摘要:

Journal of Analytical Atomic Spectrometry (Including Atomic Spectrometry Updates - Formerly ARAAS) JAAS Editorial Board* Chairman: J. M. Ottaway (Glasgow, UK) J. Brew (London, UK) M. S. Cresser (Aberdeen, UK) L. C. Ebdon (Plymouth, 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. A d a m (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 (Umed, Sweden) K. Fuwa (Tokyo, Japan) A. L. Gray (Guildford, UK) S.Greenfield (Loughborough, UK) G. M. Hieftje (Bloomington, IN, USA) G. Horlick (Edmonton, Canada) J. J. LaBrecque (Caracas, Venezuela) J. M. Mermet (Villeurbanne, France) Ni Zhe-ming (Beijing, China) N. Omenetto (lspra, Italy) E. Pl5ko (Bratislava, Czechoslovakia) R. Sturgeon (Ottawa, Canada) 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) *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) H. Hughes (Anglesey, UK) P. N. Keliher (Villanova, PA, USA) K. Kitagawa (Nagoya, Japan) C. W. McLeod (Sheffield, UK) K. W. Jackson (Saskatoon, Canada) F. J. M. J. Maessen (Amsterdam, The Nether- *D. Littlejohn (Glasgow, UK) lands) *J. Marshall (Middlesbrough, UK) J. M. Mermet (Villeurbanne, France) E. Norval (Pretoria, South Africa) I. Novotny (Bmo, 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) *B. L. Sharp (Aberdeen, UK) W. Slavin (Norwalk, CT, USA) R. D. Snook (London, UK) R. Stephens (Halifax, Canada) J. Stupar (Ljubljana, Yugoslavia) A.Taylor (Guildford, UK) M. Thompson (London, UK) *A. M. Ure,(Aberdeen, UK) B. Welz (Uberlingen, FRG) J. B. Willis (Victoria, Australia) *D. L. Miles (Wallingford, UK) *J. M. Ottaway (Glasgow, UK) *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 W1V OBN. Telephone 01-437 8656. Telex No. 268001 Journal ofAnalytical Atomic Spectrometry (JAASI (ISSN 0267-9477) is published bimonthly by The Royal Society of Chemistry, Burlington House, London W1V OBN, UK.All orders accompanied with payment should be sent directly to The Royal Society of Chemistry, The Distribution Centre, Blackhorse Road, Letchworth, Herts. SG6 1HN. UK. 1986 Annual subscription rate UK f165.00, Rest of World €182.00, USA $319.00. Air freight and mailing in the USA by Publications Expediting Inc., 200 Meacham Avenue, Elmont, NY 11003. USA Postmaster: send address changes to Journal o f 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, 1986. 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. nformation for Authors :uII details of how to submit material for )ublication in JAASare given in the Instructions o Authors in Issue 1. Separate copies are ivailable on request. The Journal of Analytical Atomic Spectrometry JAAS) is an international journal for the publi- :ation of original research papers, short papers, :ommunications and letters concerned with the levelopment and analytical application of itomic spectrometric techniques.The journal Nil1 be published bimonthly, will include com- Jrehensive reviews of specific topics of interest :o practising atomic spectroscopists and will ncorporate the literature reviews which were previously published in Annual Reports on Analytical 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- enceiemission 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- Full papers, describing original work. Short papers, also describing original work, but of limited breadth of subject matter.Communications, which must be on an urgent matter and be of obvious scientific importance. Communications should not be simple claims for priority: this facility for rapid publication is 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: sidered. Editor, JAAS Judith Brew The Royal Society of Chemistry, Burlington House, Piccadilly, London W1V OBN, UK US Associate Editor, JAAS Dr. J. M. Harnly US Department of Agriculture, Beltsville Human Nutrition Research Center, 8LDG 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). MembersoftheJAASEditorial 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 of each published contribution are supplied free of charge.Journal of Analytical Atomic Spectrometry (Including Atomic Spectrometry Updates - Formerly ARAAS) JAAS Editorial Board* Chairman: J. M. Ottaway (Glasgow, UK) J. Brew (London, UK) M. S. Cresser (Aberdeen, UK) L. C. Ebdon (Plymouth, 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. A d a m (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 (Umed, Sweden) K. Fuwa (Tokyo, Japan) A. L. Gray (Guildford, UK) S. Greenfield (Loughborough, UK) G. M. Hieftje (Bloomington, IN, USA) G. Horlick (Edmonton, Canada) J. J. LaBrecque (Caracas, Venezuela) J. M. Mermet (Villeurbanne, France) Ni Zhe-ming (Beijing, China) N. Omenetto (lspra, Italy) E. Pl5ko (Bratislava, Czechoslovakia) R. Sturgeon (Ottawa, Canada) 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) *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) H. Hughes (Anglesey, UK) P. N. Keliher (Villanova, PA, USA) K. Kitagawa (Nagoya, Japan) C. W. McLeod (Sheffield, UK) K. W. Jackson (Saskatoon, Canada) F. J. M. J. Maessen (Amsterdam, The Nether- *D. Littlejohn (Glasgow, UK) lands) *J. Marshall (Middlesbrough, UK) J. M. Mermet (Villeurbanne, France) E. Norval (Pretoria, South Africa) I. Novotny (Bmo, 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) *B.L. Sharp (Aberdeen, UK) W. Slavin (Norwalk, CT, USA) R. D. Snook (London, UK) R. Stephens (Halifax, Canada) J. Stupar (Ljubljana, Yugoslavia) A. Taylor (Guildford, UK) M. Thompson (London, UK) *A. M. Ure,(Aberdeen, UK) B. Welz (Uberlingen, FRG) J. B. Willis (Victoria, Australia) *D. L. Miles (Wallingford, UK) *J. M. Ottaway (Glasgow, UK) *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 W1V OBN.Telephone 01-437 8656. Telex No. 268001 Journal ofAnalytical Atomic Spectrometry (JAASI (ISSN 0267-9477) is published bimonthly by The Royal Society of Chemistry, Burlington House, London W1V OBN, UK. All orders accompanied with payment should be sent directly to The Royal Society of Chemistry, The Distribution Centre, Blackhorse Road, Letchworth, Herts. SG6 1HN. UK. 1986 Annual subscription rate UK f165.00, Rest of World €182.00, USA $319.00. Air freight and mailing in the USA by Publications Expediting Inc., 200 Meacham Avenue, Elmont, NY 11003. USA Postmaster: send address changes to Journal o f 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, 1986. 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. nformation for Authors :uII details of how to submit material for )ublication in JAASare given in the Instructions o Authors in Issue 1. Separate copies are ivailable on request. The Journal of Analytical Atomic Spectrometry JAAS) is an international journal for the publi- :ation of original research papers, short papers, :ommunications and letters concerned with the levelopment and analytical application of itomic spectrometric techniques.The journal Nil1 be published bimonthly, will include com- Jrehensive reviews of specific topics of interest :o practising atomic spectroscopists and will ncorporate the literature reviews which were previously published in Annual Reports on Analytical 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- enceiemission 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- Full papers, describing original work. Short papers, also describing original work, but of limited breadth of subject matter. Communications, which must be on an urgent matter and be of obvious scientific importance. Communications should not be simple claims for priority: this facility for rapid publication is 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: sidered. Editor, JAAS Judith Brew The Royal Society of Chemistry, Burlington House, Piccadilly, London W1V OBN, UK US Associate Editor, JAAS Dr. J. M. Harnly US Department of Agriculture, Beltsville Human Nutrition Research Center, 8LDG 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). MembersoftheJAASEditorial 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 of each published contribution are supplied free of charge.

ISSN:0267-9477    

DOI:10.1039/JA98601FX021

出版商:RSC    

年代:1986

数据来源: RSC

摘要:

JASPE2 l(6) 401-488,169R-200R (1986) December 1986 Journal of Analytical Atomic Spectrometry Including Atomic Spectrometry Updates CONTENTS NEWS AND VIEWS 401 Atomic Spectrometry Viewpoint-Jean-MicheI Mermet 401 Obituary-John M. Ottaway 403 406 Conference Reports 407 ASU Highlights-David Hickman 408 Book Review-J. C. Riviere 408 Conferences and Meetings 410 Papers in Future Issues The Evolution of the ICP as an Ion Source for Mass Spectrometry -Alan L. Gray PAPERS 41 1 421 429 433 437 443 449 453 457 461 467 473 479 484 485 Applications of Spark-source Mass Spectrometry in the Analysis of Semiconductor Materials. A Review-Jozef Verlinden, Renaat Gijbels, Freddy Adams Determination of Phosphorus by Graphite Furnace Atomic Absorption Spectrometry. Part 1. Determination in the Absence of a Modifier-Adilson J.Curtius, Gerhard Schlemmer, Bernhard Welz Determination of Trace Amounts of Nickel and Cobalt in Silicate Rocks by Graphite Furnace Atomic Absorption Spectrometry: Elimination of Matrix Effects with an Ammonium Fluoride Modifier-Rokuro Kuroda, Toshihiko Nakano, Yasuharu Miura, Koichi Oguma Rapid Screening Method for the Determination of Platinum and Palladium in Geological Materials by Batch Ion-exchange Chromatography and Graphite Furnace Atomic Absorption Spectrometry-Charles H. Branch, Dawn Hutchison Determination of Silicon in Gallium Arsenide by Electrothermal Atomisation Atomic Absorption Spectrometry Using the L'vov Platform-Marco Taddia Analyses of Solid Samples by Graphite Furnace Atomic Absorption Spectrometry Using Zeeman Background Correction-Glen R.Carnrick, Barbara K. Lumas, William 6. Barnett Effects of Ageing of Pyrolytically Coated Tubes on the Determination of Refractory Elements by Electrothermal Atomisation Atomic Absorption Spectrometry-M ichel Hoenig, Frank Dehairs, Ann-Marie de Kersabiec Direct Microcomputer Controlled Determination of Zinc in Human Serum by Flow Injection Atomic Absorption Spectrometry-Kirsten Wiese Simonsen, Brent Nielsen, Arne Jensen, Jan Rud Andersen Determination of Iron by Atomic Absorption Spectrometry after Synergistic Extraction of the Iron(ll1) - 5,5'-Methylenedisalicylohydroxamate - Tributyl Phosphate Complex- Fermin Capitan, Doming0 Gazquez, Mercedes Sanchez, Luis Fermin Capitan-Vallvey A Study of the Formation of Atoms and Dry Aerosols Above a Graphite Rod Sample Introduction Device Used for Inductively Coupled Plasma Atomic Emission Spec- trometry-John R.Dean, Richard D. Snook Silicate Rock Analysis by Energy-dispersive X-ray Fluorescence Using a Cobalt Anode X-ray Tube. Part 1. Optimisation of Excitation Conditions for Chromium, Vanadium, Barium and the Major Elements-Philip J. Potts, Peter C. Webb, John S. Watson Determination of Tin by Non-dispersive Atomic Fluorescence Spectrometry Coupled with a Hydride Generation Technique-Taketoshi Nakahara, Tamotsu Wasa Simultaneous Detection of Alkylselenide, Alkyllead and Alkyltin Compounds by Gas Chromatography Using a Multi-channel Non-dispersive Atomic Fluorescence Spec- trometric Detector and Miniature Flame as Atomiser-Alessandro D'Ulivo, Paolo Papoff ERRATA Flame Atomic Emission Spectrometric Determination of Boron in Methanolic Solu- tions: Influence of Fluoride on the Solute Transport Efficiency-A.Canals, Vicente Hernandis, J. V. Sala COMM U NlCATlON Background Atomic Absorption in Graphite Furnace Atomic Absorption Spectrometry -Lindesay R. Macdonald, Thomas C. O'Haver, Barbara J. Ottaway, (the late) John M. Ottaway ATOMIC SPECTROMETRY UPDATE 169R 193R References Minerals and Refractories-David A. Hickman, Joan M. Rooke, Michael Thompson Typeset and printed by Heffers Printers Ltd, Cambridge, EnglandJASPE2 l(6) 401-488,169R-200R (1986) December 1986 Journal of Analytical Atomic Spectrometry Including Atomic Spectrometry Updates CONTENTS NEWS AND VIEWS 401 Atomic Spectrometry Viewpoint-Jean-MicheI Mermet 401 Obituary-John M.Ottaway 403 406 Conference Reports 407 ASU Highlights-David Hickman 408 Book Review-J. C. Riviere 408 Conferences and Meetings 410 Papers in Future Issues The Evolution of the ICP as an Ion Source for Mass Spectrometry -Alan L. Gray PAPERS 41 1 421 429 433 437 443 449 453 457 461 467 473 479 484 485 Applications of Spark-source Mass Spectrometry in the Analysis of Semiconductor Materials. A Review-Jozef Verlinden, Renaat Gijbels, Freddy Adams Determination of Phosphorus by Graphite Furnace Atomic Absorption Spectrometry. Part 1. Determination in the Absence of a Modifier-Adilson J. Curtius, Gerhard Schlemmer, Bernhard Welz Determination of Trace Amounts of Nickel and Cobalt in Silicate Rocks by Graphite Furnace Atomic Absorption Spectrometry: Elimination of Matrix Effects with an Ammonium Fluoride Modifier-Rokuro Kuroda, Toshihiko Nakano, Yasuharu Miura, Koichi Oguma Rapid Screening Method for the Determination of Platinum and Palladium in Geological Materials by Batch Ion-exchange Chromatography and Graphite Furnace Atomic Absorption Spectrometry-Charles H.Branch, Dawn Hutchison Determination of Silicon in Gallium Arsenide by Electrothermal Atomisation Atomic Absorption Spectrometry Using the L'vov Platform-Marco Taddia Analyses of Solid Samples by Graphite Furnace Atomic Absorption Spectrometry Using Zeeman Background Correction-Glen R. Carnrick, Barbara K. Lumas, William 6. Barnett Effects of Ageing of Pyrolytically Coated Tubes on the Determination of Refractory Elements by Electrothermal Atomisation Atomic Absorption Spectrometry-M ichel Hoenig, Frank Dehairs, Ann-Marie de Kersabiec Direct Microcomputer Controlled Determination of Zinc in Human Serum by Flow Injection Atomic Absorption Spectrometry-Kirsten Wiese Simonsen, Brent Nielsen, Arne Jensen, Jan Rud Andersen Determination of Iron by Atomic Absorption Spectrometry after Synergistic Extraction of the Iron(ll1) - 5,5'-Methylenedisalicylohydroxamate - Tributyl Phosphate Complex- Fermin Capitan, Doming0 Gazquez, Mercedes Sanchez, Luis Fermin Capitan-Vallvey A Study of the Formation of Atoms and Dry Aerosols Above a Graphite Rod Sample Introduction Device Used for Inductively Coupled Plasma Atomic Emission Spec- trometry-John R.Dean, Richard D. Snook Silicate Rock Analysis by Energy-dispersive X-ray Fluorescence Using a Cobalt Anode X-ray Tube.Part 1. Optimisation of Excitation Conditions for Chromium, Vanadium, Barium and the Major Elements-Philip J. Potts, Peter C. Webb, John S. Watson Determination of Tin by Non-dispersive Atomic Fluorescence Spectrometry Coupled with a Hydride Generation Technique-Taketoshi Nakahara, Tamotsu Wasa Simultaneous Detection of Alkylselenide, Alkyllead and Alkyltin Compounds by Gas Chromatography Using a Multi-channel Non-dispersive Atomic Fluorescence Spec- trometric Detector and Miniature Flame as Atomiser-Alessandro D'Ulivo, Paolo Papoff ERRATA Flame Atomic Emission Spectrometric Determination of Boron in Methanolic Solu- tions: Influence of Fluoride on the Solute Transport Efficiency-A. Canals, Vicente Hernandis, J. V. Sala COMM U NlCATlON Background Atomic Absorption in Graphite Furnace Atomic Absorption Spectrometry -Lindesay R. Macdonald, Thomas C. O'Haver, Barbara J. Ottaway, (the late) John M. Ottaway ATOMIC SPECTROMETRY UPDATE 169R 193R References Minerals and Refractories-David A. Hickman, Joan M. Rooke, Michael Thompson Typeset and printed by Heffers Printers Ltd, Cambridge, England

