediments by Inductively Coupled Plasma Mass Spectrometry-James W. McLaren, Diane Beauchemin, Sheir S. Berman Plasma Potential Measurements for Inductively Coupled Plasma Mass Spectrometry with a Centre-tapped Load CoiCR.S. Houk, Jonathan K. Schoer, Jeffrey S. Crain Determination of Selenium by Graphite Furnace Atomic Absorption Spectrometry. Part 1. Interaction Between Selenium and Carbon-Jiii DBdina, Wolfgang Frech, lngela Lindberg, Erik Lundberg, Anders Cedergren Comparison of Interferences and Matrix Modifiers in the Determination of Gold by Electrothermal Atomisation Atomic Absorption Spectrometry with Zeeman-effect Background Correction-Joseph Egila, David Littlejohn, (the late) John M. Ottaway, Shan Xiao-quan Direct Determination of Gold in Whole Blood and Plasma by Electrothermal Atomisa- tion Atomic Absorption Spectrometry Using Zeeman-effect Background Correction and Matrix Modifications-Shan Xiao-quan, Joseph Egila, David Littlejohn, (the late) John M. Ottaway Direct Determination of Cadmium in Urine by Electrothermal Atomisation Atomic Absorption Spectrometry-David J.Halls, Murdoch M. Black, Gordon S. Fell, (the late) John M. Ottaway Determination of Phosphorus by Graphite Furnace Atomic Absorption Spectrometry. Part 3. Analysis of Biological Reference Materials-Adilson J. Curtius, Gerhard Schlemmer, Bernhard Welz Determination of Copper in Biological Microsamples by Direct Solid Sampling Graphite Furnace Atomic Absorption Spectrometry-Les E bdon, E. HyweI Evans Determination of Trace Amounts of Thorium and Uranium in Coal Ash by Inductively Coupled Plasma Atomic Emission Spectrometry after Extraction with 2-Thenoyltri- fluoroacetone and Back-extraction with Dilute Nitric Acid-Eijiro Kamata, Ryozo N a kas h i ma, M asa m ic h i Fu r u ka wa Direct Atomic Spectrometric Analysis by Slurry Atomisation.Part 3. Whole Coal Analysis by Inductively Coupled Plasma Atomic Emission Spectrometry-Les E bdon, John R. Wilkinson Preparation of Solutions for the Standard Additions Method in Flame Atomic Absorption Spectrometry-Paw& Koscielniak Removal of Phosphate and Silicate Interferences in the Determination of Magnesium, Calcium and Strontium by Atomic Absorption Spectrometry-M. M. El-Defrawy, M. E. Khalifa, A. M. Abdallah, M. A. Akl Determination of Sulphur Compounds by Fully Automated Molecular Emission Cavity Analysis-Nikolaos P. Evmiridis, Alan Townshend ATOMIC SPECTROMETRY UPDATE 43R 69R References Clinical and Biological Materials, Foods and Beverages-Alistair A. Brown, David J.Halls, Andrew TaylorJASPE 2(3) 263-342,43R-78R (1 987) April 1987 Journal of Analytical Atomic Spectrometry Including Atomic Spectrometry Updates CONTENTS NEWS AND VIEWS 263 Atomic Spectrometry Viewpoint-Richard F. Browner 264 Conference Reports 267 ASU Highlights-Alistair A. Brown 267 Conferences and Meetings 268 Papers in Future Issues PAPERS 269 277 283 287 293 299 305 31 1 317 32 1 325 329 333 339 Determination of Rare Earth Elements in Geological Samples by Inductively Coupled Plasma Source Mass Spectrometry-Alan R. Date, Dawn Hutchison Determination of Trace Metals in Marine Sediments by Inductively Coupled Plasma Mass Spectrometry-James W. McLaren, Diane Beauchemin, Sheir S. Berman Plasma Potential Measurements for Inductively Coupled Plasma Mass Spectrometry with a Centre-tapped Load CoiCR.S. Houk, Jonathan K. Schoer, Jeffrey S. Crain Determination of Selenium by Graphite Furnace Atomic Absorption Spectrometry. Part 1. Interaction Between Selenium and Carbon-Jiii DBdina, Wolfgang Frech, lngela Lindberg, Erik Lundberg, Anders Cedergren Comparison of Interferences and Matrix Modifiers in the Determination of Gold by Electrothermal Atomisation Atomic Absorption Spectrometry with Zeeman-effect Background Correction-Joseph Egila, David Littlejohn, (the late) John M. Ottaway, Shan Xiao-quan Direct Determination of Gold in Whole Blood and Plasma by Electrothermal Atomisa- tion Atomic Absorption Spectrometry Using Zeeman-effect Background Correction and Matrix Modifications-Shan Xiao-quan, Joseph Egila, David Littlejohn, (the late) John M.Ottaway Direct Determination of Cadmium in Urine by Electrothermal Atomisation Atomic Absorption Spectrometry-David J. Halls, Murdoch M. Black, Gordon S. Fell, (the late) John M. Ottaway Determination of Phosphorus by Graphite Furnace Atomic Absorption Spectrometry. Part 3. Analysis of Biological Reference Materials-Adilson J. Curtius, Gerhard Schlemmer, Bernhard Welz Determination of Copper in Biological Microsamples by Direct Solid Sampling Graphite Furnace Atomic Absorption Spectrometry-Les E bdon, E. HyweI Evans Determination of Trace Amounts of Thorium and Uranium in Coal Ash by Inductively Coupled Plasma Atomic Emission Spectrometry after Extraction with 2-Thenoyltri- fluoroacetone and Back-extraction with Dilute Nitric Acid-Eijiro Kamata, Ryozo N a kas h i ma, M asa m ic h i Fu r u ka wa Direct Atomic Spectrometric Analysis by Slurry Atomisation. Part 3. Whole Coal Analysis by Inductively Coupled Plasma Atomic Emission Spectrometry-Les E bdon, John R. Wilkinson Preparation of Solutions for the Standard Additions Method in Flame Atomic Absorption Spectrometry-Paw& Koscielniak Removal of Phosphate and Silicate Interferences in the Determination of Magnesium, Calcium and Strontium by Atomic Absorption Spectrometry-M. M. El-Defrawy, M. E. Khalifa, A. M. Abdallah, M. A. Akl Determination of Sulphur Compounds by Fully Automated Molecular Emission Cavity Analysis-Nikolaos P. Evmiridis, Alan Townshend ATOMIC SPECTROMETRY UPDATE 43R 69R References Clinical and Biological Materials, Foods and Beverages-Alistair A. Brown, David J. Halls, Andrew Taylor

ISSN:0267-9477    

DOI:10.1039/JA98702BX011

出版商:RSC    

年代:1987

数据来源: RSC

摘要:

I I I I I I I I I I I I I I I I I I I I I I I I I I I I FOLD HERE I JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY MAR‘87 READER ENQUIRY SERVICE FOLD HERE I I t I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I 1 Postage will be paid by Licensee Do not affix Postage Stamps if posted in Gt. Britain, Channel Islands, N. Ireland or the Isle of Man I I I BUSINESS REPLY SERVICE Licence No. WD 106 Reader Enquiry Service Journal of Analytical Atomic Spectrometry The Royal Society of Chemistry Burlington House, Piccadilly LONDON WIE 6WF England I I I I I I I I 1 I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I 1 I I I I I I I I I I I I I I I I I ! I I I I ! I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I1988 Winter Conference On Plasma Spectrochemis try San Diego, California, USA January 3-9, 1988 The 1988 Winter Conference on Plasma Spectrochemistry, fifth in a series of biennial meetings sponsored by the ZCP Information Newsletter, will feature developments in plasma spectrochemical analysis by inductively coupled plasma (ICP), d.c.plasma (DCP), microwave plasma (MIP) and glow- and hollow-cathode discharge (GDL, HCL) sources. The meeting will convene Monday, January 4 to Saturday, January 9,1988 at the San Diego Princess resort and convention centre in San Diego. Expert short courses at introductory and advanced levels and an exhibition of spectroscopic instrumentation also will be included.Call for Papers and Submission Schedule Papers describing original work with plasma spectrochemical applications, fundamentals and novel instrument development are solicited for presentation in the lecture and poster sessions. Title and 50-word abstracts are due July 2,1987, and for accepted papers, full abstracts are due October 2,1987. Manuscripts for publication in the proceedings are requested by January 9, 1988. ~ ~~~ ~~ Programme and Objectives Symposia organised and chaired by recognised experts will include the following topics: (1) Sample introduction and transport phenomena; (2) Instrumentation and automation, including on-line analysis and remote systems; (3) Excitation mechanisms and plasma characteristics; (4) Interferometry; (5) Atomic fluorescence; (6) Glow and hollow-cathode discharges; (7) Flow injection analysis; (8) Chromatography and plasma detectors; (9) Plasma source mass spectrometry; (10) Industrial applications of ICP mass spectrometry; and (1 1) Sample preparation and pre-concentration techniques.Six plenary and 15 invited lectures will be presented. Three afternoon poster sessions will feature applications, automation and new instrumentation. Four panel discussions will address critical development areas. Plenary, invited and submitted papers will be published as the official conference proceedings following the meeting after peer review in Journal of Analytical Atomic Spectrometry, September 1988 issue. Instrument Exhibition A three day exhibition of spectroscopic instrumentation and chemicals, electronics, glassware, publications and software supporting plasma spectroscopy will complement the scheduled sessions.Expert Short Courses Introductory and advanced four-hour short courses will be offered January 2-3 and 9-10, 1988. Designed to provide background and intensive training in popular topics of plasma spectrochemistry , these will cover analytical applications, instrumentation, sample introduction and various techniques (e.g. , plasma diagnostics, scientific writing chemical and physical pre-concentration and applications of isotope dilution and tracers). Further details on all aspects of the Conference can be obtained from: Dr. Ramon M. Barnes Department of Chemistry, GRC Towers, University of Massachusetts, Amherst, MA 01003-0035, USA (413) 545-2294 ~~ Circle 008 for further information1988 Winter Conference On Plasma Spectrochemis try San Diego, California, USA January 3-9, 1988 The 1988 Winter Conference on Plasma Spectrochemistry, fifth in a series of biennial meetings sponsored by the ZCP Information Newsletter, will feature developments in plasma spectrochemical analysis by inductively coupled plasma (ICP), d.c.plasma (DCP), microwave plasma (MIP) and glow- and hollow-cathode discharge (GDL, HCL) sources. The meeting will convene Monday, January 4 to Saturday, January 9,1988 at the San Diego Princess resort and convention centre in San Diego. Expert short courses at introductory and advanced levels and an exhibition of spectroscopic instrumentation also will be included.Call for Papers and Submission Schedule Papers describing original work with plasma spectrochemical applications, fundamentals and novel instrument development are solicited for presentation in the lecture and poster sessions. Title and 50-word abstracts are due July 2,1987, and for accepted papers, full abstracts are due October 2,1987. Manuscripts for publication in the proceedings are requested by January 9, 1988. ~ ~~~ ~~ Programme and Objectives Symposia organised and chaired by recognised experts will include the following topics: (1) Sample introduction and transport phenomena; (2) Instrumentation and automation, including on-line analysis and remote systems; (3) Excitation mechanisms and plasma characteristics; (4) Interferometry; (5) Atomic fluorescence; (6) Glow and hollow-cathode discharges; (7) Flow injection analysis; (8) Chromatography and plasma detectors; (9) Plasma source mass spectrometry; (10) Industrial applications of ICP mass spectrometry; and (1 1) Sample preparation and pre-concentration techniques.Six plenary and 15 invited lectures will be presented. Three afternoon poster sessions will feature applications, automation and new instrumentation. Four panel discussions will address critical development areas. Plenary, invited and submitted papers will be published as the official conference proceedings following the meeting after peer review in Journal of Analytical Atomic Spectrometry, September 1988 issue. Instrument Exhibition A three day exhibition of spectroscopic instrumentation and chemicals, electronics, glassware, publications and software supporting plasma spectroscopy will complement the scheduled sessions.Expert Short Courses Introductory and advanced four-hour short courses will be offered January 2-3 and 9-10, 1988. Designed to provide background and intensive training in popular topics of plasma spectrochemistry , these will cover analytical applications, instrumentation, sample introduction and various techniques (e.g. , plasma diagnostics, scientific writing chemical and physical pre-concentration and applications of isotope dilution and tracers). Further details on all aspects of the Conference can be obtained from: Dr. Ramon M. Barnes Department of Chemistry, GRC Towers, University of Massachusetts, Amherst, MA 01003-0035, USA (413) 545-2294 ~~ Circle 008 for further informationI andysed my c I I I ARL’s new 3410 ICP spectrometer brings ICP within your reach Now every laboratory involved in solutions elemental analysis can afford to employ the fast, sensitive ICP technique.The new affordable ARL 3410 ICP with MinitorchTM and IBM-PC-XT makes it all possible, and offer these advantages over other systems: lower instrument cost, with ARL’s MinitorchTM; ARL Applied Research Laboratories SA En Vallaire C~-1204 ECUBLENS / Switzerland Tel. (021) 34 97 Austria: (0222) 36 41 52 France: (1) 34 61 94 00 Germany: (021 1) 71 30 06 Spain: (1) 457 50 08 Sweden: (08) 730 o2 95 United Kingdom: (0582) 573 474/9 lower operating costs - lower power usage, lower argon flow give savings of up to 40% over conventional instruments; easier to operate - ARL’s ICP software is spe- cially written for the powerful IBM-PC-XT. The ARL 3410 offers the high performance and flex- ibility of ICP in the most cost-effective package. Can you afford to be without it? ARl APPLIED RESEARCH LABORATORIES Circle 001 for further information

ISSN:0267-9477    

DOI:10.1039/JA98702FP013

出版商:RSC    

年代:1987

数据来源: RSC

摘要:

42 ASU REFERENCE INDEX VOL. 2 (1987) Xu, Yi., 8711226 Xu, Z . , 871.536, 871937 Xue, H . , 871237 Yakimova, N . M., 871970 Yamada, H., 871367 Yamada, K . , 871582. 8711271 Yamada, M., 8711903 Yamamoto, I.. 871244 Yamamoto, M., 871288, 871 1475, 871C 1623 Yamamoto, Y.. 871288, 871 1439 I 871 1475, 87lC 1623 Yamashita, H.. 871372 Yamazaki. H., 871252 Yamazaki. N., 871478 Yamazaki, S.. 8711692 Yan, D., 8711235 Yan, W. Z . , 8711983 Yanagihara, S . , 8712017 Yang, J . , 871273 Yang, L., 87i1449 Yang. M., 871275. 871530 Yang. M. H., 87/303, 871342 Yang, P.. 87lC1375 Yang, X., 87i265, 8711538. Yang, X. D., 8711890 Yang, Y.. 8711214. 8711538 Yang. Z . , 871532 Yao. J., 871524. 8711228 Yao, I,. , 871608 Yao. S., 871276 Yap, C. T., 8716.50 Yasuda. K., 871367 Y asuda, M I , 87lC 1623 Yasui, A ., 8711990 Yatcs, D. A . , 871C555, 87lC1343, 871C1668, 871C 167 1 871C2044 Yates, D. E., 87/88 Yatsenko, L. F.. 8711481 Ybanez, N., 8711240 Ycah, K. S.. 871919 Yeung. E. S . , 871653 Yi, J . , 8711448 Yngstriim. S . . 871287 Yokoi. S . , 8712017 Yokota, F., 8711440 Yonemoto, T., 871437 Yoo, A., 8711501 Yoo. Y. J., 87lC170 Yoon, R.-H.. 871C1630 Yoshida, H., 8711546, 8711547, 8711954 Yoshida, Z . , 871377 Yoshimura, C . , 8711302 Yoshimura, E., 8711692 Yoshimura, K . , 87180 Yoshino, T., 8711582 Yotsuyanagi, T., 8711579 You. S . , 8711226 You, Y . , 871528 Yu. G. X., 8711983 Yu, H.. 871593 Yu, X. Z.. 8711906 Yuan, Z.-N., 871383 Yudclcvich, I. G., 871936, Yurko. R. J . . 87lC558 Zagatto, E. A. G., 871438 Zailaf, M., 8711534 Zakhariya, A. N., 8711901 Zakrevskaya. L.V . . 8711899 Zakrzcwski, Z., 87171 Zalts, A., 87152 Zandcr. A. T., 871123. 871666 Zander. U . , 87lC1000 Zaray, G., 871C1365 871 1482 Zaruba, K., 871C1866 Zauke, G. P., 8711064 Zawadzka, T., 8711315 Zeeman, P. B., 87165 Zclentsova, L. V., 8711482 Zendehnam, A., 871C193 Zeng, X. J.. 8711978, Zhan, G., 87024, 871337, Zhang, C. S.. 8711981 Zhang, €4. U., 8712098 Zhang, J . , 871939 Zhang, J . M., 8711883 Zhang, L.. 871492 Zhang, L. X., 8711981 Zhang, P., 871241 Zhang, Q., 871930 Zhang, S.. 8 7 / 3 3 , 871362, Zhang, W.. 87182 Zhang, X . , 871502 Zhang, Y., 871502, 871526 Zhang, Z . , 871265. 871C2044 Zhang, Z. Y.. 871C2056 Zhao, K. H., 87!1986 Zhao, W.. 8711890 Zhao, X . , 87024 Zhao, Y., 8712081 Zhcbrakov, D. N., 8711270 Zhcn. R. Q., 8711984 Zheng, X..87iC2044 Zhcng, Y., 871585. 8711487, Zhong, X., 871326 Zhong, Y.. 871274, 871485. Zhou. D.. 871453 Zhou. J . , 871243 871C2056 871 1977 871584 87120 13 871 1493 Zhou, M., 871243 Zhou, Y., 871336 Zhou, Z . , 871273, 871607, Zhu. B . . 871237 Zhu, D.. 871241 Zhu, M.. 87/82 Zhu, w., 871937 Zhukova, N. G., 8712012 Zibarova, Yu. F., 871322 Zicai, C., 871633, $71965 Zihlmann, J., 8711893 Zil'bershtein. Kh. I., 87196, Zil'bcrstein, Ch. I.. 87/C1153 Zima, S., 871C1067 Zimmer. K., 871957, 87/C 1095, 871C 1 12 1 Zimmerli, B., 871C1846 Zimmcrmann, R.. 87lC1028 Zizak, G., 871955, 871956 Zoellner. M., 871C816 Zolotarcva, N. I . , 871394 Zolotov, Yu. A . , 871408. 871474, 871977, 8711 190 Zorn. H . , 8711687 Zorov. N. B.. 8711484 Zou, J . , 871943 Zoumboulis. A. I.. 871489 Zumkley.H., 871C1868 Zurera-Cosano, G., 871503 Zwanziger, H., 871C1001 Zybin. A. V., 871126. 871260, 871C 1 122. 871 1548 Zyrnicki. W., 871C1054, 871C 1057 871938 871327 Typeset and printed by Black Bear Press Limited, Cambridge, EnglandSECOND SURREY CONFERENCE ON PLASMA SOURCE MASS SPECTROMETRY University of Surrey, Guildford, Surrey, UK 6th-8th July, 1987 The second Surrey Conference will be devoted solely to ICP Source Mass Spectrometry. The conference will include invited and contributed papers, a workshop and a short course. It is intended that papers presented will be published in an issue of JAAS, along with those from the Post-CSI symposium on ICP-MS, after the normal peer review procedure. Further information from: Dr. A. L. 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ISSN:0267-9477    

DOI:10.1039/JA98702BP017

出版商:RSC    

年代:1987

数据来源: RSC

摘要:

JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, APRIL 1987, VOL. 2 43R ATOMIC SPECTROMETRY UPDATE-CLINICAL AND BIOLOGICAL MATERIALS, FOODS AND BEVERAGES Alistair A. Brown* Pye Unicam Ltd., York Street, Cambridge CBI 2PX, UK David J. Halls Trace Metals Unit, Department of Biochemistry, Ro yai Infirmary, Castle Street, Glasgow G4 OSF, UK Andrew Taylor Supra-Regional Assay Service Metals Reference Laboratory, Robens Institute of Industrial and Environmental Health and Safety, University of Surrey, Guildford, Surrey GU2 5XH, UK Summary of Contents 1 Analysis of Clinical and Biological Materials 1.1. 1.2. 1.3. 1.4. 1.5. 1.6 Aluminium Antimony Arsenic Beryllium Cadmium Calcium and magnesium Chromium Cobalt Copper and zinc Iron Lithium Lead Manganese Mercury Nickel Selenium Silicon Silver Strontium Tin Vanadium General Reviews and Observations Sampling and Sample Preparation Developments in Multi-element Analysis 1.3.1.Applications for routine measurement of biological fluids 1.3.2. Specialised studies of biological fluids 1.3.3. Tissues and other solid materials Reference Mate r ia Is Progress for Individual Elements 1.5.1. 1.5.2. 1.5.3. 1.5.4. 1.5.5. 1.5.6. 1.5.7. 1.5.8. 1.5.9. 1.5.1 0. 1.5.11. 1.5.12. 1.5.1 3. 1.5.14. 1.5.1 5. 1.5.16. 1.5.1 7. 1.5.18. 1.5.19. 1.5.20. 1.5.21. Conclusions Table 1. Summary of Analyses of Clinical and Biological Materials 2 Analysis of Foods and Beverages 2.1. Sample Preparation 2.2. Sample Introduction 2.2.1. Solid sample introduction 2.2.2. Liquid sample introduction 2.2.3. Gaseous sample introduction 2.3.Speciation Studies 2.4. Developments in Methodology for Atomic Absorption Spectrometry 2.5. Developments in Methodology for Plasma Atomic Emission Spectrometry 2.6. Topical Applications Table 2. Summary of Analyses of Foods and Beverages * Review Topic Co-ordinator, to whom correspondence should be addressed.44R JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, APRIL 1987, VOL. 2 This review describes developments in atomic spectrometry relevant to clinical and biological materials, foods and beverages reported in Atomic Spectrometry Updates References in JAAS, Volume 1 (86/C266-86/ 2039) and Volume 2 (87/1-87/395). Thus it follows the review published last year (87/91). The full references, names and address of authors can be readily found from the Atomic Spectrometry Updates References in the relevant issues of JAAS.However, as an additional service to readers an abbreviated form of each literature reference quoted (except for those to Conference Proceedings) is given at the end of the review. This innovation is in response to the suggestions of readers, and other comments as to possible improvements in future reviews are always welcome. It is hoped that succeeding reviews in this series will be extended to include X-ray spectrometry although this current review is principally concerned with the applications of AAS, AFS and AES (with arcs, sparks, plasmas, flames, furnaces and lasers) as well as ICP-MS. The format of the tables is as last year, in addition to the abbreviations listed elsewhere, Hy is used to show where hydride generation was used and S, L and G in the “Analyte form“ column signify solid, liquid or gaseous sample introduction, respectively.1. ANALYSIS OF CLINICAL AND BIOLOGICAL MATERIALS In a recent conference review of analytical atomic spec- trometry in biology and medicine, Dawson (86/C543) outlined the developments most likely in the immediate future as improved accuracy and speed for ETA-AAS, more multi- element analyses by ICP- and DCP-AES, the further develop- ment of element speciation systems and the evaluation of techniques such as ICP-MS for “special” rather than routine analysis. These trends are clearly visible in the literature and conference papers reviewed (Table 1) , although significant developments in faster ETA-AAS and in applications of ICP-MS must await future years. Great interest continues to be shown in the element A1 with some important work in the determination of A1 with some important work on the determination of A1 in tissues and bones by ETA-AAS and promising developments in the application of ICP-AES to the determination of A1 in serum and water.Perhaps more important is the topical interest in Se and, for this element, the developments in overcoming background correction problems in ETA-AAS are worth studying. 1.1. General Reviews and Observations In the past year, reviews have appeared on: trace element analysis of biological materials by Veillon (87/56); some applications of ETA-AAS in clinical analysis by Norval (86/346) with special reference to tissue analysis; analytical approaches for biomedical elemental analysis by Hook et al.(86/1687); direct Zeeman AAS analysis of solid biological samples by Hadeishi and McLaughlin (86/1784) ; the determi- nation of metal ions in nerve tissue using AAS and ICP-AES by Smeyers-Verbeke (86/1684) and indirect AAS in toxi- cology by Kovatsis (86/1404). Schlemmer and Welz (87/C205) considered the factors that affect the accuracy of trace element determination in biolog- ical materials using ETA-AAS. Zeeman-effect background correction was advocated to overcome the severe spectral interferences which, they said, plague D2-arc background correction. They argued that the standard additions technique does not correct for spectral interferences and in some circumstances can actually introduce errors. Further, the establishment of parallel working curves for reference solu- tions and analyte additions is not proof of absence of interferences.They also suggested that standard reference materials are only partly useful for method development as they do not behave analytically always the same as the samples to be measured. Sotera et al. (86/C1000) have also considered background correction in the analysis of biological materials. They recommended the Smith - Hieftje system because beam alignment is less critical than for D2-arc background correc- tion and structured background errors can be corrected. They proposed that, where background is greater than the compen- sation capability of the system, it can be reduced by sample introduction via aerosol deposition and by delayed atomisa- tion techniques.The accuracy of atomisation from the platform is often stressed, but Shuttler and Delves (87/C229) have highlighted the variability of thermal characteristics of commercially available platforms and tubes, certain batches of which led to poor accuracy in their method for blood Pb determination (86/1984). The problem was associated with differences in thermal contact between the platform and the tube along the machined grooves; better results were obtained by simply placing the platform in an ungrooved tube. Developments by the manufacturer are aimed at overcoming this deficiency. 1.2. Sampling and Sample Preparation Control of contamination in sampling is of great importance, particularly for the determination of elements such as Al, Cr and Mn normally present at very low concentrations in serum.Clean-room conditions are not vital as Ericson et al. (87/81) have shown, but instead close control of the choice of swabs, syringes, needles and sample tubes, the use of cleaning procedures where necessary and the minimum of sample pre-treatment are more important. Siliconised needles were used and sample tubes cleaned with dilute HN03 and then EDTA solution. This paper is recommended reading as it not only describes sensible methods for sampling of serum, but also outlines methods for determination of Cu and Zn in serum by ICP-AES and Al, Cr, Mn, Mo and Se by ETA-AAS and shows impressive results obtained for healthy subjects and for the NBS bovine serum RM. Some of the difficulties of analysing whole blood and serum can be overcome by protein precipitation techniques.Ekanem et al. (86/1799) have used precipitation with HN03 as a sample preparation technique for FAFS and FAES. Nitric acid was compared with HC1, chloroacetic acid and TCA and was chosen because it gave the largest volume of supernatant and the same nebuliser uptake rate as aqueous standards. De- proteinisation with HN03 has been applied also to the determination of Mn in serum by ETA-AAS (86/1051). An interesting development is the use of microwave heating in the rapid dissolution of biological materials. Blust et al. (86/1472) carried out digestion of brine shrimp samplesJOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, APRIL 1987, VOL. 2 45R Table 1. SUMMARY OF ANALYSES OF CLINICAL AND BIOLOGICAL MATERIALS Technique; atomisation; analyte form AA; ETA; L AA; ETA; L Element Unm Matrix Concentration Sample treatmentJcomments Reference Ag A1 A1 A1 A1 A1 A1 A1 A1 A1 A1 A1 A1 A1 A1 A1 A1 A1 A1 A1 A1 Blood, urine, Dialysis fluids tissues Samples were digested and extracted by dithizone into IBMK (in French) Atomisation from L'vov platform was claimed to eliminate interferences and the need for matrix modifiers Extensive precautions were necessary to avoid contamination during collection and storage of the samples The authors prepared an extensive, systematic examination of analytical parameters Samples were digested with HN03.A constant temperature atomiser was designed for the analysis which compared favourably with ETA-AAS using the L'vov platform Similar treatment was used for all types of sample which were analysed by an identical heating programme 0.2-2.0 mg powdered tissue sample were placed in graphite cup-in-tube furnace and 10 p1 of 2% HN03 were added 861200 1 Sl118 Sl192 861195 861197 861304 86JC558 86/C561 86lC.562 861714 86lC919 86lC 1238 8611342 861 17 17 8611753 86J1843 8611844 8611982 8611985 87/61 8 7 I C 2 2 7 - - - - - - 257.5 309.3, 396.1 309.3 396.2 - 396.2 - - 309.3 - 309.3 - 396.2 309.3 167.1 Serum 5-220 pg 1-1 AA; ETA; L Plasma Blood, tissues AA; ETA; L AE; ETA; L AA; ETA; L Blood, plasma, water Tissues AA; ETA; S Serum Plasma, tissues Bone AA; ETA; L AE; ICP; L AA; ETA; L Freeze-dried samples were digested under pressure with HN03 Bone was freeze-dried, powdered and ashed.Calibration with aqueous standards was possible at concentrations greater than 15 pg g-' but standard additions were used at lower levels.Recovery was 100% with a centrifugal micropartition apparatus. Extensive cleaning of the apparatus with 0.5 M HC1 was necessary. Mg(N03)2 - HN03 matrix modifier was not required Digestion with HN03 - H202. Background correction was achieved with measurements at 394.4 nm Protein precipitation with HN03 was compared as a technique of sample preparation with a method that used matrix modification and the L'vov platform. Similar results were obtained with both methods and with either D,-arc or Zeeman- effect background correction combustion tube which was then placed into the furnace (in Russian) Tissue samples were dried at 110 "C, digested overnight with HN03 at 50 "C and diluted with water for analysis A review of different methods (XRF, NAA, FAES , ICP-AES, ETA-AAS and histochemical staining), sample preparation and storage for A1 measurements Interference was noted from C1-, HC104 and proteins A1 - desferrioxamine complex was extracted from samples with benzyl alcohol Plasma and urine samples were analysed after dilution with 1 mM HN03 - 0.1% Triton X-100.Tissues were digested under pressure with HN03 optimum diluent was found to be 10 mM HN03 - 0.2% Triton X-100 The method exploits a newly discovered very sensitive A1 resonance line in the low vuv Ultrafilterable A1 in serum was separated None, sample was put into a graphite Samples were digested with HN03. The AA; ETA; L Plasma AA; ETA; L Tissues Serum AE; ICP; L AA; ETA; L - 0-150 pg 1-1 Plasma 32-630 pg 1-' 1.7-3.3 pg g-' AA; ETA; L Tissues AA; ETA; L Blood, tissues Serum, dialysis Plasma, urine fluids AA; ETA; L AA; ETA; L AA; ETA; L - 3-55 pg 1-1 100-1279 pg g-l - Plasma, urine, tissues Neural tissue AA; ETA; L AE; ICP; L Serum, dialysis fluids46R JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, APRIL 1987, VOL.2 ~~ ~ Table 1. SUMMARY OF ANALYSES OF CLINICAL AND BIOLOGICAL MATERIALS-continued Technique; atomisation; Matrix Concentration analyte form Element Wnm Al - Pharmaceuticals - AA; ETA. A1 - Serum 25-100 pg 1-1 AA; ETA As - Tissues 100 ng g-1 AA; ETA As - Blood As - Serum As 193.7 Urine As - Tissues 5 pg 1-1 AA; ETA; L - AA; ETA; L 7.5-249 wgl-1 AA; Hy; L - AA; ETA; L Cd 228.8 Urine Cd - Placenta B 249.8 Plasma 2.6-16.1 pmoll-1 Be 239.4 Urine 0-16pgl-l Ca - Serum 97.4 mg 1-l - Serum, urine - Ca Cd - Blood - Cd - Urine Cd 228.8 Blood Cd - Blood - Cd - Cd - Cd AE; ICP; L AA; ETA; L AA; F; L AA; F; L AA; ETA; L - AA; F, air - 5.7-17.5 pg 1-1 C&; L AA; ETA; L - AE; ETA; L 0.05 pg 1-I AA; ETA; L AA; ETA; S AA; ETA; L Blood, plasma 0.4-16.0 pg 1-' AA; ETA; L Hair - AA; F; L Biological samples 1-50 pg g-l AA; ETA; S Sample treatmenttcomments Reference - Serum (US ml) was mixed with 0.25 ml of 1.4 g 1-1 Mg(N03)2 - 10 mll-1 Triton X-100.No interference from uraemic serum was found Acceptable recovery was obtained with H2S04 - HN03 - HzOz digestion, heating to 450 "C with MgO and Mg(N03)2 and dissolution in HN03. NHJ was used as a reducing agent and the As halide was extracted in PhMe (in French) Blood was diluted with Triton X-100 - Samples were diluted with Ni in the presence of Triton X-100 Urine was heated with H2S04 - HN03 - HC104, diluted with H20 and reacted with NaBH4 to give AsH3 (in Chinese) Ca and Mg phosphates in tissue solutions produced spectral interference in the measurement of As.This was removed by the addition of 20 yg of Ni (to 10-yl sample). Atomisation was from L'vov platform Samples were diluted 1 + 9 with 0.02 M HCI Ni(N03)2 Urine samples were diluted (1 + 3) with 1% HN03 containing 0.25% Mg(N03)2 and 0.1% TritonX-100. Be was atomised from a L'vov platform The serum proteins were precipitated with TCA and the sample centrifuged (in Chinese) Ca in clinical samples Kjeldahl flasks with 30 ml of HN03, 7.5 ml of H2S04, 2.5 ml of HC104.The pH was adjusted to 6.0-6.5, extracted with 30 ml of dithizone - benzene and re-extracted into 5 ml of 0.5 M HN03. No background correction was required during analysis (in Japanese) Cd was extracted from urine as the iodide complex with trioctylamine in butyl acetate Blood was digested with acid and the Cd extracted with trioctylamine in IBMK 200-p1 samples of blood were deproteinised by mixing with 50 p1 of HN03 and 200 pl of H20. Cd was measured by furnace atomic non-thermal excitation spectrometry (FANES) with standard additions for calibration Urine samples were diluted with (NH4)2HP04. Cd was atomised from a L'vov platform (in Chinese) Solid sampling was compared with analysis after tissue destruction. Precision was poor for solid sampling but this was a rapid method and contamination was less likely to occur Samples were digested with HN03 at 110 "C for 4 h.H202 was added and the solution heated to dryness Optimum atom trapping conditions were investigated. 164-333 fold increased sensitivity was obtained (in Chinese) oxidation of sample with H2S04. Slurry was placed into furnace for analysis A review of methods for the determination of 5-ml blood samples were digested in A carbonaceous slurry was prepared by partial 871254 871295 861384 8611050 861 108 3 8611405 87/49 8611999 8611845 86/2003 871233 8617 10 8611054 8611422 8611642 8611754 8611758 8611937 871104 871297JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, APRIL 1987, VOL. 2 47R Table 1. SUMMARY OF ANALYSES OF CLINICAL AND BIOLOGICAL MATERIALS-continued Technique: atomisation; Concentration analyte form Element Unm Matrix Urine Sample treatmenttcomments Reference Cd 871303 8611756 871234 861712 8611341 8611469 8611796 871 18 87/47 s1645 861956 8611052 8611054 8611088 8611336 8611429 86/1688 86/1849 8611894 871239 871243 871303 8611339 8611 982 8612000 871239 0.001-4.6 pg 1-l AE; ICP; L Urine samples were digested with HN03 - H2S04 - HC104. The pH was adjusted to 5 and the Cd - APDC chelate formed.This was extracted with CHC13 and back- extracted with 1 M HN03 (in Chinese) Deproteinisation with HN03 or with HN03 - Cr(N0J3.9H20 gave lower results when compared with a direct analysis method. Recovery of Co added to blood was low (4&77'/0) with the deproteinisation methods Urine was mixed (10 + 1) with a Triton X-100 - HN03 solution and assayed with Zeeman- effect background correction, or diluted (1 + 10) with H20 and assayed with D2-arc background correction or analysed with D2- arc background correction after solvent extraction - Samples were diluted with Triton X-100.Air was used to assist ashing in the furnace Samples were diluted with equal volumes of 0.3% Triton X-100. Standard additions method was used for calibration Urine was diluted 1 + 1 with H20. Atomisation of the Cr was from a graphite probe Different analytical methods were compared. Superior precision was obtained for ICP. FAAS methods were sensitive to Cr oxidation state and to other interferences - AA; ETA; L co - Blood c o 240.7 Urine a-1.2 pg 1-1 AA; ETA; L Cr Cr Bile Blood, serum - AA; ETA; L 0.05-0.67 pg1-1 AA; ETA; L Cr 357.9 Plasma, urine 10-80 nmol l-1 0.3-0.5 pg 1-1 - - - 980 yg 1-1 - - 0-5 mg 1-1 - 690-1270 pg 1-1 - - 0.2-10 pg g-1 - 1008-1419 0.00&20.2 14.9-2 1.9 CLg 1-I pg1-l nmol g-1 3 3-53.72 pmoll-1 - - AA; ETA; L AE; ETA; L AA; F, N2O - C2H2; L AA; F, air - C2H2; L AE; ICP; L AA; ETA; L AA; F, air - AA; F; L C2H2; L AA; F; L AA; F, air - AA; F; L AE; DCP; L C2H2 ; L AA; -; - AA. _ * - 9 , AA; F, air - GH2; L AE; ICP; S AA; -; L AA;-;-; AE; ICP; L AA;-;L AA; ETA; L AE; ICP; L AA;-; L Cr Urine Cr Faeces Cr Urine Urine samples were diluted 1 + 1 with H20.Interference from urine matrix was shown to be temperature related and was absent below 2400 "C Muscle specimens, 0.8-12.0 mg, were extracted with 5 m10.75 M HN03 Continuous aspiration and aliquot sampling methods were compared.Aliquot sampling with peak-area measurement was claimed to be the best procedure aspirated into the flame Erythrocytes were haemolysed and the lysate See Cd, ref. 8611054 c u c u Muscle Blood, plasma c u Erythrocytes c u Urine c u 324.8 Urine No sample treatment. Calibration was by the Samples were diluted with 1 % HN03 (In Spanish) Review of methods for sample collection and Samples were digested with 70% HN03 - 70% standard additions method preparation HC104 - H20 (1 + 1 + 1) at 60-80 "C until clear solution was obtained. Temperature was increased to reduce the volume and H20 was added for the analysis None Samples were digested in a flow system during (In Chinese) passage through a microwave oven c u c u c u 324.8 324.7 Serum, urine Serum Plasma cu 324.8 Tissues c u c u Hair Blood c u Serum c u Urine See Cd, ref.871303 (in Chinese) Fe Liver Samples were dried and digested with acid See Al, ref. 8611982 Urine was diluted 1 + 10 with HCl. Non- See Cu, ref. 871239 (in German) specific emission was measured at 259.89 nm Fe Fe Plasma, urine Urine - 259.94 Fe Blood48R JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, APRIL 1987, VOL. 2 Table 1. SUMMARY OF ANALYSES OF CLINICAL AND BIOLOGICAL MATERIALS-continued Technique ; atomisation; analyte form Concentration 0-5 pg ml-1 Sample treatmentlcomments Reference Element h/nm Matrix Biological fluids AA; ETA; L Organic Hg compounds in biological fluids were separated by GC without any preparation. The GC was coupled to an AA spectrometer Liver homogenates were extracted with 0.2 M ammonium acetate.Pd was added which increased sensitivity 50-fold Blood samples were diluted and the proteins precipitated with TCA. The supernatant was extracted twice with cysteine and then KMnO, was added. H202 was added to remove excess of KMnO, and the solution analysed released and trapped on to Au - asbestos. Thermal desorption was carried out at 750 "C for 30 s and the Hg vapour transferred by N2 into a measuring cell (in Czechoslovakian) V205 mixture Hg in serum was reduced with NaBH4, Samples were digested with a HN03 - (In Chinese) (In Chinese) Results obtained by flame photometry were compared with those given by ion-selective electrodes KH2P04 - NH4N03 used as a matrix modifier eliminated interferences Specimens of hair were dissolved in HN03 - H202 and analysed with a Ta carbide coated tube X-100 (in French) Samples were treated by the addition of Triton None Samples were diluted 1 + 9 or 1 + 99 with 0.9% saline (in Czechoslovakian) (In French) Serum was diluted 1 + 10 with saline 861672 8611468 86lC1590 8611901 8611 902 871308 871309 861958 861303 861C557 8611084 8611334 8611686 8611899 8611995 871235 8611336 8611427 8611755 8611898 8612003 871294 8611051 8611053 8611760 8715 1 861958 S1196 861690 861955 - 253.7 - AA; ETA; L Liver Blood AA; cold vap.; L AA; cold vap. ; L Serum Tissues AA; cold vap.; L AA; cold vap.; L AE; F; L AA;-;- Urine Urine Serum 6-322 pg 1-1 2.4-4.6 pg 1-1 Serum, saliva Hair AA; ETA; L AA; ETA; L Li - 670.8 670.8 - 670.8 - 670.8 - 279.5 - - 11-76 ng g-j Li 2-40 pg 1-' AA; ETA; L Li Serum AA; ETA; L AE; F, air - C2H2; L C2H*; L AA;-;- AE; F, air - AE; F; L Li Li Serum Serum - 0.01-500 pmoll-1 - 0.25-1.50 mmoll-1 - Li Li Serum Serum Urine An ion-exchange resin was used to separate See Cu, ref.8611336 (In Chinese) Three Mg species in urine were separated and measured by a coupled HPLC - AAS (with ultrasonic nebuliser) system Tissue samples were homogenised interfering materials Li AE; DCP; L AA; F; L AA;-;- Serum, urine Erythrocytes Urine - 2.4 mmoll-1 - AE; graphite filament; L AA; F; L AA* _ * - 9 , AA; ETA; L Biological fluids, Serum Serum brain 20-40 mg 1-1 18.7 mg I-' 0.7-1.0 mmoll- See Ca, ref. 8612003 (in Chinese) Higher results were obtained if serum was not separated from cells within 4 h Protein was precipitated from plasma by mixing with HN03. This prevented accumulation of carbon deposits within the furnace Matrix modifiers and calibration procedures were investigated.Aqueous calibration provided better precision than did standard additions None Calibration was by the method of standard See K, ref. 861958 Direct determination with ammonium oxalate used as matrix modifier Proteins were precipitated with TCA. The Ni was chelated with NaDDC and extracted into isopropyl acetate HN03 - H2S04 - HClO, additions (in Chinese) Homogenised samples were digested with 1 Mn Plasma 0.63-2.09 pg 1-1 Mn AA; ETA; L Brain 2-100 pg 1-1 0.3-11.2 pg1-l AA; ETA; L AA; ETA; L AE; F; L AA; ETA; L AA; F, air - C2H2; L AA; ETA; L Mn Mn 279.4 - Sweat, urine Serum Serum Serum Na Ni 23 pg 1-1 0-20 pg 1-1 Ni Serum Ni Tissues 35-102 ng g-lJOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, APRIL 1987, VOL.2 49R ~~ Table 1. SUMMARY OF ANALYSES OF CLINICAL AND BIOLOGICAL MATERIALS-continued Element Wnm Ni Ni 0 2 Pb Pb Pb Pb Pb Pb Pb Pb Pb Pb Pb Pb Pb Pb Pt Sb Sb Sb Se Se Se Se Se Se Technique; atomisation; Matrix Concentration analyte form Plasma 0.32-1.80pgl-1 AA;ETA;L Urine 0.5-32 pg 1-' Air - Blood 60-520 pg 1-1 Blood 50-500 pg 1-1 Urine - Blood 5-333 pg I-' Urine 2.5-110 pg 1-1 Tissues - Blood - Blood - Blood - Blood - Blood - Biological samples 1-50 yg I-' Blood - Urine 0.018-43.3 Body fluids, brain Blood - 1-1 0.1-500 mg 1-1 Blood, urine - Urine 12-64 pg 1-1 Liver - Serum, hair, nails - Serum - Urine 2-100 pg I-' Serum - Liver - AA; ETA; L AE; d.c.glow discharge; G AA;-;- AA; ETA; L AA; F, air - AA; ETA; L GH2; L AA; ETA; L AA; ETA; L AA; F; L AA; ETA; L AA; ETA; L AA; ETA; L AA; ETA; L AA; ETA; L AA; ETA; S AA; ETA; L AE; ICP; L AA; ETA; L AA; Hy; L AA; ETA; L Candolumin- escence; F; L AA; ETA, F; L AA; Hy; L AA; ETA; L AA; Hy; L AE; ICP; L AE; ICP; L AF; Hy; L AA; ETA; L Sample treatmentlcomments Reference Samples were diluted 1 + 1 with 1 mM HN03 - Urine was diluted with dilute HN03 0.1% TritonX-100 - - 0.1 ml of blood was added to 0.4 ml of 0.2% See Cd. ref. 8611054 Triton X-100 and 0.5 ml of H20 Samples were diluted with a solution containing Triton X-100, H3P04 and (NH4)6M07024 and incubated at 37 "C for 30 min with HN03 (in Japanese) Pb in urine was atomised from L'vov platforms Pb was released from tissues by treatment with 3 N HC1 for 18 h.