ISSN:0267-9477    

DOI:10.1039/JA98601BX023

出版商:RSC    

年代:1986

数据来源: RSC

摘要:

iv JOURNAL OF MICRONUTRIENT AN A LY SI S Editors Robert Macrae, University of Reading, UK Gary R. Beecher, Beltsville, Human Nutrition Centre, Maryland, USA Richard C. Rose, The Pennsylvania State University, Hershey, USA. The Journal of Micronutrient Analysis covers all methods for the detection and determination of micronutrients and their metabolites at a l l stages within the food chain. The term micronutrient is used to describe all minor food components known, or suspected, to have a nutritional role in man and other vertebrates. Topics include: methods intended for animal feeds, raw foodstuffs and clinical samples (blood, urine, tissue, etc.) developments of methods, application to specific areas and the interpretation of the significance of results. evaluation of techniques by comparison with alternative methods.* results of collaborative trials. Results of the application of standard methods of analysis will only be published where the interpretation of the data provides a significant contribution to our knowledge of the levels of micronutrients in important fields where such knowledge i s lacking. Nutritional papersper se will not be accepted. SUBSCRIPTION INFORMATION Volume 3 (1987) 4 issues Price: €65.00 - UK delivery; €72.00/US$119.00 - outside UK delivery. Subscriptions to all countries are airspeeded at no extra cost t o the subscriber. f sterling price is definitive. US$ price can be subject to exchange rate fluctuations. (ISSN: 0266-349X) SEND FOR A FREE SPECIMEN COPY Edited by R.E. Hester University of York The aim of this book is to provide a wide-ranging and authoritative coverage of topics which are fundamental to our understanding and appreciation of the nature of our environment.The six chapters are all written by authors who are acknowledged experts in their particular fields, with the intention of providing a sufficient depth of treament to satisfy the needs of serious students of the subject matter but in a style and level which will be found comprehensible and interesting by the generally concerned, involved, and educated layman. This is not primarily a book for the expert who already is well informed and engaged actively in environmental chemistry, although the broad range of its coverage undoubtedly will have some appeal for such experts. Rather it is aimed at students, at managers in industry, administrators, politicians, legislators, and other people with a concern for the quality of our environment and a need to understand the issues involved in its management.Brief Contents Monitoring By C N Hewitt, University of Lancaster and R M Harrison, University of Essex The Air by A G Clarke, University of Leeds Water by H fish, Natural Environment Research Council Land Contamination and Reclamation By E E Finnecy and K W Pearce, Harwell Laboratory Assessing the Ecological and Health Effects of Pollution by S Smith, King 's College, London Regulation and the Economics of Pollution Control by P Burrows, N Highton, University of York and A I Ogus, University of Newcastle upon Tyne Appendix: Information Retrieval by M L Richardson Hardcover 348pp ISBN 0 85186 907 6 Price f42.50 ($77.00) RSC Members €1 7.50 RSC Members are entitled to a 20% discount on bulk orders of 15 or more copies.Ordering : Non-RSC Members should send their orders to: The Royal Society of Chemistry, Distribution Centre, Blackhorse Road, Letchworth, Herts SG6 1 HN, UK. RSC Members should send their orders to: The Royal Society of Chemistry, Membership Manager, 30 Russell Square, London WCl B 5DT, UK. ROYAL SOCIETY OF CHEMISTRY Information ervices11 ARL QUALITY AND RELIABILITY AT WICE THE SPEED The 84OOt XRF spectrometer series - now more flexible, faster ... ARL, world leader in simultaneous XRF spectrometry, now introduces significant improvements to its sequential XRF spectrometers, setting new standards of performance and flexibility for routine and non- routine analyses.ARL quality Major features of the 8400t XRF series include: Proven thin-end window Rh anode tube for efficient X-ray excita- tion. Single or dual goniometers, the latter doubling the programme of collimators crystals and detectors for more optimum measurement and further halving the analytical time. Advanced software packages covering every analytical need, in- cluding a new investigative software and the possibility to link to central laboratory computer systems. Comprehensive sample handling and automation systems. ARL flexibility A unique user-orientated modular configuration permits the addition of further automation components as they are needed, thus increas- ing analytical capabilities in line with user requirements. We can pro- vide the instrument you need.ARL support ARL’s worldwide after-sales support network means there is an ARL team near you ready to assist with any analytical problems you may have. To find out more, contact your nearest ARL office, or write to the address below. ARL -i~mmmmm=mm APPLIED RESEARCH LABORATORIES En Vallaire CH-1024 ECUBLENS / Switzerland. Tel. (021) 34 97 01 Other offices and representatives are located throughout the world.... 1ll Ramon M. Barnes, Editor Department of Chemistry GRC Towers U n ive rsi t y of Massachusetts Amherst, MA 01003-0035 lei. (413) 545-2294 Objective The ICP lnformation Newsletter is a monthly journal published by the Plasma Research Group at the University of Massachu- setts and is devoted exclusively to the rapid and impartial dissem- ination of news and literature information related to the devel- opment and applications of plasma sources for spectrochemical analysis. Background ICP stands for inductively coupled plasma discharge, which dur- ing the past decade has become the leading spectrochemical excitation source for atomic emission spectroscopy.ICP sources are also applied commercially as an atom and ion cell in atomic fluorescence spectrometry and as an ion source for mass spec- trometry. The popularity of this source and the need to collect in a single literature reference all of the pertinent data on ICP stimulated the publication onhe ICP lnformation Newsletter in 1975. Other plasma sources, such as microwave induced plas- mas and direct current plasma jets, have also grown in popularity and are included in the scope of the ICP lnformation Newsletter. scope As the only authoritative monthly journal of its type, the ICP Information Newsletter is read in more than 40 countries by scientists actively applying or planning to use the ICP or other types of plasma spectroscopy.For the novice in the field, the ICP Information Newsletter provides a concise and systema- tic source of information and background material needed for the selection of instrumentation or the development of new meth- od olog y . Edltorial The ICP lnformation Newsletter is edited by Dr. Ramon M. Barnes, Professor of Chemistry, University of Massachusetts at Amherst, with the assistance of a 20-member Board of National Correspondents composed of leading plasma spectroscopists. The Board members from around the world report news, view- points, and developments.Dr. Barnes has been conducting plasma research on ICP and other discharges since 1968. He also serves as chairman of the Winter Conferences on Plasma Spect rochem istry. Regular Features @Original submitted and invited research articles by ICP and plasma experts. Complete bibliography of all major ICP publications from 1961 to the present. Abstracts of all ICP papers presented at major US and interna- tional meetings. .First-hand accounts of ICP developments from na- tions around the world. Special reports on microwave and other plasma progress. Calendar and advanced programs of plasma meetings. Publication of plasma-related patents.Technical translations and reprints of critical foreign- Critical reviews of plasma-related books. language ICP papers. Conference Activities The ICP Information Newsletter has sponsored five international meetings on developments in atomic plasma spectrochemical analysis since 1980 in San Juan, Orlando, San Diego, Leysin, Switzerland, and Kailua-Kona, HI. Meeting proceedings have ap- peared as Developments in Atomic Plasma Specfrochemical Analysis (W i ley), Plasma Specfrochemistry and Plasma Specfrochemistry II (Pergamon Press) as well as in special issues of Specfrochimica Acta, Part 6. Subscription lnformation Subscriptions are available for 12 issues on either an annual or volume basis. The first issue of each volume begins in June and the last issue is published in May.For example, Volume 12 runs from June 1986 through May 1987. Back issues beginning with Volume 1, May 1975 are also available. To begin a subscription, complete the attached order form, and submit it with prepayment or purchase in- formation. For additional information please call (41 3) 545-2294 or contact the Editor. Detach and send to: ICP information Newsletter, Dr. Ramon M. Barnes Department of Chemistry, GRC Towers, University of Massachusetts, Amherst, MA 010031.0035 Telephone (41 3) 545-2294 Start a subscription for the following issues (complete): [ ] Volume(s) - (June 198-- May 198-) or [ J 198- (January-December) I enclose: [ ] prepayment or [ ] purchase order (No. 1 or [ ] Send invoice. 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ISSN:0267-9477    

DOI:10.1039/JA98601FP041

出版商:RSC    

年代:1986

数据来源: RSC

摘要:

... Vlll ~ ~ Following publication of Annual Reports on Analytical Atomic Spectroscopy Vol. 14, this series will be discontinued. Much of the material covered, however, will appear in journal of Analytical Atomic Spectrometry OMS) under the heading Atomic Spectrometry Updates. ANNUAL REPORTS Annual Reports M Analytical Atomic Spectroscopy Vdums 14 Hardcover 460pp ISBN 0 85186 677 8 Price $65.00 ($1 17.00) Still available: Vol. 3 (1973) 0 85186 253 6 212.00 ($22.00) Vol. 4 (1914) 0 85186 254 4 217.00 ($30.00) Vol. 5 (1975) 0 85186 751 X $20.00 ($36.00) Vol. 6 (1916) 0 85186 747 2 226.00 ($41.00) Vol. 1 (1977) 0 85186 731 5 525.00 ($45.00) Vol. 8 (1918) 0 85186 630 1 225.00 ($45.00) Vol. 9 (1979) 0 85186 727 8 237.00 ($66.00) Vol. 10 (1980) 0 85186 717 0 239.00 ($70.00) Vol.11 (1981) 0 85186 701 3 E53.00 ($95.00) Vol. 12 (1982) 0 85186 697 2 E45.00 ($81.00) Vol. 13 (1983) 0 85186 687 5 255.00 ($99.00) Special Package Price (Vols 3-14) 2282.00 ($508.00) Ordering: Orders should be sent to The Royal Society of Chemistry, Distribution Centre, Blackhorse Road, Letchworth, Herts. SG6 lHN, U.K. Non-RSC member prices quoted. RSC members are entitled ro a discounr on most publications. Derails available from: Assisrant Membership Officer, The Royal Society of Chemistry, 30 Russell Square, London WClB 5DT, U.K. US$ prices quoted. ROYAL Information Services ON ANALYTICAL ATOMIC SPECTROSCOPY VOL 14. Edited by L Ebdon, Plymouth Polytechnic and M S Cresser, University of Aberdeen This publication reports on current developments in all branches of analytical atomic emission, absorption and fluorescence spectroscopy with reference to papers published and lectures presented during 1984.Much of the information is presented in tabular form for ease of reference. Brief Contents: ATOMIZATION AND EXCITATION: Arcs, Sparks, Lasers and Low-Pressure Discharges; Plasmas; Flames; Elect ro t her ma1 Atomization; Vapour Generation. INSTRUMENTATION: Light Sources; Optical Systems and Detectors; Background Correction; Automatic Sample Introduction; Instrument Control and Data Processing; Complete Instruments; Commercial Instruments. METHODOLOGY: New Methods; Detection Limits, Precision and Accuracy; Standards and Standardization. APPLICATIONS: Chemicals; Metals; Refractories and Metal Oxides, Ceramics, Slags and Cements; Minerals; Air; Water; Sods, Plants and Fertilizers; Foods and Beverages; Body Tissues and Fluids.REFERENCES AUTHOR INDEX SUBJECT INDEX ‘I. . . , an essential reference work for atomic spectroscopists and for chemists concerned with trace metal analysis.” - J E Page, Chemistry and Industry, reviewing Vole 11vi 1987 WINTER CONFERENCE ON PLASMA AND LASER SPECTROCHEMISTRY LYON, January 12-16,1987 FEATURES The 1987 Winter Conference on Plasma and Laser Spectrochemistry will feature recent developments in this field. The Conference topics will include the various types of plasmas (ICP, DCP, MIP and GDL) and hyphenated methods such as ICP-MS, chromatography, flow injection and Fourier transform spectroscopy. A symposium will be devoted to different aspects of laser spectrochemistry (laser induced atomic fluorescence, intracavity laser absorption and laser enhanced ionisation spectrometry).The Conference will cover fundamental aspects, technological developments and applications, along with manufacturer seminars. The Conference will be held in Lyon, January 12th to January 16th, 1987 at the Mapotel Best Western Hotel. The official language of the Conference will be English. SCIENTIFIC PROGRAMME A large number of plenary lectures will allow the presentation of the state of the art in plasma and laser spectrochemistry. Although some oral presentations will be accepted, poster presentations are highly recommended in order to facilitate exchange of information and to overcome language problems. Original papers will be published following the meeting after peer review in the Journal of Analytical Atomic Spectrometry.Information stands will be available for plasma and laser instrumentation companies. INVITED SPEAKERS The following scientists have been invited to present plenary lectures on plasma and laser spectrochemistry: T. Berthoud (Fontenay, France), M. Blades (Vancouver, Canada), P. W. J. M. Boumans (Eindhoven, The Netherlands), J. Broekaert (Dortmund, FRG), R. F. Browner (Atlanta, USA), L. Faires (Los Alamos, USA), H. Falk (Berlin, GDR), K. Govindaraju (Nancy, France), G. M. Hieftje (Bloomington, USA), G. Horlick (Edmonton, Canada), G. Knapp (Graz, Austria), C. W. McLeod (Sheffield, UK) and G. C. Turk (Gaithersburgh, USA). REGISTRATION Further details and Conference and Hotel registration forms may be obtained from: J.M. Mermet, Winter Conference, Laboratoire des Sciences Analytiques, Bat. 308, Universite Claude Bernard - Lyon I, 69622 Villeurbanne Cedex, France.vi 1987 WINTER CONFERENCE ON PLASMA AND LASER SPECTROCHEMISTRY LYON, January 12-16,1987 FEATURES The 1987 Winter Conference on Plasma and Laser Spectrochemistry will feature recent developments in this field. The Conference topics will include the various types of plasmas (ICP, DCP, MIP and GDL) and hyphenated methods such as ICP-MS, chromatography, flow injection and Fourier transform spectroscopy. A symposium will be devoted to different aspects of laser spectrochemistry (laser induced atomic fluorescence, intracavity laser absorption and laser enhanced ionisation spectrometry).The Conference will cover fundamental aspects, technological developments and applications, along with manufacturer seminars. The Conference will be held in Lyon, January 12th to January 16th, 1987 at the Mapotel Best Western Hotel. The official language of the Conference will be English. SCIENTIFIC PROGRAMME A large number of plenary lectures will allow the presentation of the state of the art in plasma and laser spectrochemistry. Although some oral presentations will be accepted, poster presentations are highly recommended in order to facilitate exchange of information and to overcome language problems. Original papers will be published following the meeting after peer review in the Journal of Analytical Atomic Spectrometry. Information stands will be available for plasma and laser instrumentation companies.INVITED SPEAKERS The following scientists have been invited to present plenary lectures on plasma and laser spectrochemistry: T. Berthoud (Fontenay, France), M. Blades (Vancouver, Canada), P. W. J. M. Boumans (Eindhoven, The Netherlands), J. Broekaert (Dortmund, FRG), R. F. Browner (Atlanta, USA), L. Faires (Los Alamos, USA), H. Falk (Berlin, GDR), K. Govindaraju (Nancy, France), G. M. Hieftje (Bloomington, USA), G. Horlick (Edmonton, Canada), G. Knapp (Graz, Austria), C. W. McLeod (Sheffield, UK) and G. C. Turk (Gaithersburgh, USA). REGISTRATION Further details and Conference and Hotel registration forms may be obtained from: J. M. Mermet, Winter Conference, Laboratoire des Sciences Analytiques, Bat.308, Universite Claude Bernard - Lyon I, 69622 Villeurbanne Cedex, France.... Vlll XXV Colloquium Spectroscopicum lnternationale Toronto, June 1987 Post CSI Symposia Inductively Coupled Plasma Mass Spectroscopy June 28-30,1987, Lake Muskoka, Canada Further information from: Dr. Chris Riddle, Chief Analyst, Geoscience Laboratories, Ontario Geological Survey, 77 Grenville Street, Room 11 17, Toronto, Ontario M7A IW4, Canada Graphite Furnace Atomic Absorption June 28-July 2, 1987, Huntsville, Ontario, Canada Further information from: Dr. J. A. Holcombe, Department of Chemistry, University of Texas at Austin, Austin, Texas 7871 2-1 167, USA or Dr. R. E. Sturgeon, Analytical Chemistry Section, Division of Chemistry, National Research Council of Canada, Ottawa K1A OR9, Canada Second Surrey Plasma Source M; July 6-8, 1987, Gui Zonference on ISS Spectrometry dford, Surrey, UK Further information from: Dr.A. L. Gray, Department of Chemistry, University of Surrey, Guildford, Surrey, GU2 5XH, UK 1987 PITTSBURGH CONFERENCE Once again, the RSC is organising a tour group for Members of the Society attending the Pittsburgh Conference. Travel will be with TWA from London Heathrow to Kennedy, New York, and will include coach transfer to Atlantic City and accommodation on a room-only basis in selected hotels close to the Convention Centre. Additional requirements such as transfer to Heathrow and personal onward itineraries after the meeting can be catered for, as well as car hire, assistance with visas etc. The pressure on hotel space in Atlantic City is enormous, as any visitor to previous Pittsburgh Conferences will testify. Our rooms are already reserved, so booking with the RSC Group is your guarantee of good accommodation and a trou ble-f ree meeting. For further details, please telephone Karen Mizel on 01-437 8656 extension 250. IN SPECTURAL SOURCES 0 High quality 0 High intensity High spectural purity 0 High stability& long life Hollow cathode lamps at the lowest available prices! Although a relatively new name in H.C. lamps, SIP Analytical Limited combines personnel each with over 25 year's manufacturing experience with purpose built, high capacity manufacturing plant, to produce a high quality, reliable product at significantly lower prices. A comprehensive range of tubes to fit all makes of instrument available ex- s t oc k For further details contact:- S. 1. P. ANALYTICAL LTD Unit 1, All Saints Industrial Estate, All Saints Avenue, Margate, Kent CT9 50W Tel: (0843) 221295. - Telex: 826932