(Me)3Pb was extracted into CHC13 - EtOAc. HPLC was used to separate Pb species which were analysed by coupled ETA-AAS. Samples were digested with acid for the measurement of total Pb concentrations Three methods were compared. Chelation - solvent extraction and FAAS and ETA- AAS with D2-arc or Zeeman effect background correction Samples, 200 p1, were mixed with 200 pl 1% H3P04 and 10 pl taken for the analysis (in German) Blood was diluted 1 + 19 with NH3 - NH4H2 PO4 - (NH4)H2.EDTA. O2 was used in the 550°C ash phase. Pb was atomised from a L'vov platform atomised from a graphite probe of results obtained with different batches of graphite tubes and platforms Samples, diluted with Triton X-100, were See Pb, ref.8611984. Described variability See Cd, ref. 871297 A 5-fold dilution with dilute surfactant was See Cd, ref. 871303 (in Chinese) used See Mg, ref. 8611898 Samples were ashed with HN03 - H2S04 (in German) The study described acid digestion of samples and then a comparison of furnace programmes, types of graphite tubes and calibration methods Sb in urine at pH 3-4 was extracted as the APDC chelate into IBMK. 0.2 ml was adsorbed on to CaO - CaSO, for candoluminescence spectrometry V205 or with HN03 - HClO,. The Se was electrolysed on to Pt wire and atomised by simultaneous electrothermal and flame heating Samples were digested with HN03 - HClO, and the H2Se pre-concentrated on Chromosorb W at - 150 "C HNO, with HClO, was used at 75-210 "C to digest the samples.SeVI was reduced to selenite by heating with HC1 selenonium ion Tissue was digested with HN03 - H2S04 - HPLC was used to isolate the trimethyl- - 8611986 871236 8611333 8613 16 86/71 1 86111354 8611086 8611420 8611423 8611757 8611795 8611984 87lC 182 871C229 871297 871298 871303 8611898 8611752 8611900 8611981 861388 861389 861C560 86lC1227 8611439 Pd was added to remove the effect of Hg on the sensitivity of Se measurements in an organic matrix 86f146850R JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, APRIL 1987, VOL. 2 Table 1. SUMMARY OF ANALYSES OF CLINICAL AND BIOLOGICAL MATERIALS-continued Technique; atomisation; analyte form AA; ETA; L AA; ETA; L Element Unm Matrix Blood Biological samples Concentration Sample treatmentkomments Reference Pd was used as a matrix modifier to stabilise Se during the ash phase Solid samples were digested with HN03 under pressure.The solution was diluted 1 + 1 with matrix modifier and atomised from a L'vov platform A discrete aqueous sample was sucked into a flow of HCl, delivered to a pre-reduction coil at 95 "C and mixed with NaBH4. H2Se was evolved and swept to a heated atomiser cell 0.1% Mg(N03)2 - 0.5% Pd(N03)2 - Samples were diluted 1 + 4 with modifier Four digestion methods were compared and A procedure for gradual destruction was (Ni, Mg) gave concordant results developed with HN03 - H2S04 - HC104 taken to a final temperature of 310 "C in special long-neck flasks See As, ref. 87/49 Pt was used as a matrix modifier to suppress interference from phosphate and Fe - 86lC15 16 861C1542 8611718 8611759 8611938 8612029 87/16 87149 87lC211 871242 87/50 871299 8611856 8611999 861957 87lC206 Sl645 861C583 8611052 8611088 8611292 8611336 8611426 861 1429 8611685 Se Se - Se Biological samples 0.7-30 pg 1-1 AA; Hy; L Se Se 196.0 - Blood, liver Plasma 50-100 pg I-1 AA; ETA; L AA; ETA; L Se Liver AA; Hy; L AA; Hy; L Se Biological fluids AA; ETA; L AA; ETA; L Se Se Tissues Blood, serum - 196 - 33-500 pg 1-1 11.5-50.25 mgl-l AA; -; L Se Serum, seminal Urine fluid Ionisation interference was eliminated by dilution with LiCl Si 251.6 AE; DCP; L C2H2; L AA; ETA; L AA; F, N20 - Sn species were released by treatment with 6 M HC1 for 4 h, extracted into CHC13 - ethyl acetate and separated by HPLC.Detection was by coupled ETA-AAS to isolate Sr from Ca3(P04), Ion-exchange chromatography was employed See B, ref.8611999 Sn Tissues Sr Sr V V Bone Plasma Urine Urine AA; -; - AE; -; - AE; ICP; L 407.8 0.22-0.64 pmoll-1 0-100 pg 1-1 AA; ETA; L V was extracted from urine with cupferron - IBMK Urine samples were digested with HN03 - HC104 and extracted with 8-hydroxy- quinoline into IBMK See Cu, ref. 51645 AA; ETA; L AA; F, air - C2H2; L AA; F, air - C2Hz; L Zn Zn 213.9 213.9 Muscle Cerebrospinal fluid 20-170 pg 1-l Samples were diluted with 0.01 M EDTA, placed on to a Pt loop, dried and the assembly transferred into the flame which also had a slotted tube atom trap See Cu, ref. 8611052 Samples were diluted 1 + 9 with H20 Blood was diluted 1 + 24 with 0.1 M HC1. See Cu, ref.8611336 Plasma was digested with HN03 in a closed (In Spanish) Samples were aspirated as discrete aliquots Samples of serum were diluted 1 + 4 in H20 vial at 130 "C for 1 h and results compared with those obtained by continuous sampling. Poor sensitivity and precision was afforded by the aliquot sampling method (in Spanish) See Cu, ref. 86/1688 See Mg, ref. 8611755 See Cu, ref. 8611849 Erythrocytes Urine Blood, serum AA; F; L AA; F; L AA; F; L Zn Zn Zn - 213.8 - - 1.2-350 pg 1-l 442-8297 pg 1-' 213.9 - Serum, urine Plasma AE; DCP; L AA; F, air - GH,; L AA; -; - AA; F; L Zn Zn - 0-10 mg 1-I 9.32-11.61 mgl-I - Zn Zn 213.9 - Erythrocytes Blood, plasma Zn Zn Zn Plasma Urine Tissues 8611688 8611755 8611849 - AA; F; L AA; F, air - AE; ICP; S AA; F; L AA; F; L GH,; L - 213.9 None Samples were diluted 1 + 4 with H20 Cells were harvested by differential centrifugation Samples were diluted 1 + 4 with H20 See Cu, ref.871239 8611894 8611994 8611996 Zn Zn Zn Hair Serum proteins Leukocytes Zn Zn Serum, plasma Blood 600-1840 pg 1-1 - AA; -; L AA; -; L 861 1997 871239JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, APRIL 1987, VOL. 2 51R ~~ ~ ~ Table 1. SUMMARY OF ANALYSES OF CLINICAL AND BIOLOGICAL MATERIALS-continued Technique ; atomisation; Matrix Concentration analyte form Sample treatmentlcomments Reference Element Unm Serum 1482-1634 pg I-' AA; -; L Blood, urine - AA; F, air - CzHz; L See Cu, ref. 871243 (in Chinese) Protein in blood was precipitated by TCA. Serum and urine samples were diluted with H20. Slotted tube atom trap was used in flame (Cd, Cu, Pb and Zn) Tissue samples (1 g) were digested with 2 ml of aqua regia on a hot-plate for 30 min.The solutions and sera or urines were diluted with Li solution Proteins were precipitated with TCA. Slotted tube atom trap was used in the flame (Cd, Cu, Pb and Zn) 0.1 g of cellulose was suspended in 200 ml of urine, 1 mg of In added and pH adjusted to 8.5-9.0. The cellulose, with adsorbed metal hydroxides, was collected by filtration and the metals eluted with 2 ml of 2 M HC1 Samples were ashed at 450 "C in a muffle furnace Evaluation of a serum RM by an inter- laboratory study Simultaneous multi-element AA with carbon furnace atomisation 1 ml of serum was digested with HN03 - HC104 871243 Sl918 861C563 861C580 861C599 861667 861676 861C779 861977 861C995 8611025 86lC1110 861C1225 8611293 8611337 8611340 8611408 8611459 861 1797 8611798 8611799 8611998 8612002 861C2037 87/56 87181 8711 12 - Zn Various - (4) Various - ( 5 ) Serum, urine, - AE; DCP; L kidney Various - (4) Serum, urine - AA; F, air - CzH2; L Various - (8) Urine - AA; For ETA; L AE; ICP; L Various - Various - Various - Various - Various - Various - Various - Various - (18) (15) (10) (10) (18) (9) (12) Biological samples - AF; -; S Serum - Serum - AA; ETA; L Serum - AE; ICP; L Pancreatic stones - Urine - AE; DCP; - AE; ICP; L Y was added to undiluted urine as an internal standard Faeces - Tissues - MS; ICP; L AE; ICP; L AA; -; L Samples were dried, lyophilised and fat removed by CHC13 - methanol extraction.The powder was digested with HN03 at less than 100 "C Hair was washed, dried and ground to prepare a hair RM Various - Various - Various - (13) (7) (6) AA;-* - AE; I& L AE; d.c.arc; S Hair Serum Hair AE; ICP; L Hair was digested with HN03 - HC104 (95 + 5 ) , Co was added as an internal standard and diluted with HzO (in Chinese) (In German) Various - Various - Various - Various - Various - ( 5 ) ( 5 ) (7) (6) Tissues - Serum, urine - AA; F; L Samples were diluted and aspirated with a flow Samples were diluted and aspirated with a flow (In Chinese) injection analysis manifold injection analysis manifold Cerebrospinal fluid - Hair - AA; F; L AE; d.c. arc;- Blood - AE or AF; F; L Protein was removed by precipitation with Samples were diluted 1 + 9 with 0.01 M HC1 HN03 (Ca, Mg, P and Si) Various - Various - Various - (4) (18) (4) Urine - AE; ICP; L AE; ICP; L AA; ETA; L Serum, tissues - Blood, urine, - dialysis fluid Samples were analysed with furnace heating programmes that were much shorter than conventionally used (60-72 s) (Al, Ca, Cd and Pb) Review of the aDDlication of ETA-AAS to trace Various - Biological samples - AA; ETA; L element anah& in biological samples Review of procedures for sample collection, storage and analysis that allow for accurate measurements of trace elements in serum HN03 was used in preference to NH4N03 or (NH4)2HP04 as a matrix modifier. Samples were assayed without pre-treatment (in German) (As, Cd, Pb and Se) Various - (7) Serum - - AA; ETA AA; ETA Various - (6) Urine - L Biological materials - 871C205 Various - (4) S52R JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, APRIL 1987, VOL.2 Table 1. SUMMARY OF ANALYSES OF BODY FLUIDS AND TISSUES-continued Technique; atomisation; Element Unm Matrix Concentration analyte form Sample treatmentlcomments Reference Various - Biological materials - Hair - Various - (10) (4) Various - Serum - Blood, serum, urine - Various - (10) (4) AE; ICP; L Samples were digested with acid in a 871238 AA; -; - Methods involving digestion with HN03 and 871240 microwave oven ashing with a muffle furnace were compared. Wet ashing was suitable for Fe, dry ashing for Cu, Mn and Zn AE; ETA; L (In Hungarian) 871301 AA; ETA; L Blood and sera were diluted 1 + 1 with 0.2% Triton X-100. Urine was analysed without treatment (Al, Cr, Mn and Pb) (in German) 871302 directly in polythene or polypropylene autosampler cups (polystyrene cups were unsuitable) with 100 p1 of HN03 for 5 min in a commercial microwave oven.Water (1 ml) was added and the samples analysed by ETA-AAS. Microwave digestion with HN03 has also been used for the rapid digestion of samples for ICP-AES (87/238). A further novel idea was the incorporation of a microwave oven into a FI system for on-line mineralisation of whole blood samples (87/239). Digestion does not always need to be complete for trace metal analysis and two papers (86/C1974, 87/297), discussed further under Cadmium and Lead (sections 1.5.5 and 1.5.12), outline rapid partial digestion procedures. Dry- and wet-ashing techniques were compared as sample preparation techniques for hair analysis by Friel and Ngyuen (87/240).Dry ashing was recommended for Cu, Mn and Zn, but not for Fe which seemed to be partially lost. For Fe, wet ashing with HN03 was preferred. 1.3. Developments in Multi-element Analysis 1.3.1. Applications for routine measurement of biological fluids With their multi-element capability, ICP- and DCP-AES techniques have the potential to take over some of the more common determinations normally carried out in clinical laboratories by AAS and colorimetric procedures. Using inductively coupled plasma atomic emission spec- trometry, Mianzhi and Barnes (86/977) showed that ten elements, Ba, Ca, Cu, Fe, K, Mg, Na, P, Sr and Zn, could be determined in serum by ICP-AES with coefficients of varia- tion of from 0.7 to 6%. Sample digestion with HN03 - HC104 allowed standardisation with simple aqueous standards and gave more reliable results than ten-fold dilution of the sample.This latter procedure only gave reliable results for Ca, Mg, Na, P and Sr. Tanaka and Hayashi (86/1998) determined Ca, Mg, P and Si in urine by ICP-AES using just ten-fold dilution with 0.01 M HC1 and calibration with matrix-matched stan- dards. A rapid screening method for nine potentially toxic elements, As, Cd, Cr, Cu, Mn, Ni, Pb, Se and Zn, in urine has been described by Kimberley and Paschal (86/1025). Sequen- tially scanning ICP-AES was used with a N2-purged mono- chromator and a cross-flow nebuliser. An internal standard Y was added to both standards and samples. Direct current plasma atomic emission spectrometry has been shown to be a practical routine technique for the determination of Cu, Mg and Zn in serum and urine by Roberts et al.(86/1336). Serum samples were diluted with 1% V/V HN03 containing 0.1% V/V Triton X-100 and urine samples with 1% V/V HN03 containing 1 M LiN03. Calibra- tion was possible with simple aqueous standards. Results correlated well with those obtained by AAS. Kinsey and Fisher (86/C563), also using DCP-AES, have determined Cu, Fe and Zn in serum and urine after dilution of samples 1 + 5 with Li solution to give a final Li concentration of 0.5 g 1-1. 1.3.2. Specialised studies of biological fluids To extend multi-element analysis to the more difficult elements present at lower concentrations, pre-concentration is required for ICP-AES. Burba and Broekaert (86/C599) described multi-element pre-concentration using coprecipita- tion with Fe or In as hydroxides on cellulose.At pH 9.5-10, most elements were efficiently coprecipitated, but a few such as Al, U and V had maximum separation efficiency in neutral solution. The separated hydroxides bound to the cellulose were then eluted with 2 M HCl. The technique was shown to be suitable not only for ICP-AES but also FAAS and ETA-AAS. Direct determination of elements at low concentrations can be carried out by ETA-AAS and the multi-element version, simultaneous multi-element atomic absorption spectrometry (SIMAAC), has excellent potential, as Harnly has discussed (86/C520,86/C779). Detection limits are comparable to those of conventional line source AAS at wavelengths above 280 nm.At lower wavelengths, the lack of intensity of the Xe-arc source leads to SIMAAC detection limits becoming progres- sively worse and at the Zn wavelength (213.9 nm) the detection limit is ten-fold poorer than that of line source AAS. The technique has been successfully applied to the determina- tion of Cu, Fe and Zn in serum and separately for the determination of Al, Co, Cr, Mn, Mo, Ni and V (86/C779), as was discussed in last year’s Update (S/194, S/987). Graphite furnace atomic emission spectrometry also has potential for multi-element analysis. Papp et al. (86K288) built a 12-channel spectrometer for the determination of trace elements in biological fluids. This has been applied to the determination of Al, Ba, Co, Cr, Cu, Li, Mn, Mo, Ni and V in serum and lymphocytes (87/301).Concentrations in serum with and without digestion were in good agreement. Sequential analysis of cerebrospinalfluid for Ca, Cu, Fe, K, Mg, Na and Zn by FI-FAAS has been reported by Burguera et al. (86/1797). The sample was injected into a carrier stream of de-ionised water and standards prepared to contain physiolog- ical concentrations of albumin (and Na and P for certain determinations). For 12 healthy subjects, mean concentra- tions of 3387, 90.8, 46.1, 27.3, 0.30, 0.062 and 0.071 mg 1-1 were obtained for Na, K, Ca, Mg, Fe, Cu and Zn, respec- tively. Analysis of urine for the elements Cd, Co, Cu, Ni, Pb and T1 by ETA-AAS has been described by Berndt et al. (87/112). Normal concentrations of Cd, Cu and Pb could be measured directly, but pre-concentration was required for Co, Ni and TI.JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, APRIL 1987, VOL.2 53 R 1.3.3. Tissues and other solid materials Multi-element analysis of diet samples has been made more straightforward by inductively coupledplasma atomic emission spectrometry. Abdulla et al. (86/C1225) analysed representa- tive diets of teenagers in Sweden by wet digestion with HN03 and determined Ca, Cu, Fe, Mg, Mn and Zn by ICP-AES and Cd, Hg, K, Na, Pb and Se by AAS. The power of the ICP-AES technique was shown by Shiraishi et al. (8611720) on ashed diet samples by first determining the major elements Ca, K, Mg, Na and P at high dispersion and then, with that knowledge, standards were matrix matched for the determina- tion of 13 minor and trace elements.The versatility of the technique is obvious from recent studies, which include: 18 elements in livers and kidneys of dogs (86/2002); six elements in human hair (86/1340); inorganic elements in caterpillars, their diet and excrement (86/C849); forensic specimens, including tissues (86/305); and 21 elements in Chinese herbal medicines (86/C1237). The direct current plasma technique offers similar possibili- ties. Frank and Peterson (86/745) described their experience with this technique for the determination of 14 elements in biological materials of plant and animal origin. Care was necessary in optimisation and maintenance of the system to get acceptable stability. Long-term stability was then about 5% RSD. Analysis of NBS RMs indicated good accuracy.About 50 samples could be analysed per day which is equal to 700 individual determinations. Eighteen major, minor and trace elements have been determined in pancreatic stones by DCP-AES (86/C995) and this evidence together with studies by X-ray diffraction, SEM and energy-dispersive XRF allowed a picture of the structure of the stone and a possible mode of formation to be put forward. Concentrations of Cd, Cr, Ni, Pb and Zn in human lung, liver, spleen and kidney, determined sequentially by atomic absorption spectrometry, have been reported by Seemann et al. (86/1408). Attempts to analyse tissue by inductively coupled plasma mass spectrometry showed that the type of digestion used can cause problems, as McLaren et al. (86/C116) noted. Digestion with a mixture of HN03, HC104 and H2S04 resulted in spectral overlap by sulphur- and chlorine-containing mole- cular species. Dry ashing followed by dissolution in 0.1 M HN03 was advised.The potential of ICP-MS for metabolic studies using stable isotopes was discussed by Ting and Janghorbani (86/C1110). For studies with 70Zn, 58Fe and W u , most interferences were negligible or correctable with the instrument but 58Ni poses a major interference problem for 5*Fe, which needed to be solved by chemical separation. 1.4. Reference Materials Recent standard reference materials developed by the National Bureau of Standards are: SRM 955 lead in blood; SRM 2670 freeze-dried urine; and SRM 909 human serum (86/C544). Veillon et al. (86/676) described the characterisation of a bovine serum RM (NBS RM 8419).Recommended values for Al, Ca, Co, Cr, Cu, Fe, K, Mg, Mn, Mo, Na, Ni, Se, V and Zn have been produced. In Japan, Okamoto et af. (86/1293) prepared and certified a hair material for Ca, Cd, Cr, Cu, Fe, Hg, K, Mg, Mn, Na, Ni, Sr and Zn which is available from these authors. 1.5. Pragress for Individual Elements 1.5.1. Aluminium Determination of A1 continues to be of topical interest. Two reviews, from a Conference on Aluminium-related Disease in 1984, by Wills and Savory (86/1843) and Gitelman and Alderman (86/1844) surveyed methods generally for the measurement of A1 in clinical materials and determination by ETA-AAS, respectively. The former contains recommenda- tions for specimen collection and control of contamination. A further review on techniques of trace element analysis of water used in dialysis (87/21) discussed A1 measurement and found that the addition of acid to samples did not improve their storage stability.Methods using inductively coupled plasma atomic emission spectrometry seem to be of current interest. A Spanish group (86/C561) have critically compared ICP-AES determination at 396.1 nm with determination by ETA-AAS and concluded that, where A1 levels in serum, water and dialysis fluids are above 30 yg 1-1, ICP-AES is better but ETA-AAS has the superior detection limit and needs to be used at levels below this. The same group, collaborating with UMIST in Man- Chester, UK, have been pursuing better sensitivity with the ICP-AES technique by using three modifications: electrother- mal vapourisation of the sample; direct insertion on graphite into the plasma; and FI analysis with on-line pre-concentra- tion (87/C172). The most significant development is that of Tyler (87/C227), who was able to use the more sensitive 167.08-nm line in the VUV which shows less interference from other elements.Modification in the form of a purgeable periscope had to be made to the spectrometer to minimise the optical path length in air. Detection limits for A1 in water of 0.6 pg 1-1 and in serum of 1.5 pg 1-1 were achieved making the sensitivity comparable to that of ETA-AAS. More methods for A1 in serum by ETA-AAS have appeared but there is little that is new. The method of Van der Voet et al. (86/304) is interesting in that, using the same conditions and pre-treatment (ten-fold dilution with 0.2% Triton X-loo), whole blood, serum and water could be analysed.Two methods emphasise the use of Zeeman-effect background correction (S/192, 86/1985). As the background absorbance for the determination of A1 in serum is very low and there are no reports of any problems with D2 background correction, the type of background correction is largely irrelevant. As Bradley et al. showed (86/1342), results with the two types of background correction are equivalent. In their method, Andersen and Reimert (86/C562, 86/l985, 87/C146) diluted plasma and urine 1 + 1 or 1 + 3 with a solution 0.001 M in HN03 and 0.1% in Triton X-100 and injected 20 pl on to a platform in a pyrolytically coated graphite tube. Standard additions were used for calibration.Dilution of serum 1 + 4 with distilled water only was recommended by Guillard et al. (S/192). They used tantalum carbide coated graphite tubes and found that standard additions and calibration against simple standards gave identical results. Bel'skii et al. (86/1717) developed a novel procedure in which undiluted plasma was placed in a graphite boat and inserted into an electrothermal atomiser. Unreasonably high values of 32-56 pg 1-1 were obtained for the plasma of healthy subjects. The earlier work of Brown et al. (S/985), which claimed differences in calibration slope between normal and uraemic sera by direct determination, must be regarded as a red herring. This has not been found by other workers. Mikkelson and Windleborn (87/295) tried to duplicate the conditions of Brown et al.but found no significant difference in analytical recovery between normal and uraemic sera. Bradley et al. (86/1342) have shown that the protein precipitation method of Brown et af. gave results equivalent to those obtained with the direct stabilised temperature platform furnace (STPF) method of Leung and Henderson (Clin. Chem., 1982,28,2139) which Brown et al. had claimed gave these differences in slope. For soft tissues, dissolution techniques included digestion with HN03 and H202 (86/C1238), high-pressure digestion with HN03 (86/1985) and digestion overnight with HNO? at 50-70 "C (86/1753, 86/1985, 87/61). Thomassen and Radziuk (86/C558) demonstrated that it was possible to determine A1 directly in biopsy samples down to ca.0.5 pg g-1 using a cup-in-tube system designed for solid sampling. Calibration was by aqueous standards, using a less-sensitive spectral line for analysis. The limitation to measurement was not the54R JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, APRIL 1987, VOL. 2 instrument sensitivity but general contamination. Bouman et al. (86/1753) applied their method based on wet digestion of samples followed by ETA-AAS determination to the analysis of a range of tissues. Their values for controls are worth studying and are ca. 2 pg g-1 dry weight for brain, kidney and heart, for example. A patient with dialysis motor neuropathy had much higher values. Inductively coupled plasma AES was used by Vujicic et al. (86/C1238) to determine A1 in digests of tissues from rats.To obtain improved sensitivity, the conical spray chamber was replaced with a double cyclone spray chamber system. Smeyers-Verbeke and Vereeelen (86/714) determined A1 in bone of rats by first freeze-drying, coarse-fracturing in a PVC vessel, then pulverisation by the "brittle-fracture technique. " The powder was then low-temperature ashed and the ash dissolved in 10% V/V HCl or extracted with saturated EDTA for determination by ETA-AAS. Results for both treatments were similar although in 3 out of 13 samples lower results were obtained with EDTA extraction. Andersen and Reimert (86/1985, 87/C146) washed bone samples with methanol, defatted with chloroform and then digested the dry sample with HN03 at 70 "C overnight. For healthy unexposed individuals, the A1 content of bone was found to be 0.5- 5.0 pg 8-1.The dangers of A1 transferred to the blood stream by haemodialysis has stressed the caution with which we must view A1 contamination of preparations given intravenously. Andersen and Helboe (87/254) used ETA-AAS to measure high A1 concentrations in Factor VIII and IX given as antihaemophilia preparations; monitoring of these products for A1 concentration was recommended. Similar observations have been made by Fell et al. (Lancet, 1986, i, 380) who in addition found high A1 levels in plasma protein solutions and in albumin solutions used for blood plasma exchange (Lancet, 1986, ii, 467). McGraw et al. (86/1802) obtained data on the A1 content of milk formulas and intravenous fluids used for infants. All of these studies indicated that monitoring of these products should be carried out and further studies are needed on patients treated with them to assess A1 accumulation.In furthering understanding of the processes of accumula- tion and removal of Al, two studies looked at the speciation of Al. Pleban and Delbridge (86/C919) separated ultrafilterable A1 using the Amicon centrifugal micropartition apparatus with a membrane of 10 000 relative molecular mass cut-off and determined A1 by ETA-AAS. Extensive prior cleaning of the membrane with HC1 and de-ionised water was found to be necessary. Ultrafilterable A1 was 15-25%0 in patients on dialysis and increased to >50% when the patients were treated with desferrioxamine (DFO) for removal of Al. Desferriox- amine and its A1 complex was measured in blood plasma and urine by Allain et al.(86/1982). They converted DFO into its Fe complex with excess of Fe and extracted it into benzyl alcohol; the A1 complexes were extracted directly and both were determined, as Fe and Al, respectively, by ETA-AAS. 1.5.2. Antimony Liidersdorf et al. (86/1752) determined Sb in whole blood by hydride generation AAS after digestion with HN03 and H2S04. An RSD of 5.1-7.7% was achieved. A novel approach was used by Clark and Pate1 (86/1981) who determined Sb in urine by candoluminescence at 480 nm on a CaO - CaS04 matrix in an air - H2 flame after extraction of the Sb with APDC into IBMK. The results were compared with those obtained with ETA-AAS and showed reasonable agreement. 1.5.3. Arsenic Direct methods for As in serum (86/1083) and whole blood (86/1050) by ETA-AAS were developed; this has considerably simplified these determinations. Both methods used Ni as a matrix modifier and add a surfactant, Triton X-100.The method of Eaton and McCutcheon (86/1050) had a sensitivity of 5 pg 1-1, sufficient for the detection of exposure to As. Pegon (86/1083) achieved a detection limit of 0.4 pg 1-1 for As in serum. With Ni as matrix modifier, the ashing temperature could be increased to 1600 "C and the sensitivity was independent of the type of tube and mode of atomisation (wall or platform). Zeeman-effect background correction was used. Analysis of normal sera gave a mean concentration of 4.7 with a range of 2.2-6.7 pg 1-1. Wang and Lu (86/1405) determined As in urine with hydride generation AAS after digestion with H2S04, HN03 and HC104.Levels of As in urines of 120 healthy adults ranged from 7.5 to 249 pg 1-1. A comparative study of different mineralisation procedures for As determination in animal tissues was made by Van Hoeyweghen and Hoenig (86/384). The recommended pro- cedure was a combination of wet and dry ashing in which the tissue was first wet digested with a mixture of H2S04, HN03 and H202, evaporated to dryness, then dry ashed at 450 "C with MgO and Mg(N03)2 and dissolved in HN03. After reduction with NH41 in the presence of HCl, the As halides were extracted into toluene for determination by ETA-AAS. In a later method described by the same workers (87/49), extraction was avoided by direct determination of the digest with Ni as a matrix modifier.Calibration was with aqueous standards. The speciation of As as arsenate, arsenite, methylarsonic acid and dimethylarsonic acid has been achieved with anion- exchange HPLC separation using a linear gradient from water to 0.5 M (NH4)2C03 (87/13). The species were detected by ICP-AES at 197.19 nm with the spectrometer directly on-line. The method was applied to a study of As metabolism in cultured cell suspensions. 