ISSN:0267-9477    

DOI:10.1039/JA98601BP045

出版商:RSC    

年代:1986

数据来源: RSC

摘要:

JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, DECEMBER 1986, VOL. 1 169R ATOMIC SPECTROMETRY U PDATE-MINERALS AND REFRACTOR1 ES David A. Hickman" The Metropolitan Police Forensic Science Laboratory, 709 Lambeth Road, London SEI 7LP, UK Joan M. Rooke Department of Earth Sciences, The University, Leeds LS2 9JT, UK Michael Thompson Applied Geochemistry Research Group, Department of Geology, Imperial College of Science and Technology, London SW7 ZBP, UK Summary of Contents 1 Sample Preparation 1.1. 1.2. 1.3. 1.4. 1.5. 1.6. Trendsin Sample Preparation Solid Sample Introduction 1.2.1. Slurry injection 1.2.2. Laser ablation and spark generation of aerosols 1.2.3. Direct insertion into plasmas 1.2.4. Remote ramp heating 1.2.5. Solid sample analysis in atomic absorption spectrometry Decomposition with Acids Fusion Methods Separation and Pre-concentration Sample Preparation for Inductively Coupled Plasma Mass Spectrometry 2 Atomic Emission Spectrometry 2.1.Arc or Spark Excitation 2.2. Flame Excitation 2.3. El ect rot he r ma I Atom isat io n 2.4. Inductively Coupled Plasma 2.5. Direct Current Plasma 2.6. Microwave Plasma 3 Atomic Fluorescence Spectrometry 4 Atomic Absorption Spectrometry 4.1. Flame Atomisation 4.2. Elect rot he rmal Atom isat ion 4.3. Other methods 5 Inductively Coupled Plasma Mass Spectrometry 6 Comparison of Methods 7 Analysis of Certified Reference Materials Table 1. Summary of Analyses of Minerals and Refractories This review is the sixth Atomic Spectrometry Update (ASU), and completes the cycle of reviews which began in Issue 1 of JAAS.The six Updates have covered most of the material that was formerly published in ARAAS, and it is intended that they will be published annually, in the same sequence, in successive volumes of JAAS. As it has been necessary to accommodate the change-over period from ARAAS to JAAS - ASU, the six reviews have each covered different lengths of time; this review is based on abstracts received between 1st September 1984 and 1st May 1986. References prefixed by S/ or S/C are listed in the supplement that has been distributed to subscribers to JAAS, and references with an 861 prefix are listed in the issues of Volume 1 of JAAS. The material reviewed corresponds to ARAAS Chapters 4.3 "Refractories and Metal Oxides, Ceramics, Slags and Cements" and 4.4 "Minerals," but in this review the sample types are not considered separately.The authors would welcome any comments on this review or suggestions for future reviews. * Review Topic Co-ordinator, to whom correspondence should be addressed.170R JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, DECEMBER 1986, VOL. 1 1. SAMPLE PREPARATION 1.1. Trends in Sample Preparation Sample preparation, the conversion of the raw sample material into a form suitable for presentation to an instrument, is often regarded as the “Achilles Heel” of atomic spectrometry, a time-consuming and messy ordeal that has to be endured before the analyst can get down to the real business of instrumental analysis. For this reason there has been increas- ing interest and a moderate degree of success in the direct use of solid samples with no prior chemical preparation.This approach, if eventually completely accomplished, could cer- tainly reduce the labour-intensive stages of analysis and cut over-all costs. Some enthusiasts of solid-sample presentation have asser- ted that methods of chemical preparation are always time consuming, tedious or labour intensive. Improvements in technique, however, have enabled large batches of samples to be handled with a minimum of attention from the analyst. In favourable instances no more is needed than a dissolution of the sample, sufficient selectivity being achieved by atomic spectrometry. Dissolution of minerals and refractories is generally more difficult than any other class of material. Nevertheless, with the advent of the PTFE bomb and of lithium metaborate fusion, dissolution is rarely an inherent major problem. It seems unreasonable to assume that chemical decomposition will be completely avoidable even when solid introduction methods are eventually perfected.The intrinsic selectivity of atomic spectrometry, even for the best available methods, is strictly limited. To achieve better selectivity, chemical separations will still be required, a recourse not associated with solid-sampling techniques. Thus there has been a steady interest in rapid methods of achieving such separations, especially in low trace analysis, an area where interference is often the main limiting factor. The application of inductively coupled plasma mass spec- trometry is likely to revolutionise many aspects of elemental analysis. However, it imposes new demands on chemical sample preparation, and solid-sampling methods may eventu- ally prove to be ideal for ICP-MS.1.2. Solid Sample Introduction 1.2.1 . Slurry injection Numerous studies of slurry injection into the ICP, DCP and flames have been made, all with Babington-type nebulisers. The technique has been used by several groups for the analysis of coal and coal ash (S/C278, S/C299, S/C324, S/C1180), and also for other materials such as Ti02, soils, ferroalloys and slags (S/C725, WC1171, S/C1176). Practical problems encountered in empirical studies have forced workers to look at the fundamental behaviour of nebulised slurries, and some improvements have resulted. Ebdon (86K1196) identified the benefits of solids injection in ICP-AES as (i) no change to existing equipment and (ii) the possible use of simple aqueous standards. The latter point is especially important in solid sample work, as preparation of solid standards can be a major limitation in many methods.Particle size is a critical parameter in slurry nebulisation, and by spraying kaolin slurries Ebdon was able to show that only the smaller particles reached the plasma. With an enlarged ICP injector tube (3 mm), however, particles with diameters <8 pm reached the plasma (86K1196). The different injection system of the DCP is even more favourable in this respect. Slurry concentrations of up to 20% m/V can be nebulised, but a dispersant is necessary to prevent aggregation (86/C881, 86/C1196, 86/C1569).Transport - atomisation efficiency approaches that of simple solutions for favourable matrices such as kaolin and coal (86/1432). However, problems are more likely with refractory materials and multi-phase sub- stances such as soils and rocks. Slurry injection into the ICP of zeolites as a suspension in xylene has been reported (8611442). Despite the nominal absence of chemical preparation in slurry nebulisation, physical preparation of samples remains a lengthy operation. The technique may well prove especially advantageous in process control, for materials that are already finely powdered. 1.2.2. Laser ablation and spark generation of aerosols Despite the simplicity of the method, progress with laser ablation has been slow since its inception. Thompson (86/C808) used a ruby laser to mobilise material from thin or small geological samples into an ICP.Good precision was obtained when elements were ratioed to a major constituent, and no sample preparation was required. Mitchell et al. used a low-energy high-repetition rate YAG laser to mobilise steel and copper ore into a DCP (S/C320,86/1464). They obtained good accuracy, RSDs of 3-1070, and a detection limit of ca. 100 pg g-1 for Cu. Gray demonstrated the use of a high-repetition rate ruby laser for sample ablation into an ICP mass spectrometer system (86/196). These results represent little advance on previously reported work, and it is clear that some fundamental studies of ablation processes are required. True simultaneous analysis is needed to exploit properly these transient signal methods.A high-voltage spark was used, with apparent success, to generate an aerosol of ferromanganese nodules for injection into an ICP. The main problem of this technique is the differential erosion of various mineral phases, and this hinders representative sampling (86/C1139). 1.2.3. Direct insertion into plasmas Horlick et al. (S/C304,86/C1136) described a cup device that is suitable for the direct injection of solids, as well as micro- volumes of solution, into the ICP. Detection limits as low as 1 pg could be obtained in favourable circumstances with samples of ca. 1 mg. Calibrations were reported for relatively volatile elements (Ag, As, Cd, Cu, Ge, In, Li, Pb, Sn and Zn) over three orders of magnitude. A novel combination of this system with laser ablation allowed material ablated at a remote site to be collected in a graphite ring, which was subsequently heated in the cup.Brenner and co-workers (86/C756, 86/C1137) have warned of difficulties with geolog- ical materials due to selective volatility and complex mineral- ogy. These effects are likely to be similar to the corresponding problems in arc or spark AES analysis. 1.2.4. Remote ramp heating A combination of an element detector with thermal analysis can be used to monitor the liberation of an element as a function of temperature. This neglected technique provides information on speciation by monitoring chemical changes at characteristic temperatures. Bauer (86K1602) used MIP-AES to measure carbon liberated during the ramp heating of carbonate mixtures, and showed that it was possible to resolve the signals due to several carbonates (Ca, Fe, Mg, Pb and Sr) likely to occur in geological samples.There seems to be scope for a wider study of such combinations of techniques. 1.2.5. Solid sample analysis in atomic absorption spectrometry Langmyhr and Wibetoe (864725) have reviewed comprehen- sively the topic of direct solid analysis by atomic absorption spectrometry, including both flame and furnace methods, and they listed 458 references. A combined flame and furnace AAS method has been applied to the direct analysis of biological and geological samples (36/C937). Oreshkin et al. (86/C455) have investigated the direct analysis of various environmental samples.JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, DECEMBER 1986, VOL.1 171R 1.3. Decomposition with Acids The capabilities and limitations of acid mixtures have been reviewed (86/C1246), but no novel developments of wide applicability have emerged over the past 21 months. Various mixtures of acids have been used, the most common being combinations of HC104, HN03 and HF. The use of sealed tubes under moderate pressure is more popular, avoiding both the copious fume emission of open-vessel methods and the expense of bombs. Microwave heating is also becoming more widely used (86/C162). The most interesting development has been an increasing recognition of the usefulness of phosphoric acid, which has been used to dissolve alumina ceramics (86/1095) and geo- logical materials , especially for the determination of Cr (86/1041).Phosphoric acid has been recommended by Hannaker and Hou (S/609) for the rapid and complete (sic) dissolution of refractories, rocks, soils and slags. Mixtures containing perchloric and hydrofluuric acids are most popular for the dissolution of silicates and other materials. Such mixtures have been used, in open vessels, for the analysis of coal for trace elements (86/C903), rocks for Se (86/C953) and obsidian archaeological artefacts for trace element fingerprinting (86/C1259). The same dissolution procedure has been used prior to the simultaneous determina- tion of As, Sb, Se and Te in silicate rocks by hydride generation ICP-AES (86/1630). A mixture of HC104 and HF was also used in sealed tubes for digesting coal ash (86/202). Perchloric acid was used with H2S04 for the digestion of coke (86/1345).In bombs, however, the use of HC104 seems to be avoided. This reflects mainly a commendable caution in the use of this substance, but also the fact that less hazardous acids can be used effectively at the higher temperatures available in bombs. Thus HCI alone was used at 140-160 "C to dissolve garnets (WC457, 86/735), HF - aqua regia for the analysis of cement (86/1298) and rocks and sediments (86/1016), HF - HCI for the dissolution of zirconium oxide for the determina- tion of impurities by ICP-AES (S/C446, 86/C500, 86/C501) and HF - HN03 for the digestion of coal ash (86/1412). Borides of chromium, molybdenum , titanium and zirconium have been dissolved in H2S04 - HN03 (S/64), and silicon nitride in HCl - HN03 (S/66).An alternative oxidant, KC103, has been used in the dissolution of sulphide ores by acid mixtures in sealed tubes in a microwave oven (86/1619). Weissman (86/C1200) used various acid mixtures for the complete dissolution of corro- sion-resistant glasses in bombs and by microwave heating. 1.4. Fusion Methods Fusion methods have been reviewed for glasses, ceramics and refractories (86K1246). No new departures are apparent. Lithium metaborate remains a most popular fusion agent in this area and seems capable of rendering soluble most silicate and oxide phases. Its main drawback, the requirement for a high dilution of the sample, appears to be no deterrent to its use. Lithium metaborate fusion has been used as a prelude to the determination of Mn (86/1277), Mo (86/692) and Sn (861692, 86/1617) in rocks by AAS and for the determination by ICP-AES of rock-forming elements in the presence of large amounts of U and Th (864636).It has been used also for the analysis of fly ash (86/C1584). Grognard and Piolon (86/1620) used an H2S04 pre-treatment to an LiB02 fusion to prevent the loss of T1 in fly-ash analysis. Lithium tetraborate has been recommended as a flux for the analysis of bauxites and Bayer muds by ICP-AES (861C1555). The use of nun-borate fluxes has been less widely reported. A fusion with KCN was used for Sn determination in rocks and minerals (86/1830), and an Na2C03 - K2S207 mixture was recommended for solubilising electroslag remelting slags prior to FAES and FAAS (86/1789). Sodium carbonate alone has been advocated for special glasses (S/C275) and silicon carbide (S/216), and has been compared with acid dissolution methods for corrosion-resistant glasses (S/C277).Walsh (86/662) used K2CO3 for B determination in rocks by ICP-AES. The soluble B033- was separated from the water insoluble residues, and excess of K was removed by the addition of HC104. The high dilution normally required with fusions has been avoided by Lichte and Riddle (S/C720), who designed a nebuliser - torch combination for ICP-AES that could operate continuously with 5% m/V solutions. 1.5. Separation and Pre-concentration There continues to be considerable interest in methods of pre-concentrating and separating determinands from other- wise troublesome matrix elements or fluxes. Predictably , the elements involved have been mainly those occurring at low trace levels.Most reports, however, have been concerned with a single determinand or with a small group of elements. A more substantial effort is needed to perfect the chemistry and technique required for rapid multi-trace element separations. Great interest in the determination of precious metals is evident. Branch and Hutchison (86/1637) studied the critical factors in the solvent extraction of Au into ketones as a prelude to FAAS analysis of geological materials, and they identified Fe co-extraction as an important problem. Pre- concentration of Au in geochemical analysis has been repor- ted by several other workers (Table 1). Silver has been cleanly separated from other transition metals by zephiramine (86/ 1031).Interference from Ca has been eliminated in the FAAS determination of Ag and Cd in limestone by precipitation with oxalic acid (86/1018). Co-extraction of iron is a common problem in the solvent extraction of halo-complexes. Some workers recommend reduction with ascorbic acid to inhibit Fe extraction (86/678 , 86/682). Thompson and Liang (86/72) used ascorbic acid - KI to minimise Fe extraction with Mo as the chloride into heptan-2-one during the determination of Mo in geological materials by ICP-AES. Elements that have been extracted as groups include the rare earths and gallium - indium - thallium. The REEs have been determined by spectrography , after an ion-exchange or similar separation, and ashing of the substrate (86/1017, 8611371).They have also been determined by thin film XRF after ion exchange and co-precipitation (86/679). Haines (S/C1164) separated the REEs as insoluble fluorides after fusion with KHF2. Gallium, In and T1 have been extracted as chloro- complexes into a variety of solvents (Table 1). Several workers have reported the simultaneous separation of several elements. Viets et al. (S/188) extracted Ag, As, Bi, Cd, Cu, Mo, Pb, Sb and Zn into Aliquat 336 - IBMK from an HCl - KI - ascorbic acid mixture. This method was applied to the FAAS analysis of geological materials, after a fusion with K2S207. Nicolas (S/C1192) reported the quantitative extrac- tion of Ag, Au, Pd and Pt into diantipyrylmethane solution in CHC13 from 0.6 M H2S04 containing KI and ascorbic acid. The tricaprylylmethylammonium ion was used to extract Ag, As, Bi, Cd, Co, Mn, Mo, Ni, Pb, Sb, Se, Te and Zn, and in this method the co-extraction of iron was also prevented by ascorbic acid (86K637).Barnes (SK1147) used a poly- (dithiocarbamate) chelating resin to separate Ag, Pd, Pt, Ta, Th and U from aqueous solutions derived from the decompo- sition of geological materials. 