1.5.4. Beryllium Paschal and Bailey (86/1845) showed that Be can be deter- mined in urine without interference by applying the STPF concept in ETA-AAS. Samples were diluted 1 + 3 with a modifier of 0.25% n ~ l V M g ( N 0 ~ ) ~ and 0.1% VWTriton X-100 and analysed against simple standards. Coefficients of varia- tion of 4.1 and 10% for within-batch and between-batch analyses, respectively, were achieved for a urine containing 4.8 pg 1-1 Be.1.5.5. Cadmium A review by Stoeppler (86/1682) on Cd determination in biological and environmental samples has been published. Problems of sample collection, storage and preparation were discussed and analysis by AAS and voltammetry described and compared. A novel approach to the determination of Cd in blood is the use of furnace atomic non-thermal excitation spectrometry (FANES) by Falk et al. (86/1642). It is interesting that, with the low pressure used in this system, Cd could be atomised from CdC12 at temperatures as low as 140 "C. For the determination of Cd in blood however, deproteinisation with HN03 and an atomisation temperature of 600 "C were used.Although the tolerance of the FANES technique to interfer- ences was demonstrated to be better than that of ETA-AAS, some interference was still present and calibration was by standard additions. A detection limit of 0.2 pg 1-1 Cd in blood was achieved. Piperaki (86/1422) determined Cd in blood by ETA-AAS after acid digestion and extraction with trioctyl- amine into IBMK. A similar approach was used by Matsushita (86/710), who extracted with dithizone into benzene and then back-extracted with 0.5 M HN03. Measurement by ETA-AAS was made without background correction. Roberts and Clark (86/1937) also digested blood using HN03 and H202 but determined Cd directly on the digest. Their method was applied also to the measurement of Cd in blood plasma and used in studies of rabbits given oral Cd.JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, APRIL 1987, VOL.2 55R Three new methods for Cd in urine were reported, but only one allowed the direct determination. Liang (86/1754) used the STPF concept in ETA-AAS with (NH&HP04 solution as modifier and Zeeman-effect background correction. Lin et al. (87/303) favoured ICP-AES but this required a pre-treatment which involved digestion, extraction with APDC into chloro- form and then back-extraction into 1~ HN03. Solvent extraction of Cd as an iodide complex into butyl acetate was used by Flanjak and Hodda (86/1054) for determination by FAAS. Progress continues to be made in the application of solid- and slurry-sampling techniques for Cd in tissues. A compari- son of solid-sampling ETA-AAS with analysis after digestion for Cd in placenta has been made by Herber et al.(86/1758). Both methods gave good accuracy but the digestion method gave better precision. Solid sampling was quicker and less subject to contamination. Motkosky and Kratochvil (86/C1974) looked at slurry sampling with ETA-AAS for the assessment of the homogeneity of Cd in RMs. A slurry of 0.1 g of material in 10-300 ml of 5% V/V HN03 gave results which agreed satisfactorily with certified values for most of the materials studied. Its application to the assessment of homogeneity was limited because more than 90% of the Cd was extracted into the HN03. However, this does allow very rapid normal analysis in that a lengthy digestion can be replaced by a few minutes vigorous stirring with dilute HN03.A similar approach was used by Fagioli et al. (87/297). They used partial wet digestion with concentrated H2S04 and direct analysis of the carbonaceous slurry. 1.5.6. Calcium and magnesium A review by Gosling (87/233) on Ca measurement in clinical biochemistry covered requirements for Ca determination, pre-analytical errors and described and compared methods. Only 8% of laboratories who participated in the UK External Quality Assessment Scheme used AAS for measuring Ca despite the general recognition that it is the primary method for Ca determination and suitable as a reference technique. Most laboratories use colorimetric procedures, many as part of multi-channel analysers, which are more suited to large- scale routine use.The concentration of Mg in erythrocytes is about three-fold greater than in serum. Because of this, delay in separation may lead to erroneously high values, as Martin and McGregor (87/294) have shown. A delay of 24 h led to an 11% increase in serum Mg and differences in serum Mg concentrations became significant after separation had been delayed for only 4 h. Cai et al. (86/2003) determined Ca and Mg in cord blood and neonatal blood serum by deproteinisation with TCA followed by FAAS. By measuring whole blood Mg and plasma Mg by FAAS, Jiao et al. (86/1427) obtained erythrocyte Mg concentrations by calculation. Mean concentrations found in healthy women were 1.51 mmol l-1 in whole blood, 0.95 mmol l-1 in plasma and 2.40 mmol l-1 in erythrocytes. Wu and Robinson (86/1755) attempted speciation of Mg in urine using HPLC interfaced with FAAS.Three forms of Mg were found, the major form being the ionic form. 1.5.7. Chromium Zeeman-effect ETA-AAS has been used by Schermaier et al. (86/1341) for the determination of normal and elevated Cr concentrations in whole blood and serum. Whole blood was diluted 1 + 3 with dilute Triton X-100 and serum 1 + 1 and both were analysed against matrix-matched standards using a pyrolytically coated tube and air ashing in one of the char steps. Samples from healthy individuals gave a mean concen- tration of 0.37 pg 1-1 for whole blood and 0.13 pg 1-1 for serum; detection limits were 0.03 and 0.02 pg 1-1, respectively. The availability of the NBS bovine serum RM with a recommended value of 0.30 2 0.05 pg 1-1 (86/676) should help with the development of methods for this difficult determina- tion.A novel approach to the determination of Cr in urine has been made by Baxter et al. (86/1796) who used ETA-AES with probe atomisation and wavelength-modulation background correction. A less expensive monochromator with lower resolution was used in this study instead of the kchelle spectrometer used in previous studies. Nevertheless, Cr could be determined down to 0.3-0.5 pg 1-1 in urine. Comparison was made with determination by ETA-AAS. In both methods, matrix effects were minimised and analysis could be achieved with simple aqueous standards. Reasonable agree- ment was achieved between results obtained by the two methods. The ETA-AAS method used D2-arc background correction which had previously been stated (Guthrie, B.E., Wolf, W. R., and Veillon, C., Anal. Chem., 1978,50,1900) to be inadequate to remove background at the Cr wavelength. The problem with D2-arc background correction was investi- gated by Halls and Fell (87/47) and ascribed to breakthrough of emission from the matrix under the high gain settings necessary. By lowering the atomisation temperature to 2400 "C, the effects disappeared and correction was com- pletely satisfactory. The toxic form of Cr is believed to be CrVI. By using solvent extraction with a liquid ion exchanger and ETA-AAS of the extracts, Cavalleri et al. (86/712) studied the intravenous administration of CrV* to rats, When Cr appeared in the bile, less than 1% was present as CrVI.Chromium(V1) is obviously rapidly converted into Cr"1 in the blood. Morris et al. (86/1469) studied a group of stainless-steel welders who had been using high-chrome welding rods. A number of symptoms, including cracked lips and a rash on arms and hands were seen. This group had a higher plasma Cr concentration (mean 25 nmol 1-1) than other unexposed employees (mean 14 nmol 1-1 = 0.7 pg 1-1) and higher urine excretion (4.7 pmol per mole of creatinine) compared with the controls (1.3 pmol per mole of creatinine) . Measurement was by ETA-AAS using the procedure reviewed last year (S/615). Seemann et al. (86/1408) determined Cr concentrations in human tissues by ETA-AAS. Highest levels were found in the lung. Concentrations in muscle, liver and kidneys of slaugh- tered animals were measured by Schindler (86/746) using a digestion with HN03 for 45 min followed by ETA-AAS with a modifier of Mg(N03)2.The determination of Cr infaeces when chromium sesquiox- ide is used as a marker involves the measurement of much higher concentrations, but it is still not without its problems, as Lee et al. (87/18) have described. They compared titration with iron(I1) ammonium sulphate, AAS determination with air - C2H2 and NzO - C2H2 flames and determination by ICP-AES. The AAS methods showed poorest precision and were highly sensitive to interferences, oxidation state of Cr and changes in flame chemistry as a result of changes in operating conditions. 1.5.8. Cobalt In a comparison of the direct ETA-AAS determination of Co in whole blood with two methods involving deproteinisation with nitric acid and a HN03 - CT(NO~)~ mixture, respectively, Heinrich and Angerer (86/1756) showed that both deprotein- isation procedures significantly underestimated the Co con- centration. Only with the direct method was satisfactory recovery of added Co shown. Another comparison, in this instance of three methods for Co in urine, was made by Bouman et al.(87/234). These were direct measurement by ETA-AAS after 11-fold dilution with water (method D), measurement by ETA-AAS of the organic extract after solvent extraction (method E) and direct measurement by Zeeman-effect ETA-AAS after dilution 1 + 0.1 with a Triton X-100 - nitric acid solution (method Z). At56R JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, APRIL 1987, VOL.2 elevated concentrations, good agreement was obtained between all three methods, but normal levels could not be measured by method D. Methods E and Z gave reference values in the ranges (rl.0 and 0-1.2 pg 1-1, respectively; these methods had similar detection limits and precision. 1.5.9. Copper and zinc Smith and Holbrook (86/1688) reviewed methods for the determination of Cu and Zn in plasma and serum by AAS and interpretation of results in assessing Cu and Zn nutritional status. In view of the now well-established straightforward methods for determination by AAS with simple dilution of the sample, the appearance of new methods with more compli- cated preparation or more costly apparatus seems wasteful of human and material resources. Thus this year we have the determination of Zn in plasma by FAAS after 1-h digestion with €€NO3 (86/1426), determination of Cu (86/956) and Zn (86/1292) in serum by Zeeman-effect AAS and we are shown yet again (86/1997) that there is no difference between plasma and serum Zn concentrations.Liska et al. compared con- tinuous aspiration and microsampling in both peak-height and peak-area mode for Cu (86/956) and Zn (86/1292). Microsam- pling with peak-area evaluation was the most satisfactory in both instances. After dilution of the plasma 1 + 4 with distilled water, 2 0 0 4 aliquots were injected into the microsampling device. Whole blood was also analysed in the same way after dilution with 0.1 M HCl, 1 + 4 for Cu and 1 + 24 for Zn. Matrix-matched standards were used in all instances.Differ- ent conclusions were reached in another comparison of microsampling and continuous nebulisation for Zn in whole blood and plasma (86/1685). In this study, the injection method gave a loss of sensitivity (16-3270) and a loss of precision, but allowed the use of a smaller sample volume. Burguera et al. (87/239) reduced sample requirements for determination of Cu and Zn in whole blood by use of FI. A microwave oven was included in the flow system to mineralise the samples. Coefficients of variation of less than 3% were achieved. Liska et al. (86/1088) determined Zn in urine by FAAS after dilution of the samples 1 + 9 with water and calibration with standards in a NaCl - KC1 matrix or with commercial urine controls. For measurement of Cu, urine was nebulised directly and calibration made by standard additions.Copper levels in urine are normally low (<50 pg 1-1) and are better determined with pre-concentration or with a more sensitive technique, such as ETA-AAS. Flanjak and Hodda (86/1054) pre-concen- trated by extracting Cu as its iodide complex with tri-n- octylamine into butyl acetate. Results obtained were in good agreement with those by ETA-AAS. Patterson et al. (86/ C920) used ETA-AAS with platform atomisation and Zee- man-effect background correction in their method for Cu in urine. On separation of urine with HPLC and FAAS detection, Robinson and Wu (86/1755) found many Zn species including the ionic form. Complete digestion does not seem necessary for the determination of Cu and Zn in tissues. Bhattacharya et al.(S/645) extracted Cu and Zn from muscle biopsies with 0.75 M HN03 for subsequent determination without interference by FAAS. A mixture of HN03, HC104 and H20 (1 + 1 + 1) was used by Marrella and Milanino (86/1849) for extraction from rat tissues. Single strands of hair were analysed for Cu and Zn by ICP-AES using a direct sample insertion device (86/1894). Results compared well with conventional methods. Measurement of serum Cu and Zn provides only a crude indicator of Cu and Zn deficiency and it has long been a hope that the measurement of a particular cell or species in blood could provide a more sensitive indicator. In this review year, methods for erythrocytes (86/1052), Zn in leukocytes (86/ 1996) and distribution of Zn between albumin and a2-macro- globulin (86/1994) provided techniques towards that aim.Agarwal and Henkin (86/1052) compared haemolysis and HN03 digestion as pre-treatment procedures for the deter- mination of Cu and Zn in erythrocytes by FAAS and essentially similar results were obtained. However, there was increased instrumental noise in the determination of Cu in the acid digests, which was ascribed to undissolved particles in the extract. A detailed description of a technique for the separation of mononuclear and polymorphonuclear leuko- cytes was given by Purcell et al. (86/1996). This involved a fractionation on a Ficoll - Hypaque gradient with care to avoid contamination with platelets and extraneous Zn. For 29 healthy female adults, mean Zn values of 123 f 26 pg per 106 cells and 49 k 11 pg per 1010 cells were obtained for mononuclear and polymorphonuclear leukocytes, respec- tively.Killerich and Christiansen (86/1994) used ultracentrifu- gation for separation and found that most of the Zn in serum was bound to albumin with a highly significant correlation between serum Zn and serum albumin ( r = 0.74). The a2-macroglobulin bound fraction was 5-6% in controls and was unchanged in patients with cirrhosis of the liver and diabetes mellitus, but lower (ca. 2%) in patients with chronic renal failure. A novel approach to the determination of Zn is the use of the electrically heated platinum loop in conjunction with FAAS, which Ozcan and Ataman (86/C583) applied to the determination of Zn in cerebrospinal fluid. Drying of 30 pl of sample at 225 "C and ashing at 363 "C were carried out with the loop outside the flame; the loop was then moved by an electromagnet into the flame and simultaneously heated for atomisation.Chemical interferences were a problem which resulted in a requirement for standard additions for calibra- tion. 1.5.10. Iron Inductively coupled plasmas featured in two methods for Fe. Leflon and Plaquet (86/2000) determined Fe in urine by ICP-AES with a standard additions technique. Good correla- tion with a spectrophotometric method using bathophenan- throline was shown but the ICP-AES method has the advantage that it was not subject to interference by desferriox- amine, a chelating agent used in therapy for the removal of Fe. Ting and Janghorbani (87/15) combined ICP-MS with stable isotope dilution for the accurate isotopic analysis of human faeces for 54Fe and 58Fe to a relative standard deviation of ca.1%. Interference from 54Cr and 5XNi were overcome by instrumental correction and chemical removal , respectively. A method for the determination of Fe in liver tissue based on wet digestion and AAS determination was described by Preu et al. (86/1339). Iron concentrations of 17.0-21.9 and 14.9-20.1 mmol kg-1 were found in livers of men and women, respectively. 1.5.11. Lithium Lithium in serum is usually measured to monitor the therapy of patients with manic depression treated with Li2C03. This review year has seen an interest in measuring natural levels of Li in serum and it will be interesting to follow the findings from these studies. For monitoring therapy with Li, measurements by FAES or FAAS are adequate. For example, Otruba et al.(8611686) diluted 100 pl of serum with 10 ml of saline solution and sprayed this into an air - C2H2 flame for measurement by AES at 670.8 nm. The same workers (86/1995) also found that spectrophotometric determination with thoron gave similar precision and accuracy to their FAES method over the range 0.25-1.50 mmol l-1. The spectrophotometric method required the serum to be deproteinised first with TCA, however. Soltero (861351) interfaced a microcomputer to a commercial flame photometer for the automated determination of Li and K. For measuring natural levels of Li in serum, improved sensitivity is required. Bourret et nl. (86/1084) optimisedJOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, APRIL 1987, VOL.2 57R parameters for ETA-AAS achieving a detection limit of 2 pg 1-1. Pyrolytic graphite tubes, 150 "C drying, 1000 "C ashing and 2650 "C atomisation temperatures were chosen with an addition to the sample of Triton X-100 to give a final concentration of 0.1% V/V. A range of 2-17 pg 1-1 was found for the serum of healthy adults with a mean value of 8 pg 1-1. Trapp (86/303) favoured the use of a mixture of KH2P04 and NH4N03 as a matrix modifier and measured Li in saliva by the same technique. Concentrations in saliva were about three times that in serum. Nagy et al. (86/C290) also measured Li in saliva but by FAES in an air - C2H2 flame with Cs as an ionisation suppressor. The variable concentration of the interferent K in urine could cause problems in the determination of Li by FAES (87/293).This made the previously advocated use of LiCl as an exogenous marker for determining or checking volumes of urine specimens unwise as it was possible to underestimate Li by as much as 46%. This and other interferents could be removed by separation on a strong cation-exchange resin (87/235). Lithium was eluted with 0.5 M HC1 and determined by FAES. The measurement of Li in hair is unusual. Yao-han et al. (86/C557) tackled this by dissolution in HN03 and H202, evaporation to dryness, re-dissolution in dilute HN03 and measurement by ETA-AAS using a tantalum carbide coated tube. This tube gave better sensitivity and showed little variation with HN03 concentration whereas, with a normal pyrolytically coated tube, considerable variation was seen.There was no interference from a wide range of elements. Analysis of three samples gave values of 13,27 and 71 ng g-1. No reason was given why measurement of Li in hair should be made. 1.5.12. Lead As Pb is taken out of petrol, accurate blood Pb measurements will be of great importance in assessing the impact on the population of the reduction in Pb exposure. As part of a study of monitoring these changes, Shuttler and Delves (86/1984) developed an accurate ETA-AAS method for comparison with the Delves cup FAAS technique to be used in the study; a proportion of the samples were to be re-analysed by ETA- AAS as part of internal quality control procedures. Blood samples were diluted 1 + 19 with a mixture of NH3, NH4H2P04 and (NH4)2H2.EDTA and injected on to a L'vov platform in a pyrolytically coated graphite tube for determina- tion using a programme that included an O2 ashing step at 550 "C.Calibration was with standards in blood treated similarly. Brown et al. (87/C182) overcame some of the problems of using probe atomisation in ETA-AAS by using a new design of probe that reduced the problem of sample spreading. Blood samples diluted with 0.1% V/VTriton X-100 were successfully analysed for Pb with precisions of better than 3%. Osberghaus et al. (86/1757) compared three AAS methods for the determination of Pb in blood: FAAS following solvent extraction with APDC into IBMK; dilution of blood with 0.5% V/V Triton X-100 for ETA-AAS with D2-arc background correction ; and direct graphite furnace AAS with Zeeman-effect background correction on an instrument designed for solid sampling.Results from all three methods correlated well. The third method which involved the analysis of blood directly without pre-treatment was the fastest. Other methods developed for Pb in blood by ETA-AAS involved dilution with Triton X-100 (86/711, 87/298, 87/302), dilution with dilute H3P04 (86/1795) or dilution with a solution containing Triton X-100, H3P04 and (NH&Mo,O~~ and incubation with HN03 for 0.5 h (8611086). Hee and MacDonald (86/711) compared results obtained by their method with those obtained by isotope dilution MS and ASV. The STPF concept was used in the determination of Pb in urine by ETA-AAS (86/1420). Direct determination against aqueous standards could be made down to a detection limit of 2.5 yg 1-1.Urine Pb was also determined by ICP-AES after solvent extraction (87/303) and by FAAS, similarly after solvent extraction (86/1054). Lead in tissues could be determined by slurry sampling after treatment with dilute HN03 (86/C1974) or concentrated H2S04 (87/297) as discussed for Cd. For the reference material TORT-1, however, only half of the Pb was extracted by treatment with dilute HN03. Kliissendorf et al. (8611765) applied the solid sampling method of Rosopulo et al. (S/182) discussed in last year's review to an assessment of the distribution of Pb throughout pig livers. Distribution was nearly uniform (5-16% variation), simplifying sampling. Hydride generation catalysed by addition of Ni was used for the AAS determination of Pb in shellfish by Rodriguez et al.(87/C208). Total Pb and trimethyllead in tissues were deter- mined by Orren et al. (86/1423). Lead and its complexes were released from tissues by treatment with 3 M HCl for 18 h. Trimethyllead was extracted with a chloroform - ethyl acetate mixture and separated by ion-exchange HPLC. Fractions eluted with methanolic ammonium citrate solution were analysed by ETA-AAS. Total Pb was estimated after acid digestion. 1.5.13. Manganese The availability of an NBS reference material with a recom- mended value for Mn of 2.6 k 0.5 yg 1-1 (86/676) should help in establishing accuracy in methods for serum Mn measure- ment. Many of the problems, however, relate to contamina- tion in the collection and handling of specimens.For example, Tsai and Lin (87/51) determined serum Mn by ETA-AAS using standard additions calibration but their unreasonably high mean concentration for healthy adults of 4.2 pg 1-1 (range 0.3-11.2 yg 1-1) suggests that contamination was not properly controlled. Subramanian and Meranger (864051) found that previous methods involving simple dilution all led to a deposition of a carbonaceous crust in the graphite tube and so they developed a method based on HN03 deproteinisation using calibration against matrix-matched standards. No values for normals were given. No difficulty was experienced by Brodie et al. (87/302) in using simple dilution with 0.2% Triton X-100. Standard additions calibration was used in this instance . A direct method for the determination of Mn inperspiration and urine by ETA-AAS was described by Deano and Robinson (86/1760).Concentrations found in perspiration were ca. 100 pg 1-1, wheres in urine they were less than 2 pg 1-1. In the development of a method for Mn in mouse brains by ETA-AAS with Zeeman-effect background correction, Dougherty et al. (86/1053) compared standard additions and aqueous calibration curves. The use of aqueous calibration improved precision in an SRM (NBS bovine liver) and in brains. This was due to a better defined calibration curve; care was needed in the use of standard additions because of the onset of curvature at relatively low concentrations. 1.5.14. Mercury Apparatus for the speciation of mercury compounds in biological fluids using a combination of GC and ETA-AAS was described by Robinson and Wu (86/672).The outlet of the gas chromatograph was connected to a laboratory-built carbon T-tube atomiser. Samples could be injected without pre-treatment . Cysteine has been used as a complexing agent in methods for Hg by cold-vapour atomic absorption spectrometry before. Chow and Miroff (86/C1590) used it in a modified way for the determination of Hg in whole blood and erythrocytes. Cysteine was used to extract Hg from deproteinised blood or erythrocytes to bind the element for subsequent permanga- nate oxidation. Both inorganic mercury and organomercury58R JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, APRIL 1987, VOL. 2 compounds were successfully recovered by this method. Two reports from Taiwan (87/308, 87/309) described the applica- tion of cold-vapour AAS to the determination of urinary Hg levels in workers in a chlor-alkali plant and in dental surgeries, respectively.In the first study (87/308), workers in the plant had a mean urine concentration of 43.8 k 59.3 pg 1-1 compared with a mean of 7.9 k 3.9 pg 1-1 for controls. In the second, dentists and their assistants (87/309) had a mean concentration of 4.61 pg 1-1, higher than the controls (2.41 pg 1-1). The difference in control values between the two studies is notable. The direct determination of Hg in 1-2 ng of solid samples at concentrations greater than 0.1 pg g-1 could be made using ETA-AAS with Zeeman-effect background correction, as Fleckenstein showed (86/1794). Protein-rich samples had to be finely pulverised and covered with a layer of graphite.This work, applied initially to compost, earthworms and mush- rooms, has obvious further application to clinical materials. 1.5.15. Nickel The determination of Ni in serum remains a challenge. For assessment of occupational exposure, Ghe et al. (86/690) extracted Ni from serum deproteinised with TCA into isopropyl acetate with NaDDC and determined the Ni by FAAS. As the method required 20 ml of serum, it can hardly be described as practical. More straightforward was the method of Andersen et al. (86/1986) who measured Ni by Zeeman-corrected ETA-AAS using a pyrolytically coated tube. Samples were diluted 1 + 1 with a solution 10-3 M in HN03 and 0.1% in Triton X-100. For unexposed subjects, a mean concentration of 0.65 k 0.35 pg 1-1 was found.Although the method appeared to be accurate from the checks made, it failed to give the recommended value of 1.8 _+ 0.6 pg 1-1 for Ni in the NBS reference material, RM 8419 bovine serum. Instead, a concentration of 0.48 2 0.04 pg 1-1 was found. This suggested that the recommended value may be too high and the experience of other analysts with this material is awaited. Sunderman et al. (87/236) described an improved method for Ni in urine by Zeeman-corrected ETA-AAS in which urines were diluted with dilute HN03. A detection limit of 0.5 pg 1-1 was found for urine. Results agreed well with those obtained by the IUPAC reference procedure, but this method was more rapid and straightforward for routine use than the reference method. A mean value of 2.0 pg 1-1 was found for samples from 34 persons unexposed to Ni.The same laboratory developed a method for tissue (86/955) in which sample was homogenised in polythene bags, digested with a mixture of HN03, H2S04 and HC104 and the Ni determined in the digest by ETA-AAS with Zeeman-effect background correction. The method was applied to the tissue of rats injected with NiC12 solution and showed that most of the Ni was stored in the kidney. In control rats, the highest concentration was found in the lung. 1.5.16. Selenium Special attention has been paid this year to the problem of overcorrection in background correction using a D2 source in the determination of Se in clinical materials by ETA-AAS. Hoenig and Van Hoeyweghen (87/49) found that it could be eliminated by the correct choice of the amount of Ni added (20 yg of Ni for a 10-pl sample). The addition of Pd rather than Ni allowed the use of higher ashing temperatures which removed the interference (86/C143, 86/C1516); Pd also effectively removed an interference reported from mercury (8611468).Saeed and Hauge (87/C211) found Pt also effective in overcoming the overcompensation problem. Iron, which Studer et al. (86/C921) found to influence the determination of Se with D2-arc background correction, was very well tolerated (up to 1000 mg 1-1) when Zeeman-effect background correction was used in ETA-AAS. Schlemmer and Welz (86/C1542) used Zeeman-effect background correc- tion for the determination of Se in a range of biological samples using a mixed modifier of Pd and Mg(N03)2. For milk, serum and blood, oxygen ashing was incorporated in the furnace programme.A maximum thermal pre-treatment temperature of 1000 "C was advocated for biological materials (850 "C for urine) and direct analysis against simple aqueous standards was shown to be valid. Zeeman-effect ETA-AAS was also used by Saaranen et al. (87/242) to measure Se in seminal fluid and serum of men and bulls. The mean Se concentration in seminal fluid of bulls (457 yg 1-1) was about nine times higher than that in human males (33 pg 1-1) whereas the serum concentration (49.1 pg 1-1) was less than half that found in humans (78.2 pg l-l), an interesting observation to which many appropriate comments could be made! Pettersson et al. (8612029) compared four digestion proce- dures for the determination of Se in bovine liver by hydride generation AAS.These procedures [digestion using HN03 under pressure, a HN03 - HC104 - H2S04 mixture, HN03 with Mg(N03)2 and a HN03 - HC104 mixture] gave equivalent results provided standard additions calibration was used. Readers are cautioned that, although digestion did not seem so critical with this material, for other biological samples the digestion procedure is of primary importance. For example, Ihnat et al. (86/C559) reported the results of an IUPAC Interlaboratory trial on the determination of Se in serum and urine. Results obtained by hydride generation AAS were lower than those obtained by other methods. A later IUPAC study indicated that the digestion procedure was responsible and a recommended procedure for accurate results was developed.The studies of Welz et al. (S/494, S/590) which resulted in this procedure were discussed in last year's Update (87/91); Welz described his method further (87/16). Nakata et al. (86/1718) described their miniaturised continu- ous-flow system for hydride generation in which the pre- reduction from SeVI to SeIV was also part of the system. The sample was sucked into a concentrated HC1 line and passed through a coil at 95 "C, before addition of borohydride for reduction to H2Se. Brown et al. (86/1439) developed an electrically heated atom cell for use with hydride generation atomic fluorescence spectrometry. A limit of detection of 1.4 ng in aqueous solution was obtained. The cell was used in conjunction with a commercial discrete hydride generation system to determine Se in sera.Novel ways of pre-concentration of Se have been described. Bye and Lund (86/388) used electrolysis of Se from digested samples on to a Pt wire followed by AAS with simultaneous electrothermal and flame atomisation. Piwonka et al. (86/ 389), using hydride generation, pre-concentrated H2Se on Chromosorb W at -150 "C prior to atomisation. A detection limit of 6 pg was achieved and the method was applied to hair, nails and serum. A combination of hydride generation and a graphite furnace was used by Willie et al. (86/1922) to measure Se in marine sediments and tissues by AAS. The H2Se generated was passed through the injection hole of a furnace tube at 600 "C and trapped on the graphite surface; the mechanism for this was not clearly understood.Selenium was then atomised at 2600 "C. A comparison of ETA-AAS and hydride generation with both ICP-AES and AAS for the determination of Se in serum was made by Baurells et al. (861C560). Both hydride methods gave similar results with similar precision and sensitivity. Electrothermal AAS with Cu and Mg(N03)2 as modifier gave results which were 36% lower. The IUPAC trial (86/C559) however showed that, provided the methods were correctly set up, results from hydride generation AAS and ETA-AAS were similar. Morita and Shibita (86/C1227) combined HPLC and ICP- AES for the determination of the trimethylselenonium ion inJOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, APRIL 1987, VOL. 2 59R urine following an initial fractionation on an ion-exchange column.A detection limit of 3 pg 1-1 for trimethylselenonium was obtained which barely detected any of that ion in urines from four healthy individuals showing that the amount of Se excreted in this form was normally very small. 1.5.17. Silicon Plasma emission spectrometry allows the determination of Si readily and is rekindling interest in Si in clinical studies. Rodriguez and Sneddon (87/50) measured Si in urine by DCP-AES at 251.6 nm. Good agreement was obtained in a comparison with results by FAAS in a N20 - C2H2 flame. Concentrations in healthy persons and patients ranged from 11 to 50 mg 1-1. An ICP was used by Tanaka and Hayashi (86/1998). Urine samples were diluted 1 + 9 with 0.01 M HC1 using matrix-matched standards for calibration.For healthy adults they found a mean urine Si concentration of 28.7 k 10.4 mg 1-1. 1.5.18. Silver For a study of the toxic effects on rats of Ag salts, Kacimi et al. (86/2001) developed ETA-AAS methods for Ag in whole blood, urine and faeces. Samples were mineralised and the Ag was extracted with dithizone into IBMK. 1.5.19. Strontium The interference from the calcium phosphate matrix in the determination of Sr in bone by FAES was overcome by ion-exchange separation in a method developed by Razmilic (86/1856). Mauras et al. (86/1999) showed that blood plasma Sr concentrations in patients on haemodialysis (mean 0.62 k 0.24 pmol 1-1) were higher than those in controls (0.22 k 0.06 pmol 1-1). Measurements were made by ICP-AES after dilution of the samples ten-fold with 0.02 M HC1.1.5.20. Tin For speciation of tin in mammalian tissue, Orren et al. (87/299) used ion-exchange HPLC in tandem with ETA-AAS. All Sn forms were liberated from tissue by treatment with 6 M HC1, extracted into a 1 + 1 mixture of CHCl3 + EtOAc and introduced into the liquid chromatograph. Fractions collected were then measured by ETA-AAS. Mono-, di- and tri-ethyltin compounds were successfully separated. 1.5.21. Vanadium Direct methods for measurement of V in urine by ETA-AAS seem difficult; all recently published methods used solvent extraction. Buratti et al. (86/957) used cupferron as a chelating agent to extract V into IBMK whereas Bermejo-Barrera et al. (87/C206) used 8-hydroxyquinoline. They first digested the urine with HN03 and HC104.However, Buratti etal. (861957) compared direct extraction with extraction after digestion with H2SO4 and H202 and found no significant difference. They measured normal levels in 87 random urine samples from healthy male subjects and found a mean value of 0.36 k 0.19 yg 1-1. 1.6. Conclusions It is pleasing to find that, in comparison with the last review year, reported applications of ICP- and DCP-AES in this field seem to be more realistic and the techniques seem to be establishing themselves in their best capacity. With the decrease in capital cost, running costs and size of newer ICP-AES instruments, it seems inevitable that more will appear in clinical and biological laboratories. With the techniques of rapid single and multi-element determination, the speed of determination can seem immaterial if lengthy digestion procedures have to be used to dissolve the sample.The advances of solid sampling, micro- wave heating and partial digestion show an exciting potential for the analysis of tissues and other solid materials in this field. The large number of papers appearing this year with “Zeeman AAS” in the title might lead one to imagine that this was a new technique making inroads into solving analytical problems. That this is just an alternative means of background correction seems to have been ignored in most instances and it was even claimed that the Zeeman effect would actually remove interferences that were chemical in nature (S/192). For the majority of the methods described, correction with a D2-arc system would have been just as adequate.The true advantages of Zeeman-effect background correction are seen in the work on Se (86/C921, 86/C1542) and on solid sampling (86/1784), for example. It would seem more appropriate if “Zeeman” was not included in the title unless this form of background correction was important for the determination. Some authors have done this (e.g., 86/1984). Analysts who cannot afford Zeeman systems should not despair. Ways round some of the so-called deficiencies of the D2-arc system have been found (e.g., 87/47, 87/49, 871C211). It is to be regretted that there were no applications to review of that futher alternative approach to background correction, the Smith - Hieftje system. 2. ANALYSIS OF FOODS AND BEVERAGES The technique most favoured for the determination of trace elements in foods and beverages is atomic absorption spec- trometry, which accounts for over 70% of the papers reviewed.The vast majority of the AA literature describes analytical method development for the ETA-AAS determination of ultra-trace levels (ng ml-1). There is, however, a growing interest in ICP-AES, although this technique only accounted for some 1520% of the literature. The published work (see Table 2) also tends to suggest that the elements of greatest importance are Pb, Cd, As and Hg, respectively. With respect to sample types, the two most discussed are milk and milk products and edible oils. 2.1. Sample Preparation The two most common sample preparation procedures used to solubilise biological and food samples are wet ashing and dry ashing.Many of the earlier studies on this subject (for example Gorsuch, T. T., Analyst, 1959, 84, 135) were conducted on an element by element basis. More recently however the emphasis has been aimed more towards establish- ing suitable procedures for multi-element determinations. Miller-Ihli (WC1537) reported such a study for multi-element determinations in food samples using simultaneous multi- element atomic absorption spectrometry (SIMAAC) for both flame and electrothermal atomisers. Food samples as well as60R JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, APRIL 1987, VOL. 2 Table 2. SUMMARY OF ANALYSES OF FOODS AND BEVERAGES Technique ; atomisation; analyte form Element Unm A1 - Matrix Concentration Sample treat men tlcommen ts Reference AA; ETA; L AE; DCP; L Samples were digested with 12 N HC1 for 1 h at 70 "C in a steam bath.Comparable results were then obtained when measured by AAS, DCP-AES or colorimetrically with pyrocatechol violet Samples were diluted before injection into the graphite furnace. Milk formulas contained 94-1330 yg 1-l and intravenous fluids up to 3430 yg 1-1 of A1 Ni (400 mg) were added to the samples (0.1-2 g) and heated 10-30 min in microwave oven. There was no loss of As by volatilisation during wet ashing. Other metals or phosphate did not interfere with the determination The major water soluble As compound in crab was identified as arsenobetaine by HPLC - Comparison of 3 techniques: AAS, NAA and colorimetry. Good agreement was obtained between the 3 methods. Levels of As were considerably below European Economic Community limit Samples were digested (with HN03 at 200 "C), reduced with NaBH,, and the hydride concentrated in a liquid N, cold trap.Background correction was not necessary and no chemical interferences were observed Samples were ashed at 500 "C overnight. The residues were dissolved in 10 M HC1, As" reduced to As'*' with KI and ascorbic acid and pH adjusted to 4.5-4.8. As was coprecipitated with APDC and the precipitate dissolved in HN03 - H,Oz. Ni solution was added and As assayed from L'vov platform Samples were digested with acidic KMn0, or diluted. High concentration of Ni as matrix modifier was used. Both methods were sensitive and precise but slightly higher values were found with the acidic digestion (in Chinese) CHC13 and with methanol.The extract was passed through alumina and ion-exchange columns and As compounds separated by HPLC with off-line ETA-AAS detection HN03 and sample were placed in PTFE beaker in an autoclave, and heated at 140 "C for 1 h. Ni matrix modifier was added and the sample atomised from L'vov platform. Calibration against acid standards did not give correct results samples. Residues were dissolved in 1 M HCl and NaBH, added. The AsH3 was swept into the ETA furnace maintained at 600 "C and then atomised methanol generated methyl borate vapour which was fed into the flame Ca on the surface of rice grain was extracted with HC1 (in Italian) Powder was dispersed in polyethylene glycol octylphenyl ether (0.5%), Tween 80 or ethylene glycol ethyl ether and then atomised (in Chinese) HN03 (15-100 ml), HzSO4 (0.5 ml) and ICP-AES Samples were freeze dried, extracted with Mg(N03), was added for dry ashing the H2S04 was added to the juice.Addition of 8611059 8611802 861307 8611331 8611431 8611652 861 1672 8611800 8611850 87/46 871266 8611470 8611089 8611762 Plant materials - A1 As 193.7 Milk formulas and and intravenous fluids 94-3400 pg 1-1 30-300 pg 1-1 AA; ETA; L Shrimp AA; ETA; L AE; ICP; L AA; Hy; L - As - As Crab Sugar beet pulp, molasses AA; Hy; L Single-cell protein (Pru teen) - As NBS reference materials, plants, various foods 0.047-1 3.4 g-l AA; ETA; L As 193.7 Vegetable oil 0.04-0.19 pg 1- AA; ETA; L - As - As 0.15-51.8 I.18 g- AA; ETA; L AA; ETA; L Marine and freshwater fish, shellfish - As Lobster, scallop, plaice, oyster AA; ETA; G As 193.7 Lobster, oyster B 249.7 Citrus fruit juice 50-1125 pg ml-l AA; F, N20 - C,H,; L 3&80 mg kg-1 6.2-9.3 mg g-1 AA; F, air - AA; F; L C2H2; L - Ca Ca - Rice Milk powderJOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, APRIL 1987, VOL.2 61R Table 2. SUMMARY OF ANALYSES OF FOODS AND BEVERAGES-continued Element Unm Cd Cd Cd Cd Cd Cd Cr c u c u c u c u Fe Hg Hg Hg Hg K Li Mn Mo - - - - - - - 324.7 - - 324.8 248.3 253.7 253.7 253.7 253.7 - - - 313.3 Matrix Concentration Foods, milk - Milk 0.02-0.1 pg 1-1 Seafood - Pork liver - Honey, sugar - Lobster, scallop, - Meat, liver, kidney - plaice, oyster Tea leaves Milk powder Infant formula Edible oils Edible oils Meat Foodstuffs Lettuce, wheat Seafood Processed meats Foodstuffs Honey, sugar Wheat flour Technique ; atomisation; analyte form AA; ETA; L AA; ETA; L AA; ETA; S AA; ETA; S AA; ETA; L AA; ETA; L AA; ETA; L AA; F, air - C2H2; L AA; ETA; L AE; ETA; L AA; ETA; L AA; F; L AA; F; L AA; cold vap.; L AAS; cold vap.; L AA; cold vap. ; L AA; ETA; S AE; F, air - natural gas; L AE; F; L AA; ETA; L 0.44-2.22 pg g-1 AA; ETA; L Sample treatmentlcomments Re Foods were digested with HN03 - HC104, neutralised with NH3 and precipitated with APDC. Precipitate was then dissolved for the determination Samples were digested with acid and assayed from a L'vov platform. O2 was added during the ash phase German) higher values with fresh than with freeze- dried samples compared. Dissolution in 0.01 N HNO,; ashing with HN03 and H202 at 130 "C; chelation - solvent extraction and back extraction into 2 N HN03.Equivalent results were obtained with all methods (in German) See As, ref. 87/46. Calibration against acid standards 0.5 g digested with 6 ml of HN03 at 180 "C for 45 min, 50 pg of Mg(N03)2 added as matrix modifier to 20 p1 of sample (in German) Cu was extracted as (Cu14)3--, from 2 M HCl solutions of tea samples which contained 12% KI, into IBMK and aspirated into flame Powder was dispersed in a solvent and injected into furnace or on to graphite probe Samples were dispersed with 0.5% Triton X-100 and assayed from L'vov platform. Recovery was 96.5-101.3% Oils were diluted 1 + 9 with IBMK. Copper diethyldithiocarbamate was used for internal standard diethyldithiocarbamate was used for internal standard Meat samples were digested with HN03 - V205 - HC104 in closed vessels at 155 "C for 2.3-3 h.Recovery was 8&119% (in Chinese) Food samples were digested with HN03 and H2S04. Removal of oxidising materials was achieved with NH20H and Sn2+ used to form elemental Hg Drying temperature, grinding procedure and digestion conditions were investigated for losses of Hg. No loss was evident at room temperature or at 50 "C but 105 "C was unsuitable. No losses occurred during milling. With HN03 - KBr03 digestion mixture, 9&100% recovery was found See Cd, ref. 8611764 Sample was suspended in water following Direct analysis of solid samples (in Direct analysis of solid samples. Slightly 3 methods for sample preparation were Oils were diluted 1 + 9 with IBMK. Iron maceration in household food processor and the slurry introduced into a modified flame photometer 5-50 g of homogenised food were digested with HNO, - H2S04.Recovery was 99-101% and detection limit was 0.0013 mg kg-1 (10-g sample) See Cd, ref. 8611852. Extraction method gave lower results than the 2 other procedures Dried, powdered sample was digested with HN03 and diluted with H20. Recovery was 101% (in Chinese) :ference 861C846 861961 8611764 8611765 8611852 87146 861746 8611460 8611721 8611763 87152 87/52 86J353 8611057 8611437 8611764 8611838 861201 8611852 86135262R JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, APRIL 1987, VOL. 2 Table 2. SUMMARY OF ANALYSES OF FOODS AND BEVERAGES--continued Element hlnm Mo Na Pb Pb Pb Pb Pb Pb Pb Pb Pb Pb Ru Sb Sb Se Se Sn Sn Matrix Plant tissue Processed meats Spinach Potato Foods, milk Milk Cod, plaice Fish, milk powder Spinach Seafood Pork liver Honey, sugar Foodstuffs Single-cell protein Marine organisms (Pruteen) Single-cell protein (Pruteen) Lobster, scallop, plaice, oyster Edible oils and fats Canned foods Technique ; atomisation; Concentration analyte form 0.05-0.84 pg g-1 AA; ETA; L 7.0-15.0 gl-1 1-2 pg g-1 - - 0.7-2.0 pg 1-1 0.5-4.1 ng g-1 42-105 ng g-1 0.005 pg g-1 - - - - - 1-50 pg 1-1 - - - 0.5-240 vg g-1 - Foodstuffs - Sr Ti 336.1 Milk powder - Zn - Pork liver - Various - Plant tissue - (6) AE; F, air - AA; ETA; L natural gas; L AA; F, air - (32; s AA; ETA; L AA; ETA; L AA; ETA; L AA; ETA; L AA; ETA; L AA; ETA; S AA; ETA; S AA; ETA; L AE; F; L AA; Hy; L AA; Hy; L AA; Hy; L AA; ETA; L AA; ETA; L AA; Hy; L AA; F; L AE; ICP; L AA; ETA; S AA; ETA; L Plant samples were dried and ground to a particle size of 0.5 mm, digested at 300- 310 "C with HN03 - HC104 - H2S04.The mixture was neutralised followed by additions of SnC12 and NH4SCN - Fe solutions. Mo was extracted into diisobutyl ketone and measured See K, ref. 8611838 The sample was dried and ground to a powder which was suspended in a thixotropic gel (Viscalex HV30). The slurry was injected into the furnace. O2 was introduced during ashing. Slurry concentrations of up to 10% mlV were possible Milligram amounts of ash were introduced directly into the flame with a microsampling CUP The material was oven dried and ashed. See Cd , ref. 861C846 See Cd, ref. 861961 Fish samples were digested with HN03 in a closed system.Pb was separated from the matrix and the concentration enriched by solvent extraction (NH4)H2P04 was used as a matrix modifier. Fish tissues were digested with HN03 - HC104 and atomised from a L'vov platform Powdered sample was suspended in Viscalex HV30. See Pb, ref. 861664 See Cd, ref. 8611764 (in German) See Cd, ref. 8611765 (in German) See Cd, ref. 8611852 See Li, ref. 861201. Detection limit was See As, ref. 8611652 Milk powder was dissolved in H20. 