1.6. Sample Preparation for Inductively Coupled Plasma Mass Spectrometry Sample preparation for ICP-MS is in a separate class: a new perspective is demanded, especially in relation to geological172R JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, DECEMBER 1986, VOL. 1 materials (86/C1109). Large concentrations of flux cannot be tolerated, because of matrix effects and progressive blocking of the probe orifice (S/C461).These problems were circumvented after a K2B407 fusion of tourmaline by removal of K as KC104 and B as BF3 (86lC1260). Even some of the usual acids generate problems from isobars and molecular ions (86/C1180), although nitric acid seems less of a problem than some other acids. The sample matrix can also cause problems, so that very dilute solutions of the sample are required. On the credit side, the sensitivity of ICP-MS is so good that satisfactory detection limits are available at large dilutions and with no separations. Thus there have been reports of successful determinations of Th and U in tourmaline, after dilution to 0.1% m/V (86/C1267), trace elements in archaeol- ogical silver at a dilution of ca. 0.03% m/V, with detection limits for many elements at 1 pg g-l or less (86/C1260), REEs in rocks after acid attack and dilution to 0.2% m/V (86/1670) and various elements in fluid inclusion leachates (86/C1264).Date et al. (S/C461) determined trace elements in rocks after an acid digestion. Platinum group metals and gold have been determined after an initial fire-assay separation, with very low detection limits (S/C1186, 86/C547). 2. ATOMIC EMISSION SPECTROMETRY 2.1. Arc or Spark Excitation Amongst recently published procedures for the analysis of geological materials the number of papers describing the use of classical spectrography is small compared with those where AAS or ICP-AES has been employed. However, emission spectrometry with arc or spark excitation can still satisfy almost all the criteria for the trace element analysis of the type of material that falls within the scope of this review.It enables the simultaneous determination of a number of elements to be made with good accuracy, precision, detection limits and speed, with the additional benefits of low cost and simplicity of sample preparation. It is noteworthy that most of the publications concerned with emission spectrography originate from laboratories in India, China, Yugoslavia, Czechoslo- vakia and Russia, and they are mainly concerned with the choice of spectroscopic buffer. The direct current arc is still widely used as an excitation source. Typical recent applications are the determination of V in ancient sedimentary rocks (86/C635), 12 elements in pyrite and pyrrhotite, with RSDs in the range 9-19% (86/1295), and 14 REEs in erbium oxide, with RSDs of 2.9-16.2% (9888).Date and co-workers (86/C639) chose a d.c. arc emission spectrographic method for stream sediment samples because it enabled rapid analyses to be made with good accuracy and precision. Care had to be taken with matrix corrections and with the sample preparation. The long-term reproducibility of the method was better than 10% for most elements, and each sample could be prepared and analysed for up to 33 elements in approximately 10 min. The accuracy of trace element determinations by emission spectrography has been con- sidered by PlSko (86/C134) with emphasis on the dependence of spectral line intensity on matrix composition; fractional evaporation was identified as the cause of systematic errors. In the determination of Pb and Sn in basic and ultrabasic rocks, interference from Fe was suppressed by a buffer mixture of (S + 10% C + 18% NaF), which resulted in the formation of FeS (86/752).An internal standard was employed by Egranova and Val1 (S/134) for determining Ba and Sr in rocks and ores by d.c. arc emission between carbon electrodes with a graduated channel electrode. Powdered graphite containing 50% NaCl formed the lower (narrower) part, and the sample mixed with powdered graphite containing 0.002% PdC12 was placed in the upper part of the electrode channel. Palladium was also used as an internal standard in the determination of Th, Y and Zr in river sand, which was mixed with an equal mass of graphite powder containing Pd (S/232), allowing Ta to be measured in columbite - tantalite with an RSD of 2.4% (86/1329).The effects of buffers, graphite electrode shape and d.c. arc current were studied by Yu and Jin (86/379) in the determination of 14 REEs in lutetium oxide and the RSDs were in the range 3.3-17.1%. Volke (86/1723), in developing a spectrographic method for determining Cu, Ni, Ti and V in coke, measured the d.c. arc temperature with a two-line method based on V and Zn lines, and found that NaF showed a greater temperature lowering than PbC1,; the maximum intensity of the atomic lines was at 5500 K and 2-5% NaF. The carrier effect was studied for a granitic matrix by Guirguis et al. (86lC565). They added NaCl, NaF, CaF2, CdF2 and PbF2 at 10, 20 and 30% concentration, and Ga203 and AgCl at 1 , 2 and 670, and concluded that the addition of 20% CdF2 gave good accuracy combined with better detection limits for 15 elements.Although inorganic substances are most often used as spectral buffers, Tiirker and Dogan (86/C569) have investigated NaDDC, tetramethylammonium bromide and iodide and triammonium citrate for stabilising a d.c. arc discharge; they achieved improved RSDs for the determination of Mo, Ni and V in asphaltite ash. An alternating current arc was employed by Song and Jin (S/233) for the determination of REEs in terbium oxide; a mixture of oxygen and argon was used for arc excitation. The effect of the burning period of the a.c. arc on various parameters involved in calibration has been studied (S/99). A less conventional form of sample introduction was employed by Kolosova et al.(S/135), who determined trace noble metals in ores by blowing powdered concentrates into a 22 A a.c. arc source. Spark-source excitation has been employed in the determi- nation of REEs in non-conducting substances briquetted with graphite; the accuracy, precision and detection limits could be improved by using argon containing 5% oxygen or argon saturated with water vapour (S/78). A rotating graphite electrode spark emission method with Co as internal standard has been used to determine seven elements in rocks, with RSDs in the range 3.1-8.7% (S/657). 2.2. Flame Excitation Few papers concerned with the flame emission analysis of geological material were published in the period under review. The technique is best suited to the determination of the alkali metal elements (Table 1).Flame emission from an N20 - C2H2 flame has been used to determine La, Sc and Y, and the interferences from several elements were studied (86/1831). The same flame type was used to determine Eu in HC104 - HF digests of rocks; K+ or Naf were used to suppress ionisation, and the interferences from accompanying elements were studied (86/371). 2.3. Electrothermal Atomisation A method for determining Li in acid-digested rocks by emission from a graphite furnace has been reported; interfer- ences from six rock matrix elements could be eliminated by adding H2S04, and the method gave a detection limit of 2.8 pg, lower than either FAES or graphite furnace AAS (S/C254).JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, DECEMBER 1986, VOL.1 173R 2.4. Inductively Coupled Plasma Inductively coupled plasma atomic emission spectrometry is widely used for the quantitative multi-element analysis of geological material, and the high temperature of the ICP allows the sensitive measurement of refractory elements such as B and P. Many publications refer to ICP-AES simply as an element measurement procedure, without giving experimen- tal details. Grote (S/C444) noted that the large dynamic ranges of ICP-AES make it possible to determine both major (Al, Ca, Fe and Mg) and trace (Ba, Co, Cr, etc.) elements from a single digest (i.e., percentage to p.p.b. range). For major elements the technique can provide good accuracy and precision if suitable calibration procedures and internal standardisation are employed.Problems in the determination of trace elements can be related to background enhancement and spectral line overlap from concomitant elements such as Al, Ca, Fe, K, Mg, Na, P, Si and Ti. Physical interferences in the nebulisation process can also affect adversely the accuracy and precision. Internal standardisation is often used to correct for sample transport variations, but it is encouraging to see research being undertaken into alternative methods of sample introduction for ICP-AES . Both simultaneous and sequential inductively coupled plasma atomic emission spectrometers are in widespread use. Sequential systems have the advantage of flexibility in wavelength selection, which can be used to allow for variations in analyte concentration and matrix type, but the analysis time is necessarily longer. Lichte and Riddle (S/C720) have pointed out that mineralisation in rocks may increase the element concentration of, for example, Cu, Mo, Pb, U and V from a few p.p.m.to several percent., and the selection of wavelength then becomes very important due to increased risk of spectral overlap; they described the use of a computer program that accounts for all significant spectral interfer- ences. The complex composition of geological materials can give rise to several sources of interference in ICP-AES but these can generally be minimised, if not eliminated, by the use of one or more of the following: a high-resolution spectrometer, on-line background compensation, pre-determined interfer- ence coefficients or matrix-matched standards.Lorber et al. (861C755, 86/C1182) have described a method for accurate background compensation by scanning a spectral segment on either side of peak positions. The spectrum of each interferent is then measured, and its contribution is removed mathematic- ally from the analyte signal. Many workers have noted that spectral interferences due to sample concomitants have to be taken into account to ensure accurate results, for example in the analysis of phosphate rocks (86/C760). Sat0 and Sakata (86/314) determined 15 elements in coal ash with RSDs of less than 3%, and found that only As and Pb were subject to such interferences. Mo et al. (S/C283) reported that, for matrices such as refractory materials containing A1 and Fe, careful selection of the analytical line was required in determining Mo, Ti and V, and in some instances it was necessary to use a weaker analytical line, with a consequent loss in sensitivity.In a method for determining Si in barium titanate, spectral interference by Ti on the Si 251.6-nm line could be corrected by subtraction (S/504). A number of spectral interferences were identified in the analysis of acid-digested rocks, and the most sensitive analytical lines for Co, Cr, Mn and V could not be used; inter-element correction was needed for Cr against Fe, and Pb determinations were unreliable due to A1 flank lines (86/C1536). Tanaka et al. (86/C500) determined trace ele- ments in zirconia ceramics and chose Al, Ce, Cr, Cu and Si lines that were little affected by interferences from Zr.Fujino et al. (860073) found that corrections for spectral inter- ferences were necessary in determining some REEs in phosphate minerals, but Ce, La, Lu, Sm, Y and Yb were free from such interferences and could be determined at the 1 pg g-1 level with RSDs of 1-5%. Interference correction factors were employed by Haraguchi et al. (86/312) in the simultaneous determination of up to 21 elements in acid- digested coal and fly ash. Brenner and co-workers (W707, S/C1177) have compiled an ICP atlas of real-life spectral interferences, based on measurements made with a vacuum polychromator and a very high resolution scanning monochro- mator. A computer-based method that calibrates intensity measurements and calculates line interferences was described by Burstenbinder and Luck (S/C1178).Thompson and Ramsey (86/973) reported a detailed exami- nation of matrix effects due to Ca, an important geological matrix element, on a selection of analytical lines in ICP-AES. They found that most analyte sensitivities were suppressed, by as much as 30% in some instances, but they were able to demonstrate methods of overcoming the problem. One method of eliminating a matrix effect is to separate the matrix elements, and in the determination of REEs in U02 most of the uranium was separated by solvent extraction; however, the residual amount of uranium still caused some interferences (86/C503). For the ICP-AES determination of Al, Ca, Fe, Si and Ti in acid digests of zirconium dioxide the matrix effects were found to be as much as 10% for each element under conditions that had been optimised for Mn.When compro- mise conditions were used the matrix effects fell to below 4% (861C501). In another analysis of zirconium dioxide, where nine elements were determined in acid digests, it was necessary to add matrix components to the standard solutions (8611034). Sample transport interferences can often be corrected by using an internal standard, and Sc is a popular choice. The Sc 361.384-nm line was used in the determination of W in solutions of tungsten ores (S/222). In the analysis of silicates containing major amounts of U and Zr, synthetic solutions were used for calibration and Sc was used as the internal standard (86/1636). The same internal standard has been reported as being able to compensate for both long-term drift and matrix interferences (86/C460).Other examples of internal standards are nickel, which was used in the analysis of acid-digested coal ash for 11 elements (86/202), and yttrium, which allowed neodymium to be determined in yttrium aluminium garnet with an RSD of less than 0.5% (S/C457). Samuel et al. (86/1288) determined up to 48 minor and trace elements in rocks after a fusion procedure, and found that the relative error, after interference corrections, was ca. 10%. Good analytical accuracy and precision were noted by Kane (8611323) in the analysis of 16 geological reference standards for six elements. Nagashima et al. (S/68) claimed that the ICP-AES determination of 17 major components in multi- component oxide materials, following an acid digestion, was sufficiently accurate to calculate chemical formulae, once corrections had been made for spectral interferences from co-existing elements.Although most applications of ICP-AES are multi-element , a few publications refer to detailed studies of the determination of a small number of elements. One such study, for W, listed 231 W lines and recommended four for analytical use. The effects of ICP instrumental parameters were examined and the method was applicable to acid digests of silicate rocks (S/lOl). Cook and Miles (86/437) studied the analytical suitability of several P emission lines and recommended the 178.29-nm line compared with the 213.62- and 214.91-nm lines. This was