0.19 mg kg-1 Sb in samples was reduced to SbH3 with 2% NaBH4 solution and passed through a heated silica tube. Optimum NaBH4, HC1 concentrations and gas flow-rates were determined. Ag, As, Bi, Fe, Sn and Te interfered See As, ref. 8611652 See As, ref. 87/46. Calibration against acid standards was possible Samples diluted with IBMK were injected into a furnace coated with Ta or Nb carbide.The carbide surface abolished strong matrix interferences. A detection limit of 0.3 pg 1-1 was obtained Foods were digested with HN03 - H2S04 - H202. Stannane was formed by the addition of NaBh. Recovery was 98.5%. The concentration of Sn in samples was up to 100 pg g-1 See Li, ref. 861201. Detection limit was 0.21 mg kg-l(10-g sample) A 1-g sample was heated at 450 "C for 8-9 h, fused with K2S207 in a flame and dissolved in hot H2S04. Recovery was 100-101% See Cd, ref. 8611765 (in German) Ascorbic acid was used to reduce sample matrix effects. Atomisation from L'vov platform also helped to remove suppressive Sample treatmentlcomments Reference effect of matrix 8611766 8611838 861664 861C761 861C846 861961 8611085 861C1540 8611648, 861664 8611764 8611765 8611852 86/20 1 8611652 87148 8611652 87146 86/91 861C833 861201 87117 8611765 s1591JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY , APRIL 1987, VOL.2 63R Table 2. SUMMARY OF ANALYSES OF FOODS AND BEVERAGES-continued Technique; atomisation; Element Unm Matrix Concentration analyte form Sample treatmentlcomments Reference Various - Plant tissue - AE; ICP; S Sample was introduced directly into plasma in 861386 Fish - AA; F; L Procedures for sample preparation prior to 861C597 Various - a graphite cup analysis were compared. No losses were observed with dry ashing. Poor recovery of Cd and Pb was found for digestion with HN03 - H202, while HN03 - HC104 digestion gave poor recovery for Pb (Cd, Cu, Pb and Zn) (18) (4) AE; ICP; L Kjeldahl digestion 861661 Various - Animal feeds - Various (SIMAAC) Bovine liver, rice - (15) flour, wheat flour ( 5 ) Various - Plant tissues - Grapefruit peel - Various - Plant tissues - Various - Milk - Various - (8) (21) (10) (7) Various - Food samples - (16) Various - (8) Various - Various - (4) (4) Grapefruit juice - Chocolate - Crops - Various - Total diets - Fruits, vegetables - Various - Food homogenates - Various - (18) (4) ( 5 ) Various (CSAAS) Milk powder, - ( 5 ) Pruteen Various - Milk, cereals - Various - Edible oil - (6) Various - Various foods - ( 5 ) Various - ( 5 ) Food samples - AA; ETA; L Materials were digested with HN03 - H202.861665 Samples were then injected on to a graphite probe with HN03 - H202 AE; ICP; L 861715 AE; ICP; L - 861962 Samples were digested in a microwave oven 86/ 105 8 AE; ICP; L - 8611092 AA; ETA; L Whole milk samples were injected into graphite furnace together with n-octyl alcohol.Recoveries were 95-107% and results agreed well with a dry-ash procedure 10 ml of aqua regia for 30 min. Li (5 p.p.m.) was included in the final solution and in the standards Digestion of the samples was carried out with aqua regia in a PTFE pressure vessel in a microwave oven 90-97% (As, Cd, Cu and Pb) ammonium acetate. Extracts were ashed and atomised in a graphite furnace. The atomic vapour was excited by laser irradiation and the fluorescence was measured (Co, Cu, Fe and Mn) (in Russian) AE; DCP; L 1 g of the dried sample was refluxed with 861C1230 AE; ICP; L 861C1231 AE; ICP; L AF; ETA, laser; L Samples were ashed at 450 "C.Recoveries were Analytes were extracted from samples with 8611410 8611424 - 8611720 AE; ICP; L AA; -; L AA; ETA; L AA; F, air - CzH2; L AA; ETA; - AE; ICP; L AA; F; L AA; ETA; L AA; F; L Samples were digested with HN03 - H2S04 - H2O2 (Cu , Fe , Mn and Zn) A slurry of sample in water was prepared and sprayed into graphite furnace via a Fastac sampler (in German) HC104 for effective slurry atomisation compared. Poor recovery was found with extraction methods. Dilution and char- ashing were satisfactory Dried samples were powdered to a particle size of less than 50 pm and suspended in Viscalex HV30, in-furnace O2 ashing was used to reduce organic matrix Dried samples (0.02-1.0 g) were digested with 15-75 ml HN03, 0.1-0.5 ml H2S04 in a microwave oven for 10-30 min.Recoveries were 84113% and results agreed well with those from a wet-digestion method 8611801 8611851 The samples were digested with HN03 - 8711 10 871C162 87lC 177 Particle sizes were reduced to <8 pm for 3 methods for sample preparation were 871C186 87124464R JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, APRIL 1987, VOL. 2 NBS SRMs were used extensively for the evaluation of the ashing techniques with regard to analytical accuracy and precision. Potential sources of contamination , analyte loss and a survey of trace metal contaminants in a wide range of commonly used reagents were also discussed. A study by Protasowicki (86/C597) compared dry ashing , wet ashing with a HN03 - Hz02 mixture and wet ashing with a HN03 - HC104 mixture for the determination of Cd, Cu, Pb and Zn in fish tissue.All three procedures produced accurate results for Cu and Zn determinations. Wet ashing with HN03 - HC104 resulted only in Pb losses. Taking into account all four analytes only the dry-ashing procedures, which involved mineralisation with HN03, produced acceptable accuracy and recovery of standard additions. These results are difficult to understand since, in general, dry ashing, especially with HN03 as an ashing aid, is not recommended for Cd determination. It is also difficult to understand why a HN03 - H202 wet-ash procedure would result in Cd or Pb losses. Further, wet ashing with a HN03 - HC104 mixture is, in fact, normally the recommended procedure for the determination of Pb in these samples.The comprehensive treatise by Gorsuch entitled "Radiochemical Investigations on the Recovery for Analysis of Trace Elements in Organic and Biological Materials" previously referenced is still one of the best sources of information on sample preparation procedures for trace element determinations in organic and food samples. In recent years there have been some novel ideas for sample digestion procedures. A number of papers have appeared on the use of domestic pressure cookers as alternatives to expensive steel pressure-bombs (see ARAAS, 1984, 14, 95). This review year has seen the arrival of papers reporting the use of microwave oven digestion procedures. Two papers by a Japanese research group (86/307,87/244) reported the use of a microwave oven to digest food samples for the determination of As, Cd, Cu, Mn, Pb and Zn.For As, 0.1-2.0 g of dry sample were digested with 15-100 ml of HN03 and 0.5 ml of H2SO4. Nickel (400 mg) was added to prevent volatilisation of As species during the subsequent determination by ETA-AAS. The digestion time was 10-30 min, which is considerably shorter than conventional digestion procedures. Recoveries of As added to sea-food samples were 85.9-104%. A similar procedure, but without the addition of Ni, was used for Cd, Cu, Mn, Pb and Zn determinations. Recoveries of the five metals added to the food samples were 84.3-113%. The values obtained agreed well with those from a conventional wet- digestion method. White et al. (86/715) reported the use of a microwave oven and HN03 - H202 digestion of botanical samples prior to elemental determination by ICP-AES.The elements studied included Ba, Ca, K, Mg, Mn, Na, P, S and Zn. Accuracy was confirmed by the analysis of eight reference materials. Digestion procedures for mercury determination continue to be reported, One study investigated the loss of Hg whilst drying at room temperature, 50 or 105 "C and during milling and digestion with HN03 - KBr03 (86/1437). Milling of samples did not result in losses of Hg due to adsorption by the mill or evaporation. The HN03 - KBr03 digestion resulted in recoveries of 90-100%. It was suggested that this procedure was better than a digestion with HN03 - KBr. A Chinese paper (86/353) recommended digestion with HN03 - V205 - HC104 in an enclosed vessel at 155 "C for 2-3 h.Recoveries of Hg added to meat samples were in the range 80-119%. Harms (86/1085) studied the possibility of improving the determination of low lead concentrations in marine fish by ETA-AAS. The method involved a digestion with HN03 in an enclosed vessel followed by separation and concentration of Pb by solvent extraction. The major source of systematic error was the value of the blank and special precautions were taken to minimise the blank level and variability. Results obtained for muscle tissue were 0.5-4.1 ng g-1 which were considerably below most previously published data. Okubo reported a method for the determination of arsenic in food samples by ETA-AAS. Samples were digested in HN03 - HC104 - H2S04 with the addition of 500 mg Ni to reduce volatilisation losses during digestion.Recoveries of As from seaweed were 95.4-104%. Canned tuna, shell fish and dried squid contained 1.2, 0.1 and 128.5 pg g-1, respectively. 2.2 Sample Introduction 2.2.1. Solid sample introduction The one application area which has grown in popularity almost exponentially over the past few years is the direct analysis of solids, slurries or suspensions by FAAS, FAES and ETA- AAS. Eastwood et al. (86/C671) described a microsampling cup technique for the determination of Pb in vegetation by FAAS. Milligram amounts of dried sample were weighed into a microsampling cup and then ashed externally prior to insertion directly into an air - C2H2 flame. The method was applied to samples from a field experiment to assess the distribution of Pb in potato plants grown in various Pb containing soils at different locations.A simplified slurry method for the determination of dietary salt in processed meat by FAES was reported by Wichman et al. (8611838). The recommended slurry was 2% m/V and was prepared using either a home food processor (kitchen meat grinder) or a stainless-steel homogeniser with a PTFE bearing. A wide- bore, clog-free, 19-hole, pre-mixed air - natural gas burner head was mounted on a Jarrell-Ash spray chamber with a purpose-built PTFE slurry nebuliser for atomisation of the slurry samples. Both K and Na were determined using an old filter photometer instrument. The normal analyte range in the 2% m/V slurry was 60-150 pg ml-1 for K and 80-350 pg ml-1 for Na.Although this is not a particularly demanding determination with respect to the levels of analyte in the samples, the slurry approach overcomes the need for wet- or dry-ashing procedures and is therefore less labour intensive. The direct insertion into a graphite furnace of milligram amounts of freeze-dried and fresh liver samples for the ETA-AAS determination of Cd, Pb and Zn was reported by Klussendorf et al. (86/1765). The relative standard deviations for Cd, Pb and Zn were 7-10, 5-16 and 3-570, respectively. The method could be used for official veterinary meat control and examination. In a similar study Cd, Hg and Pb in fresh and dried marine foodstuffs were determined (86/1764); the procedure was rapid enough for production control.Problems in standardisation, which have traditionally been responsible for the poor reputation of the solid sampling ETA-AAS technique, have been reduced due to the improved availability of SRMs or quality control samples. In some instances it is also possible to use aqueous standards, especially if the sample is atomised from a solid pyrolytic graphite platform or sampling boat, where isothermal atomisation conditions are approached, reducing chemical interferences. The alternative approach to solid sampling in ETA-AAS is slurry atomisation. In a series of papers based upon this approach Ottaway and co-workers (86/664,86/1648,87/C186) reported the determination of Cd in sprouts, Cd, Cu, Mn, Pb and Zn in ICI Pruteen (a single-cell protein), Cu in cabbage and pine needles and Pb in liver, tomato leaves, oyster tissue and spinach.Samples (0.5-10 g) were freeze dried, ground in an agate ball-mill for 90 min to obtain particle sizes of less than 50 pm, transferred into a tissue grinder and homogenised with 10-20 ml of distilled water. The slurry was then transferred into a 100-ml flask where 2-3 ml of a thixotropic thickening agent, Viscalex HV30, were added and the mixture was neutralised with ammonia solution. The flask was continu- ously agitated during formation of the slurry and then the thickened sample was diluted to 100 ml with distilled water. A 2 0 4 aliquot was injected into a pyrolytically coated graphite tube. During ashing, O2 was added (20 ml min-1 for 30 s, 800 "C) to avoid the build up of a carbonaceous residue in theJOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, APRIL 1987, VOL.2 65R tube. Concentrations of slurry up to 10% m/V could be tolerated. For most samples recoveries of added analyte approaching 100% were obtained using aqueous standards and peak-height measurement. A further paper from the same research group reported the determination of Cu in milk powder by ETA-AAS (86/1721) using the homogeneous dispersion method. In this method, the dried-milk sample was dispersed in a solution just before injection into the atomiser. Chemical interferences from the milk matrix were avoided when graphite probe atomisation was used. With tube-wall atomisation, the standard additions method had to be used to obtain accurate analytical results. Both these methods are elegant when compared with the conventional dry- or wet- ashing procedures, which are time consuming and are prone to contamination. Ebdon et al.(87/C162) reported the results of a comprehen- sive study on slurry nebulisation into an ICP and DCP. Parameters that critically affected slurry nebulisation included choice of nebuliser, particle size, injector tube diameter, dispersant, slurry viscosity and plasma characteristics. It was demonstrated that, for efficient atomisation, particle sizes of less than 8 pm were necessary. 2.2.2. Liquid sample introduction Recent developments in liquid sample introduction to flame or plasma instruments include various FI manifolds with the possible addition of mini-pre-concentration columns (see ARAAS, 1984, 14, 99).From the literature reviewed it is apparent that these procedures have not, as yet, obtained widespread use in the food industry. 2.2.3. Gaseous sample introduction The determinations of hydride forming elements and Hg are important in the food industry due to the toxicity of these elements and the strict control of levels allowed by govern- ment regulations. As part of a continuing collaborative study of the determi- nation of trace elements in dried sugar beet pulp and molasses, Huijbregts et al. (86/1409, 86/1431) reported on the determi- nation of arsenic. Fourteen samples of dried pulp were distributed and subjected to replicate analyses in participating laboratories. The samples were analysed by hydride genera- tion AAS, NAA and colorimetric determination after com- plexation of As with silver diethyldithiocarbamate.Good agreement was found between results obtained by the different methods. The limits of detection ranged from 0.05 to 0.1 mg kg-1. The concentrations of As found were generally considerably lower than the EEC limit for As in sugar beet pulp. Trace amounts of As in the dried pulp were related to the fuel used in the pulp driers. In marine organisms, As is usually present as an organo-arsenic compound. Saito and Iwajima (86/1331) studied the decomposition of dimethyl- arsine using a HN03 - H2S04 or HN03 - HC104 - H2SO4 mixture prior to determination of As by hydride generation AAS. The HN03 - H2SO4 digestion produced poor recoveries indicating that the dirnethylarsine was not completely di- gested. Use of HN03 - HC104 - H2S04 produced acceptable results.Other useful work on hydride forming elements includes a paper by Maker (87/48), who reported the determination of Sb in marine organisms and waters by stibine generation and AAS. As the levels were so low, Sb was coprecipitated with 5% m/V lanthanum hydroxide solution to pre-concentrate the Sb and also to remove potential interferences. A solution of potassium iodide - ascorbic acid was added prior to reduction by 2% m/V NaBH4 solution to reduce SbV to Sb"1. The detection limit was 0.0018 pg ml-1. For a solution containing 0.05 pg ml-1 Sb, the relative standard deviation was 3.6%. Alvarey and Caper (86/C833) reported the determination of Sn in foods by hydride generation AAS. Samples were digested in H202 - HN03 - H2S04.The analytical range for the method was 0.5-240 pg 8-1; the limit of detection was 0.2 pg 8-1. A mean recovery of 98.5% was obtained for ten canned foods with added Sn. Tin concentrations in canned foods ranged from below the detection limit to about 100 To obtain an additional improvement in sensitivity for hydride generation procedures it is possible to collect the evolved hydride in a liquid N2 trap. After pre-concentration, the trap is removed from the liquid N2 and allowed to heat up, producing a fast, transient atomic absorption peak. This procedure was used to determine As, Sb and Se in ICI Pruteen (86/1652). Detection limits for As, Sb and Se were 0.1,O.l and 0.5 ng, respectively. The method produced improved sensitiv- ity, good precision, freedom from interferences and did not require background correction.Another method to improve the sensitivity of the hydride generation procedure was reported by Sturgeon et al. (87/266). In this method the evolved hydride was introduced into the centre of a graphite furnace held at 600 "C where it was trapped on the surface of the graphite tube. Old, used, graphite tubes produced trapping efficiences 10-15% better than new, pyrolytically coated graphite tubes. After collection, the hydride was atomised at 2600 "C for 4 s. Calibration was achieved by use of aqueous standards. The method was applied to the determina- tion of As in marine sediments, tissues and sea water. Sample volumes of 10-500 p1 produced detection limits (three times the standard deviation of the blank) of 60 pg g-1 in sea water, 0.2 pg g-1 in sediments and 0.15 pg 8-1 in tissues.Precisions of 2-3% were typical for the analyses of these samples. The determination of Hg in foods did not receive as much attention as in previous years (86/353, 86/1057, 86/1090, 8611437). 2.3. Speciation Studies The literature on speciation is still growing rapidly, especially in the environmental, clinical and food application areas. Of particular interest is the identification of As species in fish and shellfish. Lawrence et al. (86/1850) coupled an HPLC separa- tion with ETA-AAS detection, The major organic forms of As in fresh marine fish, such as haddock, halibut, cod, herring, mackerel, sole, lobster, scallops and shrimp obtained through- out Canada were identified as arsenobetaine and, in shrimp only, arsenocholine.Fresh-water fish, including pike, bass, carp, pickerel, whitefish, yellow perch and striped perch, contained no arsenobetaine or arsenocholine but did contain methanol-extractable As, which was not identified. The extraction procedure included freeze drying of the tissue, Soxhlet extraction with chloroform (which was discarded) and then Soxhlet extraction with methanol. The methanolic extracts containing the organoarsenic compounds were puri- fied by alumina and ion-exchange chromatography and then subjected to reversed-phase HPLC on a 30 cm X 4.6 mm p- Bondapak CI8 column with 10% methanol in distilled water (pH adjusted to 3.5 with glacial acetic acid) as the mobile phase. The arsenobetaine levels for marine fish were 0.15- 51.8 pg g-1 (wet weight). A similar study on crab meat using HPLC - ICP-AES showed that the major water soluble form of arsenic in three species of crab was arsenobetaine (86/1331). Ebdon et al.(87/C158) presented a review on recent advances in trace metal speciation by coupled chromatography - atomic spectrometry. Couplings described included GC - FAAS, HPLC - hydride generation AAS, HPLC - UV pho- tolysis - hydride generation AAS, HPLC - atom trapping FAAS and HPLC - ICP-MS. Applications of these procedures to estuarine waters, blood serum, forensic samples, plants, oysters and sediments were described.66R JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, APRIL 1987, VOL. 2 2.4. Developments in Methodology for Atomic Absorption Spectrometry A short review on the early history of continuum source AAS was presented by Marshall et al.(87/110). The application of a microcomputer-controlled single channel spectrometer to the analysis of milk powder and single-cell protein was described. Calcium, K, Mg and Na were determined using an air - C2H2 flame whereas the graphite furnace was used for Fe. Samples were dissolved with €€NO3 - HC104 (5 + 1). The article considered the possibility of future commercial exploitation and concluded that the technique showed great promise. A 15-channel SIMAAC spectrometer was used by Carroll el al. (86/665) to determine Al, Ca, Cd, Co, Cr, Cu, Fe, K, Mg, Mn, Mo, Ni, Pb, V and Zn in bovine liver, rice flour and wheat flour using a graphite furnace atomiser. Samples were wet ashed with HN03 - H202.Tube-wall atomisation, platform atomisation and probe atomisation were compared with respect to analytical accuracy and precision. Calibration was achieved with aqueous multi-element standards. Results indicated that the probe procedure was more accurate than the other two procedures, but less precise than platform atomisa- tion methods. The probe head design has recently been improved and therefore this conclusion may not now be quite as valid (87/C182, 87/C187). 2.5. Developments in Methodology for Plasma Atomic Emission Spectrometry The determination of Ca, Fe, Mg, Mn, P and Zn in animal feeds and plant material by inductively coupled plasma atomic emission spectrometry was reported by Lyons et al. (86/661). Samples (0.5-2.0 g) were dried and ground to pass through a 1-mm sieve.Digestion was carried out in Kjeldahl flasks with concentrated H2S04 (15 ml) and 2.8 g of a catalyst mixture containing selenium powder and sodium sulphate (1 + 300). The digested solution was diluted to 250 ml with de-ionised water. Calibration was achieved by use of aqueous standards. Accuracy was confirmed by analysis of SRMs. A similar study was reported by a Chinese research group (86/C1235). In this work samples were digested with HN03 - HC104. Nebuliser blockage problems occurred when the solutions contained greater than 40 mg ml-1 of solids. Most samples were prepared to contain salt contents in the range 3-12 mg ml-1 in 10% V/V HN03. Elements studied included Al, Ca, Cd, Co, Cu, Fe, Mg, Mn, P, Pb and Zn. A Japanese research group reported the simultaneous multi-element analysis of total diet samples for major, minor and trace elements by ICP-AES (86/1720).The major elements Ca, K, Mg, Na and P were determined with a relative error of 3%. After performing matrix matching between the sample and standard solutions with respect to acidity and major element concentrations, the minor and trace elements were determined. The elements Al, Ba, Cu, Fe, Mn and Sr were determined with a relative error of 5% whereas for Cd, Co, Cr, Mo and Ni, the error was less than 20%. Recoveries of added analyte were 100 k 5% for all elements except Co and Mo. Wolnik et al. (86/1058) reported the determination of 13 trace elements in major raw agricultural crops such as carrots, corn, onions, rice, spinach and tomatoes.Cadmium and Pb were determined by differential pulse ASV whilst Ca, Cu, Fe, K, Mg, Mn, No, Na; Ni, P and Zn were determined by ICP-AES. The samples were collected from major US growing areas uncontaminated by human activities other than normal agricultural practices. The mean value for Cd in these samples was 0.024 pg g-1 wet weight (range 0.011- 0.064 pg g-1). For Pb the mean was 0.015 pg 8-1 wet weight (range 0.002-0.045 pg g-1 wet weight). 2.6. Topical Applications By far the most widely reported applications of atomic spectrometry in analyses of foods and beverages are the determinations of trace elements in milk products. The direct determination of Ca in milk powder was reported by Yin (86/1762). The non-ionic surfactant polyethyleneglycol octyl- phenyl ether (0.5%) was used to disperse the powdered milk sample prior to analysis by FAAS.The RSD was 1.0%. Samples contained 6.15-9.53 mg g-1 of Ca depending on manufacturer. Casey et al. (86/308) studied the concentrations of Cr, Cu, Mn and Zn in human milk during the first month of lactation. Zinc was determined by FAAS whereas for Cr, Cu and Mn ETA-AAS was used. Mean Zn concentrations declined from a maximum of 11.5 pg ml-1 at 2 days to 2.98 pg ml-1 at 28 days. Changes in the other three elements were irregular. The determination of Ti in milk powders by ICP-AES was reported by Van Betteray-Kortekaas (87/17). A 1-g sample was heated at 450 "C for 8-9 h and then fused with 5 g of K2S207 and dissolved in hot H2S04 (1 + 1). Recoveries of added Ti were 100-101% with an RSD of 6.2%.A method for the determination of trace and ultra-trace elements (Co, Cr, Cu, Fe, Mn, Mo and Ni) in milk by ETA-AAS was described by Mingorance and Lachica (8611092). The sample was injected directly into the graphite furnace after addition of n-octyl alcohol. Standard additions were required to obtain accurate results. Recoveries were in the region 95-107% with precisions of 6-12%. Accuracy was assessed by comparison with results obtained from a dry-ashing procedure. One way to reduce chemical interferences and possibly eliminate the need for standard additions in ETA-AAS is to use platform atomisation. Hutchinson et al. (86/1763) used the L'vov platform for the ETA-AAS determination of Cu in infant formulas. Samples were diluted with a solution of 0.5% Triton X-100.Recoveries of 96.5-101.370 were obtained for different matrix types. The over-all precision of the method ranged from 2.5 to 4.3%. Narres et al. (86/961) reported the determination of Cd and Pb in whole milk, skim milk, condensed milk and human milk by ETA-AAS. Platform atomisation, Zeeman-effect background correction and 0 2 ashing at 600 "C were used to obtain detection limits of 0.02 and 0.7 pg 1-1 for Cd and Pb, respectively. Day to day precision was 10% for 0.1 pg 1-1 of Cd and 2 pg 1-1 of Pb. A study on the determination of A1 in milk formulas and intravenous fluids by ETA-AAS was reported by McGraw et al. (86/1802). The levels of A1 reported were 94-133 pg 1-1 for infant formulas which represented a typical daily oral dose of 17-240 pg kg-1, a potentially toxic dose to an infant.Tap water contained 10-300 pg 1-1 of A1 and intravenous fluids for parenteral nutrition contained 53400 pg 1-1 of Al. The values reported for A1 are so high that there may well be a considerable contamination problem in the analysis. The other main application area was the determination of trace elements in edible oils. Trace amounts of metals in edible oils are well known to have serious deterioration effects on the stability of the oils. The altered oil characteristics are revealed in changes of colour, odour and flavours. Copper and Fe in particular reduce the oxidation stability of the oil. Ayodele (87/C177) studied three different analytical procedures for the determination of Cu, Fe, K, Na, Ni and Zn in Cassiatora seed and oil. The procedures tested were dry ashing, dilution and extraction.Dry ashing appeared to be the more sensitive and useful procedure. Extraction methods suffered from incomplete recovery due to inefficient extraction of some organometallic compounds in the oil. Copper and Fe were determined in edible oils by a 1 + 9 dilution with IBMK and then FAAS. Standards were prepared from copper diethyldi- thiocarbamate and iron diethyldithiocarbamate in IBMK instead of the traditional organometallic compounds used as standards for traces of metals in oils. The determination of Sn in edible oils and fats by ETA-AAS was reported by Mocquellet (86/91). The strongJOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, APRIL 1987, VOL. 2 67R matrix interferences which occurred when a conventional graphite furnace was used were removed by coating the atomiser surface with niobium or tantalum carbide.Both metallic carbides ensured a complete destruction of tri- glycerides without premature losses of organotin compounds. Sample preparation involved only dilution with IBMK. A detection limit of 0.3 pg 1-1 in oil was measured. Quantitative recoveries of added analyte were obtained. Other configura- tions of graphite furnace tested, including platform atomisa- tion, did not provide good results. Two other papers on the same subject reported the determination of As in edible vegetable oil (8611800) and alkali metals in olive oils (8611761). LOCATION OF REFERENCES The full references cited in this Update have been published as follows: 861C266-861709, J.Anal. At. Spectrom., 1986, 1(2), 45R-59R. 861710-8611030, J. Anal. At. Spectrom., 1986, 1(3), 75R-85R. 8611031-8611460, J . Anal. At. Spectrom., 1986, 1(4), 107R-120R. 8611461-8611834, J. Anal. At. Spectrom., 1986, 1(5), 155R-168R. 8611835-8612039, J . Anal. At. Spectrom., 1986, 1(6), 193R-200R. 8711-871395, J. Anal. At. Spectrom., 1987, 2( 1), 29R-42R. 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 86/91. At. Spectrosc., 1985, 6, 69.861195. Analyst, 1985,110,411. 861197. Analyst, 1985,110,475.861201. Analyst, 1985, 110, 619. 861303. Anal. Biochem., 1985, 148(1), 127. 861304. J. Anal. Toxicol., 1985, 9(3), 97. 861305, Forensic Sci. Int., 1985,27(3), 157.861307. Eisei Kagaku, 1985,31,37, 861308. Am. J. Clin. Nutr., 1985, 41, 1193. 861316. Sci. 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ISSN:0267-9477    

DOI:10.1039/JA987020043R

出版商:RSC    

年代:1987

数据来源: RSC

摘要:

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Belliveau, J., Cadwell, L., Joly, P., Huwel, L., Griffin, H., Laser-induced breakdown spectroscopy (LIBS) of aqueous and ceramiclglass samples at atmospheric pres- sure and in air, (Providence Coll., Providence, RI 02918, USA). Sandoval, J. E., Gilbert, T. R., Yurko, R.J., Characterisa- tion of a novel rotating disk electrode for the analysis of lubricating oils by arc emission spectroscopy, (Dept. Chem., Northeastern Univ., Boston, MA 02115, USA). Routh, M. W., Goulter, J. E., Algeo, J. D., Tikkanen, M. W., Inductively coupled plasma Fourier transform spec- trometry instrument design, (Applied Research Labora- tories, Inc., 9545 Wentworth St., Sunland, CA 91040, USA). Routh, M. W., Tikkanen, M. W., Algeo, J. D., Goulter, J. E., Inductively coupled plasma Fourier transform spec- trometry-analytical performance and possibilities, (Applied Research Laboratories, Inc., 9545 Wentworth St., Sunland, CA 91040, USA). Lyke, R. L., McGeorge, S. 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H., A thermodynamic equilibrium model for atomisation in graphite furnace atomic absorption spec- trometry, Fresenius Z . Anal. Chem., 1986, 324, 448.(Dept. Chem., Carleton Univ., Ottawa, ON KlS 5B6, Canada). Long, S. E., Browner, R. F., Influence of water on the spatial excitation behaviour of selected elements in the inductively coupled plasma, Spectrochim. Acta, Part B , 1986, 41, 639. (Sch. Chem., Georgia Inst. Technol., Atlanta, GA 30332, USA). Rayson, G. D., Hieftje, G. M., A steady-state approach to evaluation of proposed excitation mechanisms in the analytical ICP, Spectrochim. Acta, Part B , 1986, 41, 683. (Dept. Chem., Indiana Univ., Bloomington, IN 47405, USA). Hershey, J. W., Keliher, P. N., Some hydride generation interelement interference studies utilising atomic absorp- tion and inductively coupled plasma emission spec- trometry, Spectrochim. Acta, Part B, 1986, 41, 713. (Chem.Dept., Villanova Univ., Villanova, PA 19085, USA). Goldwasser, A., Mermet, J. M., Contribution of the charge-transfer process to the excitation mechanisms in inductively coupled plasma atomic emission spectroscopy, Spectrochim. Acta, Part B , 1986, 41, 725. (Fac. Cienc., Univ. Cent. Venezuela, Caracas, Venezuela). Koropchak, J. A., Winn, D. H., Thermospray interfacing for flow injection analysis with inductively coupled plasma atomic emission spectrometry, Anal. Chem., 1986, 58, 2558. (Dept. Chem. Biochem., South. Illinois Univ., Carbondale, IL 62901, USA). Pettit, W. E., Horlick, G., An automated direct sample insertion system for the inductively coupled plasma, Spectrochim. Acta, Part B , 1986, 41, 699. (Dept. Chem., Univ. Alberta, Edmonton, AB T6G 2G2, Canada).Burba, P., Willmer, P. G., Multi-element trace pre- concentration from high-purity uranium using cellulose collectors as sample pre-treatment for atomic spectroscopy (flame-AAS, ICP-OES), Fresenius 2. Anal. Chem., 1986, 323,811. (Inst. Spektrochem. Angew. Spektrosk., D-4600 Dortmund, 1 FRG).76R 871602. 871603. 871604, 871605. 871606. 871607. 871608. 871609. 871610. 87/61 1. 87/6 12, 871613. 8716 14. 871615. 871616. JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, APRIL 1987, VOL. 2 Eierman, R. J., Piepmeier, E. H., Nitrogen isotope abundance ratio determination using molecular emission spectrometry, Anal. Chem., 1986, 58, 2474. (Dept. Chem., Oregon State Univ., Corvallis, OR 97331-4003, USA). El-Defrawy, M. M., Abdallah, A. M., Mostafa, M. A., Akl, M. A., Characterisation and elimination of interfering effects in the determination of manganese by atomic absorption spectrometry, Analz.uk, 1986, 14, 306.(Fac. Sci., Univ. Mansoura, Mansoura, Egypt). Raskevich, V. K., Maiboroda, I. K., Frishberg, A. A., Panfilova, S. Ya., Lowering of detection limits for rare earth elements in steels, Zavod. Lab., 1986, 52(6), 29. (Ukr. Nauchno-Issled. Inst. Spets. Staeil, Zaporozhe, USSR). Ryspekova, Z. A., Azimova, Z. Kh., Spectrochemical determination of platinum-group metals in mineral raw material, Zavod. Lab., 1986, 52(6), 32. (Kaz. Nauchno- Issled. Miner. Syr'ra, Alma-Ata, USSR). Aubrey, L., Monroe, R., Summary report of round robin spectrographic chemical analysis, Steel Founders Res. J . , 1986, 14,31. (USA). Zhou, Z., Wu, D., Wu, X., Liang, H., Enhancement effect of complexing agents on ytterbium in an air - acetylene flame, Guangpuxue Yu Guangpu Fenxi, 1986, 6(3), 39.(Zheijiang Inst. Technol., Hangzhou, China). Chen, X., Yao, L., Determination of chromium in 11# catalyst by atomic absorption spectrophotometry, Huaxue Shiji, 1986, 8(2), 120. (Cent. Lab., Gaoquiao Petrochem. Works, Shanghai, China). Pimenov, V. G., Timonin, D. A., Shishov, V. N., Atomic emission analysis of high-purity germanium dioxide by using vapour-phase autoclave pre-concentration of impur- ity elements in the electrode, Zh. Anal. Khim., 1986, 41, 1173. (Inst. Chem., Gorkiy, USSR). Ichioka, T., Sukenobu, Y., Sumida, N., Tanaka, K., Trace analysis for phosphorus in steel by inductively coupled plasma spectrometry using organic solvent extraction, Nisshin Seiko Giho, 1986,54, 24.(Japan). Satake, M., Mehra, M. C., Nagahiro, T., Katyal, M., Microanalysis for zinc by atomic absorption after its solid phase extraction on microcrystalline naphthalene, Orient. J . Chem., 1986, 2(2), 83. (Chem. Dept. Univ. Moncton, Moncton, NB, Canada). McKenna, M., Marr, I. L., Cresser, M. S., Lam, E., The analysis of some diving gas mixtures by microwave- induced plasma optical emission spectroscopy, Spectro- chim. Acta, Part B , 1986, 41, 669. (Dept. Chem., Univ. Aberdeen, Old Aberdeen AB9 2UE, UK). Greenfield, S., Thomsen, M., Use of organic additives for the detection of refractory elements in plasma atomic fluorescence spectrometry, Spectrochim. Acta, Part B , 1986, 41, 677. (Dept. Chem., Loughborough Univ.Technol., Loughborough, Leicestershire LEll 3TU, UK). Nygaard, D. D., Sotera, J. J., Analysis of electronic-grade organic solvents by inductively coupled plasma emission spectrometry, Spectroscopy (Springfield, Oreg.) , 1986, 1(8), 42. (Allied Anal. Syst., Waltham, MA 02254, USA). Wu, S., Chakrabarti, C. L., Marcantonio, F., Headrick, K. L., Mechanisms of atomisation of molybdenum in graphite furnace atomic absorption spectrometry, Spectro- chim. Acta, Part B , 1986,41,651. (Dept. Chem., Carleton Univ., Ottawa, Ontario K1S 5B6, Canada). Carroll, J., Marshall, J., Durie, D., Littlejohn, D., Ottaway, J. M., Tube-probe atomisation in electrothermal atomic absorption spectrometry, Spectrochim. Acta, Part B , 1986, 41, 751. (Dept. Pure and Appl. Chem., Univ.Strathclyde, 295 Cathedral St., Glasgow G1 lXL, UK). 871617. 871618. 871619. 871620. 871621. 871622. 871623. 871624. 871625. 871626. 871627. 871628. 871629. Walker, Z., "Blades, M. W., Measurement of excited state level populations for atomic and ionic iron in the induc- tively coupled plasma, Spectrochim. Acta, Part B , 1986, 41, 761. (Dept. Chem., Univ. British Columbia, Van- couver, BC V6T 1Y6, Canada). Taylor, P. D. P., De Donder, J., Qualitative and semi- quantitative ICAP-AES analysis using a computer-con- trolled monochromator, Spectrochim. Acta, Part B , 1986, 41,783. (Inst. Nuclear Sci., State Univ. Ghent, Proeftuin- straat 86, B-9000 Gent, Belgium). Mai, H., Scholze, H., Atomic transport phenomena in the glow discharge source during the analysis of powders-I.Investigation of model specimens, Spectrochim. Acta, Part B, 1986,41,797. (Zentralinstitut fur Festkorperphysik und Werkstofforschung der AdW der DDR, 8027 Dresden, GDR). Nakamura, S., Kobayashi, Y., Kubota, M., Temperature of a W ribbon furnace in electrothermal atomic absorption spectrometry, Spectrochim. Acta, Part B , 1986, 41, 817. (Natl. Chem. Lab. for Industry, Yatabe, Tsukuba, Iba- raki, Japan). de Loos-Vollebregt, M. T. C., de Galan, L., van Uffelen, J. W. M., Extended range Zeeman atomic absorption spectrometry based on a 3-field a.c. magnet, Spectrochim. Acta, Part B, 1986, 41, 825. (Lab. Anal. Chem., Delft Univ. Techn., De Vries van Heystplantsoen 2, 2628 RZ Delft, The Netherlands). Aly, M. M., Analyses of the phosphate standard of the Egyptian Nuclear Materials Corp.(phosphate-1) , Spectro- chim. Acta, Part B, 1986, 41, 837. (Nuclear Materials Corp., El-Maadi Kattamiya Road, Maadi PO Box 530, Cairo, Egypt). Falk, H., Hoffmann, E., Ludke, Ch., Schmidt, K. P., Examination of direct analysis of solid plant material by FANES (furnace atomic non-thermal excitation spec- trometry), Spectrochim. Acta, Part B , 1986, 41, 853. (Zentralinstitut fiir Optik und Spektroskopie Der Akade- mie der Wissenschaften der DDR, DDR 1199 Berlin, Rudower Chaussee 5 , GDR). De Silva, K. N., Guevremont, R., A fluidised-bed sampling system for the direct introduction of solids into an inductively coupled plasma-I. Performance characteris- tics, Spectrochim. Acta, Part B , 1986, 41, 865. (Atlantic Res. Lab., Natl. Res.Council of Canada, 1411 Oxford St., Halifax, Nova Scotia B3H 321, Canada). Guevremont, R., *De Silva, K. N., A fluidised-bed sampling system for the direct introduction of solids into an inductively coupled plasma-11. Calibration and internal reference methods, Spectrochim. Acta, Part B , 1986, 41, 875. (Atlantic Res. Lab., Natl. Res. Council of Canada, 1411 Oxford St., Halifax, Nova Scotia B3H 321, Canada). Choot, E. H., *Horlick, G., Vertical spatial emission profiles in Ar - N2 mixed gas inductively coupled plasma- I, Spectrochim. Acta, Part B, 1986,41,889. (Dept. Chem., Univ. Alberta, Edmonton, Alberta T6G 2G2, Canada). Choot, E. H., *Horlick, G., Spectral characteristics of Ar - N2, Ar - 02, Ar - air and Ar - He mixed gas induc- tively coupled plasmas-11, Spectrochim.Acta, Part B , 1986, 41, 907. (Dept. Chem., Univ. Alberta, Edmonton, Alberta T6G 2G2, Canada). Choot, E. H., *Horlick, G., Evaluation of the analytical performance of mixed gas inductively coupled plasmas, Spectrochim. Acta, Part B, 1986, 41, 925. (Dept. Chem., Univ. Alberta, Edmonton, Alberta T6G 2G2, Canada). Choot, E. H., *Horlick, G., Spatially resolved electron density measurements in Ar, N2 - Ar and O2 - Ar ICPs using a photodiode array detection system, Spectrochim. Acta, Part B, 1986,41,935. (Dept. Chem., Univ. Alberta, Edmonton, Alberta T6G 2G2, Canada).JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, APRIL 1987, VOL. 2 77R 871630. 871631. 871632. 871633. Karwowska, R., Jackson, K. W., Lead atomisation in the presence of aluminium matrices by electrothermal atomic absorption spectrometry. A comparative study of slurry versus solution sample introduction, Spectrachim. Acta, Part B, 1986,41,947. (Dept. Chem., Univ. Saskatchewan, Saskatoon, Sask. S7N OWO, Canada). Turker, A. R., Dogan, M., Determination of Mo in A1203 using a d.c. arc: effects of sodium diethyldithiocarbamate as a thermochemical agent, Spectrochim. Acta, Part B , 1986,41,959. (Gazi Universitesi, Fen-Edebiyat Fakultesi, Ankara, Turkey). Wang, X., Barnes, R. M., A mathematical model for continuous hydride generation with inductively coupled plasma spectrometry analysis--I. Hydride transfer, Spec- trochim. Acta, Part B, 1986,41,967. (Dept. Chem., GRC Towers, Univ. Massachusetts, Amherst, MA 01003-0035, USA). Zicai, C., Barnes, R. M., Characterisation of a recycling nebulisation system for inductively coupled plasma spec- trometry-I. Stability and humidified argon carrier gas, Spectrochim. Acta, Part B , 1986, 41, 979. (Dept. Chem., GRC Towers, Univ. Massachusetts, Amherst, MA 01003- 0035, USA). 871634. 871635. 871636. 871637. Carnrick, G. R., Barnett, W., Slavin, W., Spectral interferences using the Zeeman effect for furnace atomic absorption spectroscopy, Spectrochim. Acta, Part B , 1986, 41, 991. (Perkin-Elmer Corporation, 901 Ethan Allen Highway, Ridgefield, CT 06877, USA). Takada, T., Some observations on relative atomisation efficiencies in the air - acetylene flame as a function of flame temperature, Spectrochim. Acta, Part B , 1986, 41, 999. (Dept. Chem., Rikkyo (St. Paul’s) Univ., Nishi- Ikebukuro, Toshima-ku, Tokyo 171, Japan). Bax, D., van Elteren, J. T., Agterdenbos, J., The determination of arsenic with hydride generation AAS. A study of the factors influencing the reactions in the absorption cuvette, Spectrochim. Acta, Part B , 1986, 41, 1007. (Analytisch Chemisch Laboratorium der Rijksu- niversiteit, Croesestraat 77A, 3522 AD Utrecht, The Netherlands). Krupa, R. J., Winefordner, J. D., Power dependencies of ICP absorption, emission and fluorescence signals for the extended sleeve torch, Spectrochim. Acta, Part B , 1986, 41, 1015. (Dept. Chem., Univ. Florida, Gainesville, FL 32611, USA).

ISSN:0267-9477    

DOI:10.1039/JA987020069R

出版商:RSC    

年代:1987

数据来源: RSC

摘要:

JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, APRIL 1987, VOL. 2 263 Atomic Spectrometry Viewpoint Richard F. Browner Division of Analytical Chemistry, Georgia Institute of Technology, Atlanta, G A 30332, USA Professor R. F. Browner was one of the Plenary Lecturers at the 1987 Winter Conference on Plasma and Laser Spectrochemistry held in Lyon in January 1987. Our Editor Judith Brew and the Chairman of the Editorial Board Les Ebdon took an opportunity to interview Rick at the meeting. Rick, can we ask you to outline your current research interests? My current research interests centre on the use of aerosols in various aspects of analytical chemistry, and this divides up both into our more traditional areas related to elemental analysis using atomic spectrometry, and more recently ICP mass spectrometry.Additionally, we also have a very active research programme in the use of aerosols for liquid chromato- graphy mass spectrometry interfacing. It is quite interesting how we have been able to focus in on the applications of aerosols for various aspects of analytical chemistry other than the ones with which we are traditionally experienced. This area of sample introduction is one that you have made very much your own. Was it a conscious decision to develop research in this area or was it something that just evolved? The impetus to get into this area was really provided during the time that I was working in London at the Laboratory of the Government Chemist, in the Atomic Spectrometry section. This was when we took delivery of an early ARL ICP optical emission system.It became obvious dur- ing the initial testing period of the instru- ment that a fundamental weakness in the whole link-up of the system related to the sample introduction process. From this we have gone on to generalise those studies to all areas of atomic spectrometry and in fact we have become very interes- ted in the fundamental aspects of aerosol generation, aerosol transport and evapor- ation mechanisms in and of themselves. Now recently that work has expanded into ICP-MS, which is of course an expensive type of instrumentation. There is a con- siderable discussion in the UK at the present time as to whether it is easier to get grants for fundamental research in the United States than it is in the UK and perhaps the rest of Europe; you yourself mentioned that you moved from the UK to the United States.You might therefore have an opinion about that? At the time that I made the decision to move back from the UK to the US, I guess the two things that were of primary interest to me were firstly, that I felt a need to get back into an academic envi- ronment, I felt that this gave me the opportunity to pursue certain lines of research that I might otherwise not have, and secondly, what the support facilities were like on the two continents. In fact certainly at that time, and we are talking about the 1975-1976 period, the funding situation in the British universities was not in a very positive mode, and I certainly felt that the opportunities for obtaining significant funding on the things that I wanted to do were in fact superior in the US at that time.I believe that this is probably a situation that continues. Although funding in the US has become tighter in many respects, the general trend remains. In fact I would estimate that it is still considerably easier to obtain signifi- cant funding in the US than it is in the UK in many areas of analytical chemistry and analytical spectroscopy. So you would advise any aspiring analy- tical atomic spectroscopist, who could, to make his career in the United States rather than in Europe? I think that it depends very much on the type of research that one is interested in. I think for anybody interested in an area of research that requires major equipment, probably it is easier to obtain funding for it in the United States.There are specific funds set aside, which if you have a strong ongoing research programme, are pos- sible to obtain. Although I do not have direct experience of the matter, from my indirect experience of research in the UK, it appears to be much more difficult to obtain funding of that type. Conse- quently, many ongoing areas of research, where the cost of the instrumentation required to do the research is high, probably do face a significant barrier in the UK at the present time. You obviously enjoy life very much in the United States although we are always pleased to see you over here in Europe. You have been extremely successful in your research and you have a beautiful and talented American wife. Now it seems that the Americans are accepting you as one of their own especially since you have just been elected as President-elect of the Society for Applied Spectroscopy.We would like to congratulate you on that election Rick, and ask you what particular plans you have as in-coming President? Well thank you very much Les for your kind remarks. I am glad that I am still welcome to visit back in Europe! I cer- tainly enjoy coming, because I feel that my roots are still located in England. I have many personal and professional friends, and its always a pleasure to come back both to visit and to exchange scien- tific ideas. In response to your other comments I think that the scientific corn- munity , certainly the atomic spectrometry scientific community, is a very interna- tional one. I feel there are very close ties internationally, and have been as long as I have been involved with the subject, particularly between the United States and Europe.I think that this has always been exemplified by the interchange of large numbers of people who travel across the Atlantic in both directions to partici- pate in the various conferences and meet- ings that take place. This is clearly a very positive thing. Obviously it is very early days in terms of my involvement with the President- elect position of the Society for Applied Spectroscopy. I think certainly that any- body in such a position is very concerned with the health and success of the profes- sion of analytical spectroscopy. To this goal I think that while one obviously would concentrate on the problems inher- ent to the particular country that one is actually living in, nonetheless the overall professional goals of all of us remain very much the same. I think that one of the things that I should certainly consider important is to improve and strengthen the ties that exist both formally and informally between the Society for264 JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, APRIL 1987, VOL. 2 Applied Spectroscopy and the equivalent that although we both work in our own groups in Europe, especially the Royal countries that we exchange ideas, person- Society of Chemistry. I think we shall nel and technical information in the best certainly make a strong effort to do what possible way. we can to set up both formal and informal means of interchanging information and Well we would certainly want to wish you develop some mechanism for ensuring all the best Rick in your term as President of the SAS and to say how much we welcome your comments about closer liai- son between the Royal Society of Che- mistry and the Society for Applied Spectro- scopy and let’s hope we can all work towards that.