because it was not subject to unacceptable spectral interfer- ences and was less affected by shifts in spectral background caused by the high concentrations of A1 present in rocks.Phosphorus has been determined in acid-digested rocks using the 216.62-nm line, with an RSD of ca. 1% (S/C445). Phosphorus lines at 213.72- and 214.91-nm were investigated by Zhang et al. (86/C850) for the analysis of ores and minerals, but they recommended the separation of the P because of174R JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, DECEMBER 1986, VOL. 1 interferences by copper and other matrix elements. The nebulisers in most ICP-AES instruments require the sample to be in solution, and section 1 dealt with sample decomposition for inorganic matrices, describing methods based on flux fusion and acid attack. If HF is used it is necessary to employ acid-resistant nebulising systems, as most conventional nebulisers contain glass parts.Kometani (S/ C275) used an HF-resistant sample introduction system for the determination of four elements in digested glass samples, but it was necessary to keep the final HF concentration to below 5% to prevent Si blanks due to the quartz tubes of the torch. Triton X-100 was added to promote better aerosol transfer to the torch. Alternatively, a complexing agent can be added to complex the fluoride ions in solutions containing HF. Weiss- man and Merrill (S/C277) added A1 or B to digests of corrosion-resistant glasses and thus avoided attack by HF on the glass parts of their ICP system. Thompson (86/C1247) has discussed improvements or modifications to ICP-AES instrumentation to achieve higher throughput of samples; he found that periods of sample clean-out and signal stabilisation could be greatly reduced, and modifications to the software achieved further improve- ments.However, it was necessary to employ rigorous methods of matrix correction to achieve maximum accuracy. Sequen- tial ICP-AES has been employed to determine 25 trace metal constituents in 3500 samples of acid-digested coal from power plants, during a three-year period (86K1234). As conventional nebulisers require fairly large (several ml) volumes of sample solution, methods for introducing small sample volumes into an ICP are of interest. Mayes and Lippert (86/C1258) used a peristaltic pump to “starve” the nebuliser on their sequential ICP-AES instrument and thus to reduce the sample uptake rate from 2.4 to 0.5 ml min-1 (86K1258).The introduction of solid samples into plasmas was considered in section 1.2. 2.5. Direct Current Plasma Although not as numerous as ICP-AES papers, several publications refer to the use of a direct current plasma for routine analyses. A detailed paper by Feigenson and Carr (86/1416) illustrates the use of DCP-AES in practical geo- chemical analysis. For igneous rocks, three different solutions (major, minor and rare earth elements) were analysed for 29 elements. A slight matrix effect due to Ca was identified, but this could be corrected empirically. The precision was 2% or better for 22 elements, better than 5% for six further elements and ca. 6% for Rb. The accuracy of the method was assessed ”using United States Geological Survey (USGS) standards and was claimed to be sufficient for most types of petrological and geochemical research.Interference effects in the DCP were studied by Avigur and Brenner (861C759) who found that enhancements and depressions in trace element determi- nations due to the presence of Ca, Mg and Na could be overcome by matrix-matching calibration. 2.6. Microwave Plasma An interesting reference to a microwave plasma that is of relevance to this review is a paper by Bauer (86/C1602), which described the determination of C02 released from the decomposition of different carbonates (calcite, dolomite, etc.) at characteristic temperatures. The C02 was detected by carbon emission in an MIP. 3. ATOMIC FLUORESCENCE SPECTROMETRY Atomic fluorescence spectrometry has been employed for the determination of a variety of elements in geological materials, and in several of the published papers hydride generation was used to provide the free atoms for excitation.Sua et al. (86/750) employed K2Cr207 as an oxidant to prevent the reduction of Hg ions in aqua regia digests of geological samples, prior to the liberation of free Hg by KBH4 and determination by non-dispersive AFS in a furnace at 350 “C. A similar method was used by the same workers to determine Bi and they achieved a detection limit of 4 X 10-10 g (86/1076). Arsenic and Sb were liberated as hydrides from geochemical samples and determined in a double channel AF instrument that incorporated an electrothermally heated silica tube atomiser (S/139).Selenium was determined in coal ash by generating the hydride and measuring the AF signal; interfer- ences from Cu and Pd were suppressed by the addition of C1- and Fe3+ complexing ions (86/436). Larkins (86/1368) repor- ted the determination of Au in aqua regia digests of geochemical samples by non-dispersive AFS in a nitrogen- separated air - C2H2 flame. He recommended that A1 be separated with Aliquat-336 in diisobutyl ketone in order to overcome large scatter signals from this element; further steps to remove Fe, normal for an AAS procedure, were not necessary. 4. ATOMIC ABSORPTION SPECTROMETRY For several years AAS, especially when employed in the flame mode, has been at a stage of maturity where publications often refer simply to using the technique, with scant attention to experimental details.For the analysis of geological material by AAS sample decomposition is generally necessary but for specialised applications the treatment can be very simple, e.g., an acid extraction. Details of new or improved digestion procedures are described in section 1 and many others are listed in Table 1. 4.1. Flame Atomisation Substances employed to suppress ionisation in flames are of interest, and Biavati (86/1767) has made a detailed study of such interferences for the analysis of glass and feldspathic sands. He recommended the use of La for eliminating Al, P and Ti interferences in the determination of Ca, while Sr could also be used to eliminate the A1 and P interferences. In the determination of Mg, interference from Ti was eliminated byJOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, DECEMBER 1986, VOL.1 175R La, and Sr could be used to eliminate A1 interference. Occasionally publications refer to the FAAS determination of larger groups of elements, e.g., nine major components in silicate rocks (86/33). A paper by Schinkel (S/98) entitled "A universal method for analysis of waters, coals, ashes, ores, rocks, building materials, etc." gives a detailed account of the determination of 14 elements, and discusses sample prepara- tion, calibration procedure, interfering elements, interference by physical properties of the sample solution and instrumental parameters. The addition of Cs and La was recommended for the elimination of physical, chemical and ionisation effects.The analytical procedures used by workers who routinely deal with large numbers of samples are of interest. Hassett and Hassett (86/C1584) analyse approximately 600 fly-ash samples a year for Al, Ca, Fe, K, Mg, Na, Si and Ti. They employ an LIB02 fusion followed by dissolution in dilute HN03. Standards are carefully matched for matrix elements, espe- cially for Ca, and A1 is added to the Si standards. They use an N20 - CzH2 flame for all elements, but with differing flame conditions; oxidising conditions are recommended for A1 , reducing for Ca and reducing-neutral for Si. Welsch (861692) has proposed a method in which 50 samples can be analysed per day for Mo and Sn, following an LIB02 fusion. Departing from standard methodology, two groups of Russian workers have used an air - C3Hs - C4HI0 flame.This flame was employed for determining Ca in solutions of tungsten ores, any interference from Si being suppressed by La (86/415), and for analysing copper ores, when H2SO4 was found to give the highest suppression of As and Sb signals (86/40). An indirect determination by FAAS was reported by Tsuge et al. (86/234) for the determination of chlorine in silicon nitride. A known amount of AgN03 was added to prevent the vaporisation of HC1 in the acid decomposition, the precipitated AgCl was removed, and the chlorine was determined indirectly by measuring the excess of Ag in solution. 4.2. Electrothermal Atomisation There have been more publications on the use of non-flame atomic absorption spectrometry, especially ETA-AAS , than those which refer to FAAS; this reflects the improvements that are still occurring in non-flame AAS techniques and instrumentation.Promising work is being carried out on the analysis of solid samples. Sample introduction to a graphite furnace as a slurry has been applied successfully (e.g. , S/C265, S/C572, 86/C289) and the analysis of organic solvents is straightforward in ETA-AAS. A variety of solvents can be utilised, e . g . , chloroform (86/311), IBMK (S/499), butyl acetate (S/224) , cyclohexane (S/580), toluene (86/407) and diethyl ether (S/153). Electrothermal atomisation AAS is most often used to determine very low analyte levels; this is illustrated by a paper by Kable et al. (S/C1165) describing the analysis of single mineral grains, with masses down to 1 mg.Up to 38 trace elements were determined in different minerals, but it was necessary to use solvent extraction procedures for some elements. Another application of the high sensitivity of ETA-AAS is the analysis of single crystals of doped Gd - Ga garnets that had been decomposed in HCl. It was necessary to correct for the considerable background due to gallium (86/735). As ETA-AAS is often used to determine analyte levels near to the detection limit, interferences from matrix elements become extremely important. These can be correc- ted by the use of good background correction, eliminated by matrix modification or removed, e.g., by extraction; some- times a combination of these measures is used. Background correction is almost essential for ETA-AAS determinations, and important advances in this area are the Zeeman and Smith - Hieftje methods.Zeeman-effect back- ground correction has been used for the determination of noble metals in geological and mining samples (S/C1161), in the determination of T1 in fly ash (86/1620) and for suppressing Po43- interference in the determination of Fe (86/1324). Other applications have been the determination of Se in coal (86/1689), and Ga in various inorganic matrices, where Mg(N03)2 matrix modification was employed (86/1631). The Smith - Hieftje method was used in the direct analysis of gallium arsenide for Cr, enabling calibration to be made with aqueous standards (86/1650). Matrix modification generally results in an improvement in sensitivity. Iridium was used as matrix modifier in the determination of Ag; it gave a significant sensitivity enhance- ment and the ashing temperature could be raised to 1000 "C for samples in HN03 (86/1749).For the graphite furnace AAS determination of trace Cd in rock samples, iron was added to enhance the Cd atomisation and to eliminate interferences (86/434). In the determination of Ga, a six-fold improvement in sensitivity resulted from the use of nickel as matrix modifier; the suppression of the Ga signal by HC104 was probably due to the formation of GaCl (S/802). Both nickel nitrate and barium nitrate gave considerable improvement in the sensitivity of Ge determination, whilst H2SO4 led to the depression of the Ge signal, due to formation of GeS (S/1108). In analysing minerals for In, the addition of palladium had the effect of raising the maximum tolerable ashing temperature to 1200 "C (aqueous) or 1000 "C (organic extract) (86/85).Palladium was also used as matrix modifier in the determina- tion of Se; the addition of a few pg enabled the charring temperature to be raised to 1100 "C (S/509). When traces of Ga, In and Tl were determined in geological samples after extraction from HBr into butyl acetate, the matrix modifier employed was vanadium (86/1045). Two reports of Sn determinations have utilised different matrix modifiers, nickel nitrate (86/35) and ascorbic acid (86/1617), which, when used in combination with platform atomisation in a tungsten carbide-coated atomiser, was found to control the depressive effect of the organic matrix resulting from the use of various chelating compounds.Five different matrix modifiers were examined, in conjunction with atomisation from a L'vov platform, for the determination of Sb; in the absence of a matrix modifier Sb was lost at 700 "C but the use of HN03 or copper allowed pre-treatment up to 900 "C, whilst nickel or molybdenum or palladium allowed pre-treatment up to 1300 "C. The best results were obtained with palladium at B0.8 Fg per 20 p1(86/1395). Platform atomisation, now established as a most useful technique for reducing matrix interferences, is often used in combination with matrix modification. Dittrich et al. (86/35) found that platform atomisation could reduce some of the matrix interferences that result from the forma- tion of diatomic molecules between trace and matrix com- ponents.A number of papers have reported some modification to graphite furnaces. Aleksenko et al. (S/36, 86/405) determined trace amounts of Au in geological samples with a pulsed electrothermal atomiser, and found that the initial heating stage could be used to remove volatile matrix elements; combustion products were extracted pneumatically. Tubes coated with TaC were used by Taddia (86K498) to determine low levels of Si in gallium arsenide, but pre-concentration was necessary as the detection limit was inadequate. Both TaC- or ZrC-coated tubes were examined for the determination of Ge in Turkish coal, and were compared with the use of nickel matrix modification. Either ZrC-coated tubes or nickel modification gave the best results, but the former were preferred as the lifetime of the tube could be extended up to 200 firings (86/C628).A pyrographite tube lined with Ta and W foil was used by Ma et al. (86/740) for the determination of Pb; they claimed that the method was free from interferences and there was no need to use matrix modification or standard addition. The use of a Ta-lined tube instead of a pyrolytically- coated tube gave greater sensitivity in the measurement of Ce,176R JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, DECEMBER 1986, VOL. 1 Gd, La, Lu, Pr and Tb in silicate rocks (S/507). Electrothermal atomisation AAS has been used for the direct analysis of solid samples. In the determination of A1 in solid cryolite, Yoshimura and Huzino (86/753) found that the absorbance could be increased by adding approximately 1% m/V carbon black, possibly (owing to the consequential rapid decomposition of the salt and the reduction of oxide.For the direct determination of Ag, Bi, Cd, Pb and T1 in rocks it was suggested that matrix interferences could be lowered by improved design of the atomiser or by separation of the evaporation and atomisation processes (86/C455). 4.3. Other Methods Kanipayor and co-workers (S/850, 86/C937) described a combined technique in which samples are atomised from a furnace via a slotted T-tube into an air - C2H2 flame. They were able to use relatively large samples (0.2 g), thus minimising problems from sample inhomogeneity , and the method was used for the direct determination of trace elements in geological samples.Cold vapour atomic absorption spectrometry is in routine use for the determination of Hg, and has been applied to the analysis of fly ash (86/93) and coal, where a comparison of wet-digestion methods led to the recommendation of an HN03 - HC104 - (NH4)2S208 digestion at 250-300 "C (86/719). Many methods that involve hydride generation and determi- nation by either flame or non-flame AAS have been published (Table 1). Lin et al. (S/634) measured the levels of Pb in rocks and found that Al, Cu, Fe and Se caused serious interferences; Se was removed by distilling off SeF4, and the other interferences were masked by o-phenanthroline. The determi- nation of Sn in cassiterite involved subliming the powdered mineral twice with NH41 in a test-tube, prior to dissolution in tartaric - ascorbic acids and determination by hydride genera- tion AAS (S/828).In the determination of Ge in silicate rocks and sulphide ores , hydride was continuously generated from the digested sample and was passed to an N20 - C2H2 flame (86/658). Automated hydride generation was used for the determination of As and Sb in acid-digested geological material, with AAS measurement in an electrothermally heated quartz cell atomiser (S/38). The same two elements were determined simultaneously by Branch and Hutchison who compared absorption of the hydrides into AgN03 solution followed by injection of aliquots into a graphite furnace with results obtained by passing the hydrides to a heated quartz cell (S/1107). An alternative method for Sb determination involved collecting stibine in a liquid N2 trap; rapid heating was used to convey the stibine to a graphite furnace, and the method gave a detection limit of 0.21 p.p.b.