ISSN:0267-9477    

DOI:10.1039/JA9870200263

出版商:RSC    

年代:1987

数据来源: RSC

摘要:

264 JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, APRIL 1987, VOL. 2 Conference Reports Analytiktreffen 1986AX CANAS: September 15thg19th, 1986, Neubrandenburg, GDR Openin ceremony: L to R, Professor Dr. Ch. Silberstein (USSR), Professor Dr. A . Hulanicki (Polan$, Professor Dr. E. PEko (Czechoslovakia), Professor Dr. K . Zimmer (Hungary), Professor Dr. G. Ackermann (GDR), Professor Dr. G . Werner (GDR) and Dr. K . Dittrich , - (GDR) “Analytiktreffen-1986-Atomic Spec- troscopy” was organised by the Karl- Marx University Leipzig, Department of Chemistry and the Chemical Society of the German Democratic Republic, Divi- sion of Analytical Atomic Spectroscopy, and was held in Neubrandenburg, GDR, in September 1986. The Chairman of the conference was Doz. Dr. sc. K. Dittrich. Since the first conference in 1974 the series of “Analy- tiktreffen” conferences have become well established.Each year the conference concentrates on a particular aspect of analytical chemistry. Analytical atomic spectrometry was the theme of the 1978, 1982 and 1986 conferences. In 1986 “Analytiktreffen” was combined with the international conference the “IX CANAS” (Conference on Analytical Atomic Spectrometry). In the past the CANAS series was organised by a num- ber of Eastern European countries. In 1986,550 scientists from universities, research institutes, health organisations and industry took part in “Analytiktreffen 198&--Atomic Spectroscopy/IX CAN- AS.” The international character of the conference was emphasised by the fact that 150 scientists from 20 countries (Aus- tria, Belgium, Bulgaria, Canada, Cuba, Czechoslovakia, Federal Republic of Germany, France, Hungary, Italy, Japan, The Netherlands, Poland, Soviet Union, Sweden, Switzerland, Syria, United King- dom, United States of America and Yugoslavia) took active parts in the con- ference.All fields of analytical atomic spectro- scopy, atomic absorption, atomic emis- sion and atomic fluorescence spec- trometry and plasma diagnostics and the analytical aspects of X-ray fluorescence were covered. The scientific programme consisted of 53 main lectures by well known scientists, 180 posters and an exhibition of scientific instruments by 20 companies both from the GDR and abroad. The organisers tried to include numer- ous discussion sessions, this being one of the most important aspects of a confer- ence.There were eight panel discussions around the main lectures, each discussion dealing with a particular theme (ETA- AAS, ICPs, etc.) Not only were the main lectures discussed, but more general topics were also covered. In addition to the main discussion sessions there were nine more general sessions around the groups of posters and nine poster meet- ings for more direct discussions with the poster presenters. Posters were displayed throughout the whole conference, for maximum effect, with the presenters present at appropriate times. Delegates were requested to make written com- ments on the posters for later discussion in the group sessions. Well-known scientists led the poster discussions and introduced topics of Neub randen b urg gatesJOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, APRIL 1987, VOL.2 interest. The organisers would like to express their thanks to the discussion chairmen for their contributions. As at all conferences there were prob- lems with the timing. The main lectures were held in two parallel sessions each morning. In the afternoons the discus- sions and poster sessions took place. All of the poster sessions and discussions were conveniently located close to the instrument exhibition. Some companies exhibiting also held manufacturers’ symposia. The main themes of the conference were: atomic absorption spectrometry with electrothermal atomisation (ETA- AAS); inductively coupled plasmas (ICP); furnace atomic non-thermal exci- tation spectrometry (FANES) and other non-thermal excitation sources; X-ray flu- orescence and ESCA spectrometry; atomic spectrometry in relation to inor- ganic mass spectrometry and X-ray flu- orescence; problems with microwave induced plasmas (MIP); and general problems of analysis and chemometrics. Other important topics included were: hydride generation for AAS; laser evap- oratiodablation for direct solid sampling; analysis of non-metals by atomic spec- trometry; trace analysis including pro- cedures of concentration and separation, especially for biological samples and the environment; atomic fluorescence spec- trometry in extreme trace analysis; and the present state of arc discharges.The following foreign scientists presen- ted lectures on ETA-AAS: Ch. L. Chak- rabarti (Ottawa, Canada); W.Frech, (UmeA, Sweden); Ch. Gilmutdinow (Kasan, USSR); I. Havezov (Sofia, Bul- garia); J. A. Holcombe (Austin, TX, USA); W. Slavin (Ridgefield, CT, USA); R. E. Sturgeon (Ottawa, Canada); V. Sychra, (Prague, Czechoslovakia); and B. L to R, G. Werner (GDR), E. M. Sedykh USSR), K. Dittrich (GDR) and K . Niebergall r GDR) post-conference sightseeing in Berlin, GDR Welz (Uberlingen, FRG) . Contributions from GDR were given by K. Dittrich (Leipzig) and H. Falk (Berlin). Important points covered by these lectures were the minimisation of systematic errors, the enhancement of sensitivity and extending the range of application. Interference effects as molecule formation (non-disso- ciation) and problems of non-specific background, and their correction, also played a particular role in the presenta- tions. Lectures on studies of the mechanisms of atomisation (Chakrabarti, Gilmutdi- now, Holcombe and Welz), of optimum thermal (Falk, Frech and Slavin) and chemical conditions (Dittrich, Havezov and Sturgeon) and of the best atomiser material (Sychra) showed how improve- ments in AAS methods can be achieved.Although ETA-AAS is only a single- element procedure, s. Caroli (Rome, Italy), K. Dittrich, H. Falk, J. Fijalkow- ski, (Warsaw, Poland), W. Frech and J. M. Ottaway (Glasgow, UK) noted in their main lectures that it is necessary to investigate new procedures for simul- taneous multi-elemental analyses of micro-samples. The hollow-cathode dis- charge (Caroli and Fijalkowski), thermal emission in hot graphite tubes (Frech and Ottaway) and non-thermal excitation with thermal evaporation in graphite tubes, FANES, (Falk) and its further development for ions and non-metals, FINES, MONES, (Dittrich and Ottaway) were developed with this aim in mind.These last methods have good prospects for the future. The importance of the ICP was con- sidered in the main lectures by J. A. C. Broekaert (Dortmund, FRG), P. W. J. M. Boumans (Eindhoven, The Nether- lands), L. de Galan (Delft, The Nether- lands), N. Krasnobaeva (Sofia, Bulgaria), J. M. Mermet (Lyon, France), Ch.1. Silberstein (Leningrad, USSR). The major problems with plasmas are connec- ted with spectral interferences (Boumans and Mermet), sample introduction (Broe- kaert) and real analysis (Krasnobaeva). Silberstein showed extremely low detec- tion limits for the AF-ICP combination.de Galan compared the ICP technique with other techniques in relation to future development in atomic spectroscopy. The main lectures of R. M. Barnes (Amherst, MA, USA), A. L. Gray (Guildford, UK), R. van Grieken (Ant- werp, Belgium), J. Jurczyk (Gliwice, Poland), B. Pavlovic (Belgrade, Yugo- slavia) and G. Ehrlich (Dresden), B. Knull (Jena), E. Kranz (Meiningen), D. Rudolph (Schkopau) from the GDR were concerned with general and specific com- parisons of analytical methods. In the future a special role will be played by the very sensitive ICP-MS technique (Barnes and Gray) and laser ablation-MS (van Grieken). In spite qf these new develop- ments some speakers (Ehrlich, Kranz, 265 Rudolph and Pavlovic) pointed out that interest in the conventional arc discharge is being revived, e.g., as a d.c.arc plasma source. Jurczyk, Knull and Petrakiev spoke about new developments in scien- tific instruments. New developments in the field of microwave-induced plasmas were discussed by P. Tschopel (Dort- mund, FRG) and B. Ramsza (Warsaw, Poland). Non-metals in particular can be determined by these methods. In many lectures practical problems of analytical chemistry and combination procedures (hydride techniques) for sepa- ration and concentration were the main theme: D. Beljanin (Moscow, USSR), E. Gegus (Veszprem, Hungary), I. Judelev- ich (Nowosibirsk, USSR), G. Knapp (Graz, Austria) P. Schramel (Neuher- berg, FRG), R. Rautschke (Halle, GDR). Because direct solid sampling is most important in analysis, it was very useful that the analytical problems associated with X-ray fluorescence and ESCA spec- trometry were included.H. K. Bothe (Leipzig, GDR), J. Jurczyk (Gliwice, Poland), A. Meisel (Leipzig, GDR), D. Mudrack (Berlin, GDR), B. Wehner (Dresden, GDR) gave some new infor- mation about the state of the art in this area. Some of the foreign delegates: L to R, R. van Grieken (Belgium), T. Kantor (Hungary), R. E. Sturgeon (Canada), L. BCzur (Hungary), J . A. Holcombe (USA) and R. M . Barnes (USA) At the end of the conference, K. Florian, M. Matherny (Kosice, Czecho- slovakia), G. Tolg (Dortmund, FRG) and K. Zimmer (Budapest, Hungary) spoke about general problems in analysis: che- mometric problems of accuracy, further developments of atomic spectrometry, trace analysis and distribution analysis by old and new principles (Tolg). These main lectures answered some of the questions posed by G.Werner (Leipzig, GDR) in his introduction on the first day of the conference. A paperback book (of about 500 pages) containing all of the main lectures will appear in the first six months of 1987 which is being prepared by the principal266 JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, APRIL 1987, VOL. 2 organisers , the Karl-Marx University Leipzig. Any enquiries about all aspects of both of these conferences can be sent to Doz. Dr. sc. K. Dittrich, Karl-Marx University Leipzig , Section Chemistry , Talstr. 35, Leipzig, 7010, GDR. The instrument exhibition demon- strated the rapid development in scientific instruments in recent years.It was very important and useful for the visitors to see most of the instruments working under practical conditions, hence the appro- priate services were supplied to accom- modate this. Most of the manufacturers were from the optical spectroscopic industry: Zeiss GDR, ARL, HGS Analy- tik, Labtest, Leybold-Heraeus, Perkin- Elmer, Philips, Shimadzu, Siemens and Spectro, FRG. Companies with specialist equipment were: Technisches Glas GDR, Berghof and Merck FRG. Some scientific institutions exhibited unique equipment, BUNA, ZOS Academy of Sciences, ASMW, Academy of Mines and Martin- Luther University, GDR. The conference also included a number of social and cultural events in the even- ings such as an organ concert in the Johannis church, choral evening, barbe- cue with music and dancing near the Tollense Sea, a trip, with dancing, on the “Mudder Schulten” boat, two chamber music concerts in the Johannis Abbey and the main evening event was the banquet in the Stadthalle with local entertainment and dancing.Most of the participants (about 500) were accommodated in the pleasant “Hotel 4 Tore ,” Neubrandenburg. This arrangement and the scientific and social sessions and events gave the opportunity for old acquaintanceships to be renewed and new friends to the made and led to many stimulating discussions. The organ- isers thank the officials of lovely Neubran- denburg, a town in the northern part of the GDR, for their hospitality. Doz. Dr. sc. K. Dittrich Conference Chairman, “Analytiktreffen 1986- A tomspektros kopiel IX CA NA S )’ ~~ 1987 Winter Conference on Plasma and Laser Spectrochemistry: January 12th-I6th, 1987, Lyon, France The successful return of the Winter Con- ference to Europe has established the viability of a European venue for a conference on atomic spectrochemistry.A survey of the list of participants reveals that over 200 delegates from 21 countries on four continents were present, which is an accurate reflection on the international nature of the meeting. The conference was held at the Mapotel Best Western in Lyon with the majority of the delegates staying on site. This proved a most expedient choice not only in establishing a social base for the confer- ence but also in reducing the amount of travel required, no small consideration with sub-zero temperatures and substan- tial snowfalls the order of the day.The scientific programme was built around an impressive array of plenary lectures, which, together with a few con- tributed papers, occupied all day Monday and the Tuesday, Wednesday and Friday morning sessions. This format provided a comprehensive state-of-the-art review of plasma and laser spectrochemistry, start- ing on Monday with Dr. P. W. J. M. Boumans’ opening address on the com- pilation of a comprehensive ICP spectral atlas and moving on to include sample introduction, novel atom sources, detec- tion system and data treatment and end- ing with automation. The majority of submitted contribu- tions were presented as posters, the ses- sions occupying Wednesday afternoon and the whole of Thursday.Poster ses- sions play an imporant part in modern conferences. They provide a forum for the young researcher and are equally useful for those intimidated by the prospect of addressing a large audience. It is gratify- ing then to report that the standard was high with evidence that increasing care is being given to the artwork and to improve the over-all presentation. Perhaps this was to some extent stimulated by the competition for the best presented poster sponsored by Philips. This covered the three sessions and resulted in runners-up prizes for: A. G. Cox and C. W. McLeod of Sheffield City Polytechnic in conjunc- tion with D. L. Miles and J. M. Cook of the British Geological Survey; R. Garav- aglia of CISE, Italy; and C. Bergey, J. C. Birolleau and F. Thouzeau of CEA in conjunction with R.C. Durr of ESI Durr, France. The over-all winner however was J. W. M. Kocken of the University of Utrecht, The Netherlands, whose poster concerned computer enhancement of simultaneous multi-element analysis by ICP emission spectrometry. Dr. Boumans announced the winners at the banquet on the last evening, in the form of a very entertaining rhyme, which kept everyone guessing as to the nationality of the winner until the last verse. He explained how the competition had been judged as follows: A seven members jury has made up its mind. You will wonder about the judgement they could find. A heavy task was on their fourteen shoulders: To see ninety posters and the poster holders. We gave credit points for presentation, And assessed transfer of information.The essential content was beyond the competition, And the jury had a balanced international composition. Time was also found on Tuesday after- noon for a series of seminars held by the L to R: Dominic Spillane, Stephen Long, John Dean, Katherine Timmins and Peter Allenby enjoying ARL’s hospitality L to R: Mike Blades, Alan Gray and Don Douglas at the opening of the exhibitionJOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, APRIL 1987, VOL. 2 267 manufacturers and an instrument exhibi- tion was open for much of the week. The contents of the scientific pro- gramme indicate the healthy state of plasma spectrochemistry today. The importance of theoretical studies was highlighted in an excellent plenary lecture by Professor M. Blades. The growing use of flow injection techniques for speciation purposes was underlined by a plenary from Dr.C. W. McLeod and a number of other interesting submissions. Laser tech- niques were explored in many of the oral and poster presentations and are clearly going to be of continuing usefulness par- ticularly for plasma diagnostics. The use of Fourier transform spectrometers was tion, but probably the most striking feature of the conference was the growth in importance of ICP-MS with two ple- naries, a number of oral presentations and a large number of posters being presented on the topic. The technique certainly seems to have “come of age” with contri- butions now coming from industrial users in addition to those from the academic research groups and manufacturers. On the social side, the sponsoring manufacturers arranged a number of evening functions throughout the week. The weather was generally too severe to encourage an extended absence from the hotel although those who braved the elements were impressed by Lyon (and its many restaurants!). Highlight of the week was undoubtedly the conference dinner at the Chateau Pizay, a medieval banquet complete with minstrels, during the course of which your author found himself in a metal cage with a bag over his head. Why? I’m still at a loss, but for that sight as well as for the rest of an entertaining organising committee in particular Jean- Michel Mermet, Eric Janssens and Nick Omenetto. Dominic Spillane Department of Applied Chemistry and Life Sciences, Polytechnic of North London, UK Jean-Michel Mermet cutting the spectacular and instructive week we have to thank the dessert at the banquet-the Piece Montte also covered with a plenary lecture by Dr. L. Faires and a number of other contribu- tors. Other topics included were the use Gary Horlick ( L ) and Gary Hiefje in earnest of glow discharge sources, furnace atom- discussion isers and automation in sample prepara-

ISSN:0267-9477    

DOI:10.1039/JA9870200264

出版商:RSC    

年代:1987

数据来源: RSC

摘要:

JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, APRIL 1987, VOL. 2 267 Conferences and Meetings Third Italo-Hungarian Symposium on Spectrochemistry: Biomedical Research and Spec troc hemis t r y June 0-12, 1987, Ispra (Varese), Italy All enquiries about the scientific pro- gramme or attendance at the Symposium should be addressed directly to: S. Caroli, Laboratorio di Tossicologa Applicata, Istituto Superiore di Sanith, Viale Regina Elena 299, 00161 Rome, Italy. XXV Colloquium Spectroscopicum Inter- nationale June 21-26, 1987, Toronto, Canada Pre and Post CSI Symposia: Line Spectra of the Elements June 19-21, 1987, Scarborough, Ontario Graphite Furnace Atomic Absorption June 20-July 2, 1987, Huntsville, Ontario Inductively Coupled Plasma Mass Spec- troscopy June 20-30, 1987, Lake Muskoka, Ontario For any further information, including registration, contact Mr.L. Forget, Con- ference Services Office, National Research Council Canada, Ottawa, Ontario K1A OR6, Canada.268 JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, APRIL 1987, VOL. 2 Second Surrey Conference on Plasma Source Mass Spectrometry July 6-8, 1987, Guildford, Surrey, UK This is an advance notice of the Second Surrey Conference, Short Course and Workshop. Further details are available from Dr. A. L. Gray, Department of Chemistry, University of Surrey, Guild- ford, Surrey GU2 5XH, UK. Spectroscopy Across the Spectrum; Analytical Applications of Spectroscopy July 12-15, 1987, Norwich, UK The Conference (incorporating The First International Near Infrared Spectroscopy Conference) will be held at the University of East Anglia, Norwich.The aim of the meeting is to bring together spectrosco- pists from many different disciplines with the prospect of an interchange of ideas and methods. The meeting will be organ- ised into: general, poster and parallel specialist sessions, with an equipment exhibition and social programme. Plenary lectures will be presented by: K. H. Norris (USA); J. G. Grasselli (USA); D. Games (UK); L. Ebdon (UK); A. A. Fell (UK); P. Griffiths (USA); N. Sheppard (UK); M. L. Gross (USA); W. F. McClure (USA); A. Thorne (UK); C. L. Wilkins (USA); H. J. H. MacFie (UK); E. W. Stark (USA); and J. F. Tyson (UK). The plenary and keynote lectures will cover the areas of: combined techniques, data analysis and Fourier transform spectroscopy. Parallel sessions are planned in the following areas: near IR, atomic absorption, mass, NMR, microwave and IR spectroscopy, process control and chemometrics. Poster contributions are invited in these areas.For further information contact Dr. C. S. Creaser, School of Chemical Sciences, University of East Anglia, Norwich NR4 7TJ, UK. 29th Rocky Mountain Conference August 2-6, 1987, Denver, CO, USA The 29th Rocky Mountain Conference will be held at the Radison Hotel, Denver. The keynote speakers for the atomic spectroscopy symposium are Stan Crouch (Michigan State University) who will speak on laser ionisation in flames and Mike Blades (University of British Columbia) who will speak on excitation mechanisms in the ICP. There will also be a symposium on ICP-MS.As in previous years an outing is planned for the day after the symposium. For further information on the atomic spectroscopy symposium contact Dr. T. M. Niemczyk, University of New Mexico,. Department of Chemistry, Clark Hall 103, Albuquerque, NM 87131, USA. For general information of the confer- ence contact Carol Giles, Rockwell Inter- national, General Lab. Bldg. 881, P.O. Box 464, Golden, CO 80401, USA. 1988 Winter Conference on Plasma Spec- trochemistry January 3-9, 1988, San Diego, CA, USA Papers describing original work with plasma spectrochemical applications, fun- damentals and novel instrumentation developments are solicited for the 1988 Winter Conference on Plasma Spectro- chemistry to be held at the San Diego Princess resort and Convention Center in San Diego, California. Titles and 50-word abstracts should be received by July 2, 1987 and for accepted papers, full abstracts are due October 2, 1987.Manu- scripts for publication (after peer review) in the special issue of the Journal of Analytical Atomic Spectrometry are requested by January 1988. Sponsored by the ICP Information Newsletter this, the fifth in a series of biennial meetings, will feature develop- ments in plasma spectrochemical analysis as performed with inductively coupled plasma, d.c. plasma, microwave plasma or glow and hollow cathode discharge sources. Ten symposia organised and chaired by recognised experts will be presented in lecture and poster sessions, along with six plenary and 15 invited lectures. Thirty expert short courses will be taught at introductory and advanced levels. A three-day exhibition of spectro- scopic instrumentation and chemicals, electronics, glassware, publications and software supporting plasma spectroscopy will be held in conjunction with the scheduled sessions. For details, contact Dr. Ramon M. Barnes, Conference Chairman, Depart- ment of Chemistry, GRC Towers, Uni- versity of Massachusetts, Amherst, MA 01003-0035, USA.

ISSN:0267-9477    

DOI:10.1039/JA987020267b

出版商:RSC    

年代:1987

数据来源: RSC

摘要:

268 JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, APRIL 1987, VOL. 2 Future Issues will lnclude- Peak-area Measurements in Electrother- mal Atomisation Inductively Coupled Plasma Atomic Emission Spectrometry- J. Alvarado, P. Cavalli, N. Omenetto, G. Rossi and (the late) J. M. Ottaway Use of a Thermospray Nebuliser as a Sample Introduction System for Induc- tively Coupled Plasma Atomic Emission Spectrometry (ICP-AES)-K. A. Ver- meiren, P. D. P. Taylor and R. Dams Fluoride Interference on the Boron ICP Atomic Emission in Methanolic Solu- tions-A. Canals and V. Hernandis Selection of Mode for the Measurement of Lead Isotope Ratios by Inductively Coupled Plasma Mass Spectrometry and its Application to Milk Powder Analysis -J. R. Dean, R. Massey and L. Ebdon Atomic Absorption Spectrometric Method for the Determination of Phos- phorus Using Bismuth - Phosphornolyb- date Complex-P.K. Gupta and R. Ramchandran An Evaluation of the Grid-type Nebuliser for Organic Solvent Introduction to the ICP-Timothy Brotherton, Barbara Barnes, Nohora Vela and Joseph Caruso Spectral and Physical Interferences in a New Flexible Inductively Coupled Plasma Mass Spectrometry Instrument-Daniel A. Wilson, George H. Vickers and Gary M. Hieftje On-line Sequential Detection by Induc- tively Coupled Plasma Spectrometry of Trace Elements After Liquid Chromato- graphy of Biological Fluids-P. E. Gardiner, P. Braetter, B. Gerken and A. Tomiak K and L Shell X-ray Relative Intensity Measurement&. Bhan, A. Rani, S. N. Chaturvedi and N. Nath Direct Determination of Cadmium in Soil Slurries by Microsampling Cup Atomic Absorption Spectrometry-G. Rygh and K. W. Jackson Development of Hollow-cathode Radia- tion Sources. Part l. Study of the Effects of Cones Placed in the Cathode Cavity on the Emitted Light Intensity-L. Papp and L. Racz Development of Hollow-cathode Radia- tion Sources. Part 2. Study of the Effect of a Cylinder Placed in the Cathode Cavity on the Emitted Light Intensity-L. Papp Optimisation of the Analytical Condi- tions for the Determination of A1 in Human Blood Plasma and Serum by GFAAS. Part 2. Assessment of the Analytical Method-P. E. Gardiner and M. Stoeppler Atomic Spectrometry Update The Update in the June issue is-Instrumentation- John Marshall, Stephen J. Haswell and Stephen J. Hill

ISSN:0267-9477    

DOI:10.1039/JA9870200268

出版商:RSC    

年代:1987

数据来源: RSC