(86/1714). Wu (S/24, S/225) generated bismuth hydride from geological samples by reducing acid digests with KBH4; the hydride was led directly to an air - C2H2 flame and Fe was used to suppress interference from Co, Cu and Ni. The method was ten times more sensitive than direct nebulisation of solutions. Several papers refer to the hydride generation of selenium. In the analysis of coal the presence of H2S04 or HN03 in the analyte solution during reduction did not suppress the AA signal, but the presence of halide ions was necessary (86lC605). Acid decomposition was used in the analysis of zinc ore and HC1 was added to reduce Se(V1) to Se(1V); thiourea was also added to minimise Cu interference (S/175).Flow injection analysis was combined with automated hydride generation for the determination of Se down to 5 p.p.b. in rock samples; Cu and Ni interferences were controlled by 1 ,lo-phenanthroline and more than 50 digested samples could be analysed per hour (S/1101 , 86/C953). 5. INDUCTIVELY COUPLED PLASMA MASS SPECTROMETRY The first publications concerning the coupling of an induc- tively coupled plasma as the ion source with detection by mass spectrometry to produce a technique for elemental analysis appeared relatively recently, in 1980-81, and commercial instruments became available from two manufacturers in 1983. In an extremely short time, ICP-MS has achieved the position of an accepted, if not yet a widely used, analytical technique.Compared with conventional spectrometry, the use of MS as a detector would seem to provide better sensitivity, particularly for heavy elements, and certainly offers spectral simplicity and a consistently low background. The technique exhibits a wide linear dynamic range and the separation of analyte elements should be unnecessary. Mole- cular (i.e., oxide) interferences are said to be negligible. A further advantage of ICP-MS is the capability of measuring isotope ratios, with the possibility of using isotope dilution techniques. The various advantages of ICP-MS make it potentially very useful for analysing geological materials, and indeed many of the earliest applications of the technique are in this area.For example, an important paper by two of the original research- ers in ICP-MS, Date and Gray (86/115), described its application to the determination of 27 trace elements in geological samples, and the successful use of the method was demonstrated by determining 14 REEs in three international reference silicate rocks. Doherty and Vander Voet (86/1670) reported the ICP-MS determination of 14 REEs in solutions of digested rocks. They noted that operating parameters could be adjusted to minimise oxide formation, but it was necessary to correct for the residual amount of oxide. Date and co-workers have presented a number of confer- ence papers concerned with the application of inductively coupled plasma mass spectrometry to geochemical material: trace elements in rocks (S/C461), platinum group metals and Au in geological reference materials (S/C1186), REEs in rocks, minerals and concentrates (S/C1182) and trace ele- ments in calcium-rich samples such as limestones, dolomites and fluorites (86/C556).By coupling the high sensitivity of ICP-MS with the pl capacity of FI or ETA, they were able to analyse mineral fluid inclusion leachates for trace elements and to determine Pb isotope ratios (86/C1264). Other repor- ted applications of ICP-MS include those of Lichte and Meier (86/C547, 86/C790) describing the analysis of USGS CRMs, with particular interest in elements not easily determinable by other methods, e.g., Cs, Th and U. They also determined 0 s isotope ratios from the cretaceous zone in New Zealand, Pb isotope ratios in galena and, in collaboration with Church, reported the use of Pb isotopic composition as a means of fingerprinting ores (86E1113).This is obviously an area of special interest, as it has also been investigated by other workers (86/C1112). The determination of trace elements in natural silver (86/C1260) and p.p.m. levels of Th and U in tourmalines (86/C1267) have also been reported. Compared with publications from instrument manufactur-JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, DECEMBER 1986, VOL. 1 177R ers, which generally extol the advantages of their particular instrument, it is refreshing to read papers such as that written by Pickford and Brown, who compared inductively coupled plasma mass spectrometry and inductively coupled plasma atomic emission spectrometry for the analysis of samples with complex matrices, including geochemical materials.They found the two techniques to be essentially complementary: ICP-AES had limited sensitivity for heavy metals such as Pb whilst ICP-MS suffered from practical limitations in the form of molecular ion interferences, especially for elements such as Ca, Fe and V. Nevertheless, ICP-MS is attractive because of its high sensitivity for many elements and its freedom from the spectral interferences seen in ICP-AES (S/C462). It is to be hoped that more realistic appreciations of the technique will be reported in the future. Date and co-workers (86IC1109) have in fact identified several areas where problems may occur in ICP-MS. In addition to difficulties with sample introduc- tion, which are common to ICP-AES, interferences can be caused by high total dissolved solids or by molecular peaks from either the medium used for sample dissolution or from the sample matrix.Boorn et al. (86/C1180) have commented that, as acid dissolution is needed at some stage of sample preparation for most geological samples, any spectral interfer- ence from acid-derived ions (ClO, C102, SO and HSO) becomes very important. The use of HN03 in the final sample solution is said to eliminate such interferences. High concen- trations of matrix components can cause suppressions of ion signals, the suppression being proportional to the atomic mass of the matrix element. Interferences from isobaric overlap of metal oxides and from double charged ions and matrix ions such as C10+, N2+, NO+, Ar+ and Ar2+ limit the determina- tion of some elements.Matrix matching, standard addition, external calibration graphs and internal standardisation are recommended to overcome these problems. Although most reported uses of ICP-MS involve sample introduction by nebulising solutions, it can be predicted that alternative methods of introducing the sample will be investi- gated. Already Date (86/C1264) has utilised FI and ETA for the ICP-MS analysis of pl samples, and Gray (86/196) has reported the use of laser ablation in ICP-MS. 6. COMPARISON OF METHODS Many papers refer to the comparison of two or more analytical methods, especially when a new procedure or technique is being recommended in the place of existing methodology.Most of these comparisons state simply that the results “compared well” or were in “good agreement”; papers that make pertinent points concerning precision, accuracy, speed or ease of use of a method are relatively rare. Meus et al. (860345) compared flame atomisation atomic emission spectrometry with d. c. arc atomic emission spec- trometry for the determination of K and Na in coke and found that the two methods were equally accurate; d.c. arc AES gave shorter analysis times but the precisions were worse. Good agreement has been reported between atomic absorp- tion spectrometric methods (both flame and non-flame) and a variety of other techniques, such as: titrimetry, for Ba in ceramics (S/816); photometry, for Fe in granite rocks (86/C631); fluorimetry or AES, for Eu in phosphate minerals (S/580); and gravimetry, for Si, where it was concluded that AAS, although much faster and more suitable for batch analyses, was not sufficiently accurate (86K632).Reports of reliable analyses by methods that use solid samples, whether by direct insertion or slurry injection, are necessary if these techniques are to be accepted as viable alternatives for routine use. For the determination of trace Rb in granite rocks, Bao-Chuan and Hua (S/C326) used direct analysis by graphite furnace AAS, and claimed that standard addition of Rb solutions gave good agreement with the analysis of dissolved samples by AAS. In the determination of As, Cd and Pb in 90 samples of pulverised coal ash, the results obtained by slurry injection AAS were in good agreement with measurements made either by wavelength dispersive XRF spectrometry or by deuterium arc background corrected AAS of dissolved samples (S/C265, SK572).Many comparisons of inductively coupled plasma atomic emission spectrometry with other techniques, especially atomic absorption spectrometry, have reiterated the well-known capabilities of ICP-AES. In the analysis of cement, the precision of analysis was worse for ICP-AES compared with AAS, but the methods were equally accurate (86/1298). Three techniques were compared with ICP-AES for the analysis of calcined bauxites: gravimetric analysis, for Si and Al, was slow; colorimetric analysis, for Fe and Ti, was laborious; and AAS, which was found to be as satisfactory as ICP-AES for determining Ca, Cr and Mg (S/666).Voinovitch et al. (S/95) compared four techniques for determining Si02 and A1203 in silicate materials. They found that ICP-AES or XRF values for Si were more accurate than those given by AAS or d.c. arc AES, and they suggested that the AAS results were affected by carbon deposited on the burner rim, due to the reducing flame. The results for A1 given by the four techniques were similar, but again the ICP-AES or XRF methods were preferred. For the determination of P in rocks and minerals, ICP-AES was found to have similar accuracy and precision, but was simpler and faster, compared with a colorimetric procedure (SK445). As rival claims from proponents of analytical techniques are often difficult to compare objectively, a paper that described the comparison of an inductively coupled plasma with a direct current plasma using the same spectrometer is worthy of note.A slight increase in the stability of the ICP was found to be offset by a decline in the peak to background ratio for many elements. Calcium and Mg could be determined more precisely by ICP-AES whilst K and Si were better by DCP-AES. For the determination of REEs, the DCP was recommended due to increased line intensities (S/C733).178R JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, DECEMBER 1986, VOL. 1 7. ANALYSIS OF CERTIFIED REFERENCE MATERIALS Many publications refer to the analysis of geological certified reference materials as a means of assessing the accuracy of a new or modified analytical procedure. It is perhaps predict- able that such papers generally report “good agreement” between the determined concentration and the certified concentration of the particular element being studied.Only a few publications are noteworthy in that they report either the analysis of a new CRM, the detailed analysis of an existing CRM or the analyses of a series of CRMs. A report from the European Community Bureau f o r Reference Materials described homogeneity and stability tests for preparing a coal reference material (BCR No. 40). Various analytical techniques, including AAS and ICP-AES , were used by the 22 European coal analysis laboratories that participated in the certification, and certified analytical values for As, Cd, Co, Cr, F, Hg, Mn, Ni, Pb and Zn were published (S/200). A sample of city waste incinerator ash was distributed in 1983 by the same Bureau for Reference Materials (BCR No.176); the levels of Cd, Cr, Cu, Ni and Zn in this material have been determined by Taylor et al. (86/1466), using an ICP-AES procedure. A request from the South African Committee f o r Certified Reference Materials led to the preparation of three reference materials from South African coals. Approximately 15000 results were received from the 28 laboratories that participated in analysing the three coal samples (SK1194). The certification of two gold ores as reference materials has been described by Steger and Bowman (86/1276). Seventeen laboratories contributed results and recommended values were published for Ag, Au, Cu, Fe and S. The analysis of four new Canadian iron-formation reference materials for Sc, Y and REEs by ETA-AAS has been reported (S/507).Reports of single-element determinations in CRMs include: Bi in 83 geochemical reference samples (S/227), Ga in six South African primary rock standards and in 12 secondary rock standards (S/228, S/1229) and Co in six South African primary rock standards (S/C1195). Amongst publications concerned with the analyses of several standard materials are the determination of 22 major and minor elements in Geological Survey of Japan (GSJ) reference rocks (86/1013), the determination of ten major and 35 minor elements in three GSJ silicate rocks (86/1079) and the analysis of USGS rocks (86/76). Rare earth elements have been determined in 15 international sediment samples from France, East Germany, Canada and the USA (86/1804), and in Russian standard rocks where results of analyses carried out in 1973 were compared with 1983 results (S/219).Table 1. SUMMARY OF ANALYSES OF MINERALS AND REFRACTORIES Technique ; atomisation; analyte form -; -; L ?Jnm - - 328.1 338.289 328.1 - - - 309.3 - 309.3 - - - Matrix Bio-geochemical, plant tissues Geological material, plant products Ores Metals, ores Concentration ngml-1 Sample treatment procedure or by storage in borosilicate glass containers Pt or Pd as carrier, dissolve prill in aqua regia Dissolve in HC1- HN03, add triammonium citrate and NH40H Solvent extraction by formazan dissolved in dichloromethane, wash with alkaline citric acid buffer, strip with 1 M HNO, Decompose in HCl - HN03 (2 + l), evaporate, dissolve in NH40H with added oxalic acid then centrifuge to remove Ca Extract with zephiramine from 0.1-1.2 N HBr solution Dissolve in HN03, add Ir as matrix modifier; ashing at 1000 “C Comparative statistical study on 4 SRMs Study of sorption losses by filtration Fire assay: for prill mass ca.0.02 mg use Reference S/1118 SIC1 188 861383 86lC601 8611018 8611031 8611749 s195 AA or AE; ICP; L AA; F, AE; DCP; L air - C2H2; L - Trace levels Carbonate rock 0.25-1 pg g-1 AA; F, air - C2H2; L Ores Trace levels >4.5 pg Major levels AA; -; L Geochemical material Silicates AA; ETA, Zeeman; L AE or XRF or AA; ICP or d.c. arc or F; Lor S C2H2; L AA; F, N20 - AA ; ETA ;-- Refractories Cryolite Fly ash Decompose in HF - H2S04, evaporate, add HC1 solution Add 1 Yo m/V carbon black to improve determination of A1F3 and AlPO, Fuse with LiB02 at 1000 “C for 15 min, dissolve in dilute HN03, add K; study of matrix interferences amongst Al, Ca and Si Decompose 0.05-0.5 g sample with HClO, - HN03-HF and KMnO,, evaporate, dissolve residue with 6 M HCl - 20% KI - 10% AIC13 - 10% ascorbic acid; generate hydride with 1% NaBH, - 2 M HC1- 5% malic acid S1830 861753 86lC1584 S138 Use KBH, to generate hydride S1139 Geological material >0.05 pg g-1 AA; ETA, Hy - quartz cell; G Geochemical material >1.4ng AF; ETA, Hy - quartz tube; G AA; ETA, Zeeman; S Coal fly ash 0-200 pg g-1 Grind to 4 0 pm, suspend in 1% HN03 S/C265, with LiB02, Li2B407, LiN03, SIC572 Ni(N03)2 added in solution, homogenise by ultrasonic agitation during sampling179R JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, DECEMBER 1986, VOL.1 Table 1. SUMMARY OF ANALYSES OF MINERALS AND REFRACTORIES-continued Technique ; atomisation ; analyte form AA; ETA; Hy- quartz cell; L or G Element As As Au Au Au Au Au Au Au Au Au Au Au Au Au Au B B B Ba Ba Ba Be Be Bi Bi Bi Bi hlnm - - 242.8 267.59 - 242.8 - - - - - - - - 242.8 - - 249.678 249.7 - 553.6 - - - - 223.1 - - Matrix Geological material Concentration Sample treatment Reference S11107 86140 S130 Sl36 s1224 s1499 Sl1118 SIC1188 SIC1191 86130 861405 8614 16 861 1276 8611368 8611637 8611710 S164 SIC696 861662 S1134 S1816 SIC1166 861407 861 14 12 Sl24 Sl225 S1227 8611076 Decompose in HNO, - HC104, extract with HCl; either absorb into AgN0, solution for furnace injection, or atomise Hy directly in hot quartz cell Study of interferences Cu ores, industrial materials AA; F, air - C3H8 - AA;-;L C4H10; L Cu ores, concen- trates, residues 0.0410 g ton-] Heat in muffle furnace at 500-600 "C; digest with HN03 - aqua regia - HCl; extract with IBMK then wash with 10% HCI, centrifuge Place powdered sample (S60 mg) in graphite rod atomiser at 12O0-130O0C, remove ash before pulsed atomisation of analyte Dissolve in "reverse aqua regia," extract with 2-mercaptobenzothiazole in butyl acetate Decompose with aqua regia, treat with HCI, extract into IBMK; Zeeman background correction See Ag, ref.Sl1118 Rocks >0.5 ngg-* AA; ETA; S Geological material AA; ETA; L Rocks, ores, RMs >1 ng g-1 AA; ETA; L Bio-geochemical, plant tissues Geological material, plant products Beneficiation plant products Ores ng ml-1 - - 0.1 pg g-1 >0.0002 pg g-1 10-7-10-30/o 0.24,1.33 pgg-l >1 ng ml-1 -- ; ; L AA or AE; ICP; L See Ag, ref.SIC1188 AA; ETA; L On-line analytical instrumentation AA;-; L Separate using tri-n-octylamine loaded on Powder placed in channel of graphite rod Evaluation of methods polyurethane foam, desorb with thiourea Rocks Rocks AA; ETA; S or L AA or AE; -; LorS Various Sulphide ore CRMs Grind to -74 pm, mix and bottle in 200-g units; also blend with CRM MA-1, grind and bottle; interlaboratory study Digest with HCl - HN03; to avoid scatter by Al, extract with0.1% mlVsolution of Aliquat 336 in diisobutyl ketone; non- dispersive AFS and tetrabromoaurate complexes into IBMK and DIBK Pre-concentrate as hydrochloroauric acid in 5-20% aqua regia or dilute acid solutions with crosslinked polymethacrylates; elute with 0.5% Na2S03 solution H2SO4 (1 + 2) - HNO,; takes 30-60 min after reaching 150 "C add AlC13 solution constituents and the bulk of the excess of potassium salts using HClO, Mix 100 mg of sample with 200 mg of graphite powder containing 0.002% of PdCI2; pack in upper part of electrode above mixture of NaCl - graphite (1 + 1) boiling AcOH for free BaO Study of solvent extraction of the tetrachloro- Dissolve under pressure at 150-158 "C in Dissolve in HN03 - HF; volatilise Si, Fuse with K2C03, separate B from major Dissolve in HBr - HF for total Ba; leach in Geochemical material AF; F, air - C2H2; L Geological material Trace levels AA; ETA or F, air - C2H2; L Low-grade ores >0.05 pg g-1 AA;-;L Borides AA;-;L Coal ash, silicates Rocks AE; ICP; L AE; ICP; L Rocks, ores, soils 0.002-1 Yo AE; d.c.arc; S Pb - Zr - Ti piezoelectric ceramics Granite pegmatites Geochemical material Coal ash AA; F, N20 - C2H2; L C2H2; L AA; F, N20 - AA; ETA; L AE; ICP; L >5 g-l >5 x 10-11 g Trace levels vg g-' >0.3 ng g-1 Separation of Ba through precipitation of Extract acetylacetonate complexes into MePh %SO4 as carrier Digest under pressure in Parr bomb with Simple hydride generator Decompose with HC1 - HNO,, dissolve residue HN03 - HF in HC1, evaporate and add HCI - FeCl, solution; generate hydride using KBH4 solution Either hydride generation and heated quartz cell or solvent extraction and C tube atomiser Generate hydride with KBH,; non-dispersive system Minerals, lead Geological material AA; Hy, F; G AA; Hy, F, air - C2H2; G Geochemical RM Geological material AA; ETA; G or L - 0.1 pg g-1 AF; Hy; G180R JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, DECEMBER 1986, VOL.1 Table 1. SUMMARY OF ANALYSES OF MINERALS AND REFRACTORIES-continued Technique ; atomisation; Concentration analyte form >0.35 ngml-l AE; Hy, ICP; G Element Bi C Ca Ca Ca Ca Cd Cd Cd Cd Cd Cd c1 c o c o c o c o Cr Cr Cr Cr c u c u c u c u c u Eu Eu h/nm Matrix 223.061 Waters, metals , geological RM Sample treatment Acidify with 1 M HCI, generate hydride using 1% rnIVNaBH,solution with 1% rnlV NaOH To determine carbonate mineral concen- trations: decompose at characteristic temperatures with the release of C02 Fuse with Na202 in glassy carbon crucible Reference 861C1127 861C1602 86/41 861415 861417 861C1584 s177 SIC572 8613 1 1 861434 861737 8611018 861234 SIC1 195 861735 8611299 8611748 861735 86/75 1 8611 04 1 8611650 SIC1171 861737 8611464 8611619 8611748 S1580 SIC1164 >1 pg g-l of carbonate mineral 0.05-3.0% CaO AE; MIP; G AA; F, air - C2H2 or N20 - CZH2; L 0.98-4.19% CaO AA; F, air - Soils, sediments Chromium ores, concentrates Dissolve in 10% HNO,, add La(N03)3 Tungsten ore concentrates C;H, - C4H10; L AA; F, air - C2H2; L C2H2; L AF; F, air - C2H2; L AA; ETA, Zeeman; S AA; ETA; L AA; F, N2O - Ferrous metallurgy Fly ash discharges Dusts dissolved - 8-20% CaO >0.004 pg ml-1 See Al.ref. 861C1584 Semiconductor alloys Coal fly ash Coal See As. ref. SIC572 Ash at 115-240 "C in W furnace; treat with a rn-xylene or CHCI3 solution of dithizone to extract Cd Add Fe to eliminate interferences Acid digestion; separate analytes from matrix by sorption of metal iodide complexes on anion-exchange resin See Ag, ref.8611018 Rocks Iron ores, limestone >1.4 X 10-log Yg 8-l AA; ETA; L AA;-;L 0.20-1.5 pg g-l 0.008-4.5 Yo AA; F, air - C2H2; L AA; -; L Carbonate rock Silicon nitride, glass CRMs Decompose under pressure with HF - HNO, - AgN03 at 160 "C for 16 h; remove precipitated AgCl, measure excess of Ag in solution with H3P04; cation-exchange using AG50W-X8 resin and HCI - acetone solutions as eluents 160 "C Dissolve in HC104 - HCI - HF, fuse residue Decompose powdered sample in HC1 at 140- Dissolve Co in aqua regia Complex with 1-nitroso-2-naphthol at pH 6.8-8.4, extract with BuOAc in presence of ammonium tartrate See Co, r-1735 Decompose by heating with HF - H2S04, add 2 M NH4C104 as interference inhibitor Add 1 ml85% H3P04 to 0.2 g of sample, homogenise, heat for 6 h on hot-plate, add H,O; shake and centrifuge Remove surface impurities by etching, shatter into small fragments ( 4 0 mg), weigh accurately to 0.01 mg and introduce to furnace Dry in air, heat to 90 "C for 24 h, grind to <44 pm for suspension in H 2 0 See Cd, ref.861737 Silicate rock RMs 0.36212 pg g-1 AA; F, air - CzH,; L Doped Gd - Ga Tungsten carbide Ores garnet >2.5 pg g-1 - Trace levels AA; ETA; L AA; ETA; L AA; F; L Doped Gd - Ga garnet Vanadoti tano- magnetite Geochemical material AA; ETA; L AA; F, air - CzH,; L AA; F, N2O - C2Hz; L Gallium arsenide 0.23-1.0 pg g-1 AA; ETA; S Soils g-' g-' >loo pg g-1 AA or AE; F or ICP; s AA; -; L Iron ores, Steel, copper ore limestone AE; laser, DCP; S Laser ablation using relatively low energy, high repetition rate Nd:YAG laser; mix ore with cellulose binder, press at 20 000 lb in-2 into pellet Dissolve with KClO, (1.5 g) and concentrated HN03 - HF (2 + 1) in PTFE PFA vessel in microwave oven at 477 W for 3 min See Co, ref.8611748 Dissolve in H2S04, extract with 1 M bis(2-ethylhexyl) phosphate in cyclohexane at pH 2.0 Fuse with KHF2, leach with HF; filter and dissolve with HC104 - HCI for cation- exchange separation o/o levels AA; F, air - C2H2; L Sulphides Ores Phosphate minerals Trace levels 23-157 pg g-l AA; F; L AA; ETA; L Industrial materials AA; ETA; LJOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, DECEMBER 1986, VOL.1 181R Table 1. SUMMARY OF ANALYSES OF MINERALS AND REFRACTORIES-continued Technique; atomisation; analyte form AE; F, NzO - CzH2; L Element Eu Fe Fe Fe Ga Ga Ga Ga Ga Ge Ge Ge Hg Hg Hg Hg In In K K K K La La Li Li Mg Mg Mg Mn Mo Mo Unm 459.40, 462.72, 466.19 259.94 248.3 - - - - - 294.4 - 265.2 265.1 253.7 - - - 303.9 - - - - - - 441.82 - - - - - - - - Matrix Rocks Concentration >10-7% Sample treatment Decompose with HClO, - HF Reference 861371 Sl84 861C631 8611 324 S1228 St802 St1229 8611045 8611631 S11108 861C628 861658 86/93 861719 861750 8611346 86/85 8611045 S176 861 1327 8611345 8611349 8611 02 1 8611831 SIC254 8611 4 12 8614 1 861417 8611095 8611277 SIC283 Geological material Granitic rocks AE; DCP; L AA; F, air - AA; ETA, C2H2; L Zeeman; L C2H2; L AA; ETA; L AA; F, N20 - Study of matrix effects Grind to 100-200 pm, dissolve under pressure Suppression of interferences with HF - HN03 at 110-120 "C for 1 h - O.5-1.2% 103 ng ml-1 Phosphate Rock RMs Selective ion-exchange procedure Environmental material Rock RMs Geological material Use Ni as matrix modifier AA; ETA; L AA; ETA; L Selective ion-exchange separation Extract metals from 5.5 N HBr medium into n-BuOAc; add V in 2 N HN03 as matrix modifier Dissolve with H20 - HN03 - HF (5 + 1 + 1) then with H20 - HN03 (4 + 1); add Mg(NO& as matrix modifier, use standard additions method Matrix modification by Ni(N03)* and Ba(N03)2; thin-layer separation methods are described HN03 - H2S04 (24 + 24 + 1) at 100 "C for 2 h residue with HF, extract Ge into CCl, - 9 M HCl then into distilled H20, generate Hy with NaBH, Dissolve under pressure with HC104 - Digest with H3P04 - HF - HN03, treat Digest with HN03; amalgam system Digest in HN03 - HClO, - (NH&S208 at 250-300 "C using Bethge apparatus Decompose in aqua regia, add K2Cr207, transfer to Hy generator containing KBH,, measure non-dispersive AF at 350 "C - Dissolve under pressure with HC104 - HN03 HF - HCl, extract with NH41 into IBMK; add Pd as matrix modifier See Ga, ref. 8611045 Use CsCl as ionisation suppressor Phosphorus flue dust, coal fly ash, Cu ore 50-830 pg g-1 AA; ETA, Zeeman; L Semiconductor microsamples AA; ETA; L Coal >0.025 pg ml-1 1-430 pg g-1 AA; ETA; L Silicate rocks, sulphide ores Fly ash Coal 0.02-0.16 pg g-1 >0.08 pg g-1 >2.1 ngg-1 AA; cold vap.; L AA; cold vap.; L Geochemical material AF; ETA; G Geochemical CRMs Minerals, river sediments, coal fly ash Geological material Rubidium potassium dihydrogen phosphate Silicon Coke Trace levels 0.085-40 pg g-1 AA or AF; -; - AA; ETA; L AA; ETA; L AA; F, air - C2 H,; L AE; F; L AE; Ford.c.arc.; LorS AE or AA; -; L Treat with HF - H2S04 - HN03 Digest with H2S04 - HC104 for flame Characterise for pharmaceutical use by Dissolve in HC1 or HN03, use standard Without pre-concentration; study of photometry leaching into injection fluids additions method interferences, including Th, Ti, Zr and rare earths Decompose with HF - HN03 - HC104, add See Be, ref. 8611412 See Ca, ref.86/41 H2S04 Trace levels - 0.016-0.087 pg ml-1 - Glass ampoule Ca-rich rare earth Rocks fractions AE; ETA; L >60 pg 1-1 Silicate rocks >2.8 pg AE; ETA; L Coal ash Chromium ores, concentrates Trace levels 3.0-25% MgO AE; ICP; L AA; F, air - C2H2 or N20 - C2H2; L AA; F, AA; F, air - C2H2; L N20 - CZH2; L Ferrous metallurgy Alumina ceramics discharges See Ca, ref. 861417 Dissolve in H3P04 - H2S04, separate by cation exchange using 4% cross-linked resin, elute with 0.50 M oxalic acid Fuse dried sample (1 + 6) with LiB02 at 1000 "C for 2 h, treat with HCl, add Fe and Ca to control interferences Separate Mo using a cation-exchange resin in 1 . ~ HC1; other elements by direct determination in solution of sample Granite, amphibolite, biotite Refractory materials, sludge 0.0440.631 Yo AA; F, air - C2H2; L AE; ICP; L Soils, sediments, >0.06 pg g-l AE; ICP; L Treat with 6 M HC1 in capped tube at 120 "C, 86/72 rocks extract into heptan-2-one182R JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, DECEMBER 1986, VOL.1 ~~~ Table 1. SUMMARY OF ANALYSES OF MINERALS AND REFRACTORIES-continued Technique ; atomisation; analyte form AE; d.c.arc.; S Unm Matrix - Asphaltite ash Concentration Minor and trace levels Trace levels >0.5 pg g-l Trace levels - 0.5 pg ml-1 50-500 mg 1-1 Trace levels - Minor and trace levels >2 pg g-' YO levels Trace levels - >lo18 atoms cm-3 - >0.07 mg 1-1 Trace levels Trace levels - vg g-' pg g-l 4.4pg >1.5 pgg-l 50-2000 pg 1- 1 pg ml-1 >5% 0.05-9 pg g-1 Sample treatment Reference Element Mo Mo Mo Na Na Na Nb Nb Nd Ni Ni Ni Ni P P P P P P Pb Pb Pb Pb Pb Pb Pb Pb Pb Pd Pt Rb Rb S S 86lC569 86lC634 861692 8611327 8611345 8611349 s1905 861438 SIC457 86lC569 861735 8611619 8611748 s152 SIC285 SIC445 861437 86lC850 8611038 SIC572 Sl634 861737 861740 861752 86/C1112 86lC 1 1 13 8611296 86lC1585 86130 S11118 976 SJC326 SIC299 SIC728 Use NaDDC or other organic substances mixed with graphite powder and sample ( 5 + 1 + 2) to buffer d.c.arc - Fuse with LiB02, dissolve in 15% VlVHC1, See K, ref. 8611327 See K, ref. 8611345 extract into 4% solution of TOP0 in IBMK 203.84 Geological material 313.3 Rock, soil, stream - S i 1 icon - Coke sediment AE; ICP; L AA; F, AE; F; L AE; Ford.c.arc.; LorS AE or AA; -; L AE; F, AE;arc, N20 - C2H2; L N20 - C2H2 ; L Plasmatron; S AE; rcp; L - Glass ampoule 405.8 Niobite, tantalite See K, ref.8611349 Fuse with KHS04; add Fe (10 mg ml-1) and 5% HF solution as buffers Mix (1 + 1) with powdered C, blow into 100-A double-jet plasma Dissolve under pressure in HCI; use Y as internal standard See Mo, ref. 86lC569 - Minerals, ores, rocks - Yttrium aluminium garnet (YAG) - Asphaltite ash AE; d.c.arc.; S - Doped Gd - Ga - Sulphides garnet AA; ETA; L See Co, ref. 861735 AA; F, AA; F; L AE; arc; S air - C2H2; L See Cu, ref. 8611619 - Ores - Phosphorites See Co, ref. 8611748 Decompose in electric arc at 4000-5000 K; identify products Anodise, dissolve Si02 film in 0.2 M HF, determine amount and depth of Si; to other etching solutions add KF solution, evaporate, dissolve residue in H20 by ultrasonic mixing; depth profile at 120 "C for 45 min, cool, add H3B03 solution Digest under pressure with HC1- HN03 - HF Suitability of several spectral lines examined - Silicon wafers AE; filament vaporisation - ICP; L 216.62 Rocks, minerals AE; ICP; L 178.29 Geochemical material 213.618, Refractory 214.914 materials AE; ICP; L AE; ICP; L Separate using Dowex 50WX8 cation-exchange resin Dissolve sample, add H3B03 - HOAc; after cooling add HN03 - Na2Mo04 - NH4V03 and extract with IBMK See As, ref.SJC572 Tungsten trioxide AA; ETA; L Coal fly ash Rocks AA-; ETA, Zeeman; S AA; Hy; G Reaction with NaBH, - H202 in dilute HC1 after treatment for interferences by Al, Cu, Fe and Se See Cd, ref. 861737 Use pyrolytic graphite tube lined with W and Ta foil Mix powdered sample with buffer (S + 10% C + 18% NaF) to suppress Fe interference by forming FeS Use of 203Tl- 205Tl as internal isotopic ratio standard for Pb isotopic analysis Potential use of Pb isotopic analysis for regional reconnaissance studies Dissolve in hot H20 - mixed acids, precipitate Pb with Cr20+- in NH4 AcO solution at pH 3-4; use AAS for residual traces Background correction necessary for good agreement with the dithizone method See Au, ref.86130 See Ag, ref. Sl1118 Iron ores, limestone Water sediments, coal fly ashes Basic, ultrabasic rocks AA;-;L AA; ETA; L AE; d.c.arc.; S Galena, Pb-rich minerals Geochemical material, galena Ores MS; ICP; L MS; ICP; L AA; -; L combined with chemical analysis Magnesium AA; -; L aiuminium silicate Ores 0.1 pg g-1 Bio-geochemical, ng ml-l Rubidium potassium - plant tissues dihydrogen phosphate Granite Trace levels AA;-; L -; -; L AA; F, air - C,H,; L See K, ref.Sl76 AA; ETA; S Grind to 300 mesh; take up to 6 mg of sample in Grind sample to particle size <10 pm, capillary tool prepare 5% aqueous slurry for transient flow-injection Babington type nebuliser different fractions ASTM procedure D-2492-80 for extractions of Coal 0.33% AE; ICP; S Coal - AE; ICP; LJOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, DECEMBER 1986, VOL. 1 183R Table 1. SUMMARY OF ANALYSES OF MINERALS AND REFRACTORIES-continued Element Unrn Sb Sb Sb Sb Sb sc Se Se Se Se Se Se Se Se Si Si Si Si Si Sm Sm Sn Sn Sn Sn Sn Sn - - - 217.6 - 603.62 196 196.0 - - - - - - - 251.6 251.6 251.6 251.6 443.43 - 235.5 - - 235.5 - 286.3 Matrix Geological material Geochemical material Cu ores, industrial materials Geochemical material Rocks, soil, sediments Rocks Zinc ore Geological material Geological material Geological material Coal ash, sediment Coal Rocks, geological RM Coal Silicates Barium titanate Gallium arsenide Rocks Fly ash Apatite Industrial materials Ores, concentrates, residues Cassiterite in rocks Sediments Rock, soil, stream Basic, ultrabasic Rocks, minerals sediment rocks Concentration >0.05 pg g-1 >0.37 ng - Trace levels >0.21 ng g-1 >10 pg I-' g-l g- >5 ng g-1 - - 0.4-2.6 pg g-1 >5 ng g-* 0.3-2.6 pg g-1 Major levels 0.23% >2 CLg g-l 5040% (Si02) 40-56% Si02 2.6-18.1 pgg-l - O.1-1.7% - Minor and trace levels g-l >0.8 pg g-1 O.O5-17% Technique; atomisation; analyte form Sample treatment AA; ETA, AF; ETA, See As, ref.Sl38 See As, ref. Sl139 Hy - quartz cell; G Hy - quartz tube; G A A ~ F , air - C3Hs - AA; ETA; L C4H10; L AA; Hy, ETA; G AE; F, AA; Hy; G NzO - C2H2; L AA; ETA; L AA; FI - Hy; L AA; ETA, Hy - quartz cell; LorG AF; Hy; L AA; Hy; L AA; FI - Hy; L AA; ETA, Zeeman; L See As, ref. 86140 Tests on 5 matrix modifiers: HN03, Cu, Ni, Mo and Pd; dissolve sample with HCl, add Pd at 2 pg per 20 pl, add ascorbic acid Reduce with NaBH, to stibine, collect in (2.5% dv) liquid nitrogen trap then release by rapid heating of trap See La, ref. 8611831 Dissolve in HN03 - HCl, heat with HClO, - HF, add HC1; minimise Cu interference by adding thiourea Decompose with HClO, - HF - HN03, separate with thiol cotton fibre, add Pd as matrix modifier Digest with HF - HCIO, - HN03 for FI technique; add 1 ,lo-phenanthroline See As, ref.Sl1107 Suppress interferences by addition of complexing ions such as Cl- and Fe3+ Dissolve with H2S04 - HN03 - sulphamic acid, generate hydride using NaBH, (0.16%) + 0.1 M KI Digest with HF - HClO, - HN03; introduce 1 ,lo-phenanthroline into flow to control Cu and Ni interferences HN03 - HC104; separate by distillation in HC1- HBr solution Decompose with HN03 - HF, digest with AE or XRF or AA; See Al. ref. Sl95 ICP or d.c. arc orF;LorS AE; ICP; L AA; ETA, platform; L AA; F, AA; F, AE; ICP; L N2O - C2H2; L N20 - C2H2; L AA; ETA; L AA; F, N20 - C2H2; L AA; Hy; G AA; F, -; L AA; F, AE; d.c. arc; S N20 - C2H2; L AA; F, N20 - CZH2; L Decompose under pressure with HCl at 140 "C for 4 h, filter; treat insoluble part with HF (1 + 9) and H3BO3; use separately, sum results for soluble and insoluble Dissolve with HN03 - HCl in sealed tube at 100 "C for 2 h, add calcium nitrate solution as matrix modifier Dissolve under pressure with aqua regia - HF at 105 "C for 1-2 h; add H3B03 and H20 See Al, ref.86lC1584 Dissolve in hot HN03, evaporate to dryness, dissolve in HClO,, extract into cyclooctane containing 0.1 M bis-(2-ethylhexyl) phosphate See Eu, ref. SIC1164 Digest with HN03 - HF, add Na2C03 and Reference Sl38 9139 86140 8611395 8611 71 4 8611831 S1175 Sl509 s11101 Sill07 861436 861C605 861C953 8611689 995 s1504 861C498 861C632 861C1584 965 SIC1 164 SIC361 borax, fuse at 900-1000 "C, cool and dissolve in HCl - HN03 aqueous tartaric - ascorbic acid, decant and wash the insoluble residue Investigation of various methods for selective 861C638 dissolution from Sn-bearing minerals See Mo, ref.861692 861692 Sublime twice with NH41, dissolve in S1828 See Pb, ref. 861752 861752 Heat sample with cyanide fusion flux, dissolve in H20 - HC1- HF, evaporate and treat with HC1- H3BO3; chelate extraction using BPHA - toluene 8611473184R JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, DECEMBER 1986, VOL. 1 Table 1. SUMMARY OF ANALYSES OF MINERALS AND REFRACTORIES-continued Element Sn Sn Sr Ta Ta Ta Tb Th Th Ti Ti Tl Tl Tl Tl U U V V V W W Y Y Zn Zr Zr Various (42) Various (34) Various (20) Various (17) Various Technique; atomisation; hlnm Matrix Concentration analyte form 224.6 286.3, Rocks 0.1-10 pg g-1 AA; ETA; L - Rocks, minerals - AA; F, N2O - C2H2 ; L - Rocks, ores, soils 0.002-1% AE; d.c.arc.; S 271.5 Niobite, tantalite 100-1000 mg 1-l AA; F, - Minerals, ores, Trace levels AE; arc, 271.467 Columbite - 1040% Ta205 AE; d.c. arc; S N20 - C2H2; L rocks Plasmatron; S tan tali te - 283.73 - - 364.2 - - - 276.8 367.0 - - - - 407,44, 400.88, 257.14, 239.71 - 332.79 613.21 - 339.20 339.2, 349.6 - - - - - Industrial materials - AA; ETA; L River sand 0.01-1% (Tho2) XRF or AE; arc; S Tourmaline >0.1 pg g-1 MS; ICP; L Refractory - AE; ICP; L Niobite, tantalite 10-100 mg 1-1 AA; F, Environmental - ASV or AA; materials ETA; L Geological material Trace levels AA; ETA; L materials, sludge N20 - C2H2; L Geological material City waste incineration fly ash Ores Tourmaline Refractory Asphaltite ash materials, sludge Sedimentary rocks >9 Pg 2.8 pg g-1 0.027-72.09% u3°8 >o.1 pg g-' - Minor and trace levels Trace levels AA; ETA; L AA; ETA, Zeeman; L AE; ICP; L MS; ICP; L AE; ICP; L AE; d.c. arc; S AA;-;L Silicate rocks, >0.02 pg ml-1 AE; ICP; L W concentrates, alloys Ores, concentrates, Major levels AE; ICP; L River sand 0.01-1% (Y203) XRF or AE; arc; S Rocks >8 pg 1-1 AE; F, Soils CLg g-l AA or AE; For ICP; S River sand 0.01-1% (ZrO,) XRFor AE; arc; S Silicate rocks Trace levels AE; DCP; L alloys N20 - C2H2; L Coal Trace levels NAA or AE or AA; PorF;L Rocks, soils Major and trace AE; ICP; L Silicon nitride Trace levels AE; ICP; L levels Nb - Ta minerals Major and minor AE; ICP; L levels Periclase - AE; laser, (6) d.c.arc; S Sample treatment Reference 8611 617 Digest with HF - H2S04, evaporate; fuse with LiB02, dissolve in 3.2 M HCl, add ascorbic acid solution; extract Sn into 0.1 M TOA in a (2 + 1) mixture of heptane - amyl acetate Decompose by fusion with KCN, extract Sn by N-benzoylphenylhydroxylamine into toluene, use organic phase See Ba, ref. 9134 s1134 See Nb, ref. Sl905 s1905 8611830 See Nb, ref. 861438 861438 8611329 Grind sample to -325 mesh; mix 75 mg of powder with 75 mg of SO2 + A1203 + Na2C03 (8 + 1 + 1) and 50 mg of graphite powder with Pd as internal standard See Eu, ref. SIC1164 SIC1164 Mix (1 + 1) sample + graphite powder; use Pd S1232 as internal standard Fuse sample powder with K2BP07 (1 + 3), 861C1267 dissolve in 1 M HNO,, centrifuge; heat with HF and methanol, dissolve residue in 1 M HNO, See Mo, ref. SIC283 SIC283 See Nb, ref.9905 s1905 Acid decomposition; extraction with ethyl ether Pre-concentrate by adsorption from dilute acid medium with polyurethane foam in presence of C1-, Br- or I- S1153 8611032 See Ga, ref. 8611045 8611045 Digest with H20 - H2S04, fuse with 8611620 LiB02 at 950 "C for 15 min, dissolve in 10% HNO,; standard additions method HN03 - H20 - HC104 (40 + 40 + 3) ml Treat 2 g of sample with 86192 See Th, ref. 86lC1267 86lC1267 See Mo , ref. SIC283 See Mo, ref. 861C569 Determine total V then fractionate: obtain soluble organic by extraction with benzene - methanol, HC1-soluble, HF-soluble and kerogen fused with Na2C0,; add A1 as releasing agent Decompose rock powder with HN03 - HF, dissolve residue in HNO, - HC104 - HF; for concentrates use H3P04 - HF then HC1- HN03 Dissolve by fusion with Na202, stabilise solution with H3P04 See Th, ref.S1232 See La, ref. 8611831 See Cu. ref. SIC1171 See Th, ref. 9232 Decompose with NaOH - Na202 at 770 K, add HN03 - Dissolution based on fritting with Na202 Decompose with HF - HNO, under pressure at 170 "C for 16 h, dilute with H20 Decompose 5-10 mg sample with H2S04 - HF, heat to fumes, add H2S04 and 30% H202 solution, dilute to 100 ml containing NaCl (Al, Ca, Cr, Fe, Ni and Si) Excite in presence of powdered graphite SIC283 86lC569 861C635 s1101 Sl222 S1232 8611831 SIC1171 Sl232 86lC633 S113 S142 Sl66 S168 Si73JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, DECEMBER 1986, VOL. 1 185R Table 1. SUMMARY OF ANALYSES OF MINERALS AND REFRACTORIES-continued Technique; atomisation; Concentration analyte form >lo0 pg g-l AE; spark in controlled atmosphere; S Trace levels AE; arc; S Element Various Various Various Various (11) (14) Various Various (4) (6) Various Various (9) Various (10) (18) Various Various Various Various Various Various Various (6) (41) (4) (15) (30) Various Various (60) Various Various (10) Various Various Various Various Various Various (10) Matrix Oxides, fluorides, solid solutions Sample treatment Reference 978 Sl80 Sl83 Sl98 s199 s1135 Sl136 Sl188 s1200 Sl216 s1219 s1233 9244 SIC275 SIC277 SIC278 SIC279 SIC289 SIC294 SIC304 SIC3 11 SIC320 SIC324 SIC343 SIC415 SIC421 SIC444 Briquette with graphite (REEs) U compounds, zircaloy Silicon dioxide films Geological, environmental, industrial materials Periclase Use (1 + 1) KCl and LiF as carrier mixture Vapour phase decomposition by HF (REEs) Ultratrace levels AA; ETA; G - AA; F, air - C2H2 or N20 - C2H2; L Discussion of sample preparation methods, procedures, interferences; review with 68 references - AE; a.c. arc; S Powder samples (Al, Ca, Fe and Si) Ores, beneficiation products, slags >10 ng g-1 AE; a.c.arc; S Incomplete cupellation, treat Pb regulus with dilute HN03, evaporate to dryness; add powdered C, more Pb, NaCl, treat with HN03 and evaporate, dry at 190 "C for 15 min; blow into arc (Au, Ir, Pd, Pt, Rh and Ru) Incomplete cupellation, treat Pb regulus with HN03, HC1+ HN03, HCl and fuse with Na202 + KOH (noble metals) HC1- ascorbic acid - KI solution, extract with Aliquat 336 in IBMK (Ag, As, Bi, Cd, Cu, Mo, Pb, Sb and Zn) Interlaboratory study on the preparation of RM (As, Cd, Co, Cr, F, Hg, Mn, Ni, Pb and Zn) 30 min, or decompose with HF - HN03 under pressure at 170 "C for 16 h Fuse with K2S207, dissolve in Either fuse with Na2C03 at lo00 "C for Interlaboratory study (REEs) Ores, beneficiation products, slags >10 ng g-1 AA; ETA or F, air - C,H,; L Geological material Trace levels AA; F, air - C2H2 or N20 - C2H2; L Coal RM Trace levels AA, AE, AF and others Silicon carbide AE; ICP; L - Rock RMs - AE, NAA or paper chromatography Trace levels AE; a.c.arc; L Terbium oxide Coals Excite in controlled atmosphere O2 + Ar Crush samples to 4 0 pm, ash at 150 or at Na2C03 fusion method or dissolution with Dissolve under pressure with HF - HCI - HN03 Add 0.2 g of -325 mesh sample to 100 ml (Dy, Er, Gd, Ho, Sm and Y) 460 "C; interlaboratory study 5% HF(B,Ge,PandSi) in PTFE vessel at 150 "C for 2 h de-ionised H20 and 2 or 3 drops of wetting agent; agitate with magnetic stirrer during analysis Use of rapid data acquisition system for transient signals; eliminate the nebuliser Produce interelement correction factors by solution method to standardise XRF for multi-layer analysis Assessment for widely varying matrices New design for direct sample insertion device (Ag, As, Cd, Cu, Ge, In, Li, Pb, Sn and Zn) Minor and trace - AE; ICP; L AE or AA or XRF levels Silicate glasses, glass films Corrosion resistant glasses Coal Major and minor AE; ICP; L Trace levels AE; ICP; S levels Semiconductor materials Metal layers on semiconductor products Wide range Geological, biological materials Geological pigments, chromites Environmental, biological materials Coal Rocks - AE; ICP; G - XRF and AE; ICP; SorL ng g-* MS; ICP; L >o.1 pg 1-1 AE; ICP; Lor S Prepare slurry with (1 + 1) emulsifying lubricant and H20 - AE; DCP; S - AE; DCP; S Laser ablation from rotating sample Trace levels AE; DCP; S - AE; ICP; L Slurry nebulisation Design of PTFE nebuliser to eliminate drift when using LiB02 fusion Atlas of spectral interferences Geological material Major, minor and AE; ICP; L Trace levels AE; ICP; L trace levels Fuse with LiB02 - Li2B407, dissolve in HN03, treat with HF, extract FeI" with IBMK then chelate by poly(dithi0carbamate) resin; recover metals by PTFE bomb or H202 digestion (Ag, Ir, Os, Pd, Pt, Rh, Ru, Ta, Th and U) dissolve residue in HC1 Digest with HF - HC104 (1 + l), evaporate, Geological material Various - Geological material Major, minor and AE; ICP; L trace levels186R JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, DECEMBER 1986, VOL.1 ~ Table 1. SUMMARY OF ANALYSES OF MINERALS AND REFRACTORIES-continued Technique ; atomisation; analyte form AE; ICP; L Element Various ( 5 ) (9) Various Various Various Various Various (12) Various Various Various Various Various Various Various (16) (4) ( 5 ) (6) Various (14) ( 5 ) Various Various Various Various (12) (12) Various Various Various (15) Various Various Various Various Various (60) Various Various Various Matrix Zirconium dioxide Concentration - Sample treatment Reference SIC446 SIC447 S/C450 SIC456 SIC461 SIC462 SIC464 SIC465 s1507 St604 S1609 S1624 S1657 S1666 S1669 SIC687 SIC696 SIC697 SIC707 SIC712 SIC7 13 SIC720 SIC725 SIC732 SIC733 SIC734 SIC735 S1829 S1838 Dissolve under pressure with HF - HC1 - HN03 at llO"C, dilute with H20 (Al, Fe, Mn, Si and Ti) in 10% HCI (Al, Ca, Cr, Fe, Mg, Mn, Si, Ti and Zn) Study of separation procedures and spectral interferences (REEs) Digest with HNO, - HF Fuse with Na2C03 - Na2B4O7.dissolve Chromite Major and trace levels AE; ICP; L Phosphate AE; ICP; L Major, minor and Trace levels Trace levels trace levels AE; ICP; L Silicon metal, Rocks Geochemical material, fly ash, zircalo y Wide range alloys MS; ICP; L MS or AE; ICP; L Two-stage acid attack Direct comparison between ICP-MS and ICP-AES for complex matrices >O.1 ng ml-1 MS; ICP; L Assessment of performance, measurement schemes; currently need to dilute samples to 0.1% dissolved solids Geological Silicate rocks material, metals >0.1 ngml-1 MS; ICP; L Trace levels AA; ETA; L Separate lanthanides by ion-exchange; Ta-foil Device for continuous introduction of powder Decompose with condensed H3P04 lined furnace (rare earths) (Ce, La, Y and Yb) AE; ICP; S Rare earth ores Geological material Sediments Major levels AA or AE; F or ICP; L AA; -; L Extract with 0.1 M HCl (Cd, Cr, Fe, Pb and Zn) Fuse with LiB02, dissolve in 3% HNO, with Be and Co as internal standards; rotating graphite cup electrode (Al, Ca, Mg, Mn, Si and Ti) 0.2 g of sample + 1 g of flux; for alkali elements digest sample with HF - H2S04 HF - aqua regia, adsorb on SARAFION NMRR ion-exchange resin, elute with thiourea (Au, Ir, Pd, Pt and Rh) Fuse with Na2C03 + Na2B407, using Digest under pressure at 170 "C with ccgg-' 0.1-36.0% Minerals, rocks, ores AE; a.c.spark; L Calcined bauxite Major, minor and trace levels AE; ICP; L AA; ETA; L Rocks, ores Trace levels Geological, me talhrgical material Coal ash, silicates Major and trace levels AE; ICP; L Trace levels AE; ICP; L AA; For ETA; L See B , ref. SIC696 Coal, coke, fly ash Trace levels Ash at 815 "C, dissolve with HF - aqua regia - H3B03 in sealed polypropylene bottle on water bath Atlas of spectral interferences Geological material Carbonate, phosphate rocks Phosphate rocks, geological material Mineralised rocks Trace levels AE; ICP; L AE; DCP; L AE; ICP; L Minor and trace levels <1 CLgg-l Dissolve with 1 N HCI or HN03, or fuse with Na2C03 - Na2B407 mixture Cation-exchange separation (REEs) pg g-1-% Acid attack or fusion with LiB02, Na202 Suspension in an emulsifying lubricant Fusion, acid dissolution and pressure digestion Fusion with LiB02; cation-exchange for Th and REEs Fuse with Na2C03, or mixture of LiB02 + Li2B407, then acid dissolution trace impurities K202, acid dissolution after combustion in 02, or autoclave fluorination with XeF, or Na2C03 Study of mineral fluorescence in relation to Fuse with Li2B407, or fuse with Review of methods AE; ICP; L AE; ICP; S AE; DCP; L AE; DCP or ICP; L AE; DCP; L AE; F, AE; DCP; L air - C2H2; L Refractory oxides Geological material Rocks Trace levels Major, minor Major, minor Major, minor and trace levels and trace levels and trace levels Beryl ore Ores Trace levels Coal Geological and inorganic materials AA or AE; ICP; LJOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, DECEMBER 1986, VOL.1 187R Table 1. SUMMARY OF ANALYSES OF MINERALS AND REFRACTORIES-continued Technique; atomisat ion; Concentration analyte form - AA or AE; ICP; L Element Various Various (8) Various Various Various Various (17) (14) Various (6) Various Various Various Various Various (19) (6) (4) Various Various Various Various Various (38) Various Various Various Various ( 5 ) Various Various Various Various (4) Various (4) Matrix Ores, ceramics, garnets, glass Sample treatment CC14 + CuC1, at 600-800 "C or HC1+ KMn04 at 160 "C (Pt-group metals, Combined technique: sample sizes up to 0.2 g injected into graphite furnace, atomised via a slotted T-tube in flame (As, Cd, Co, Cu, Hg, Pb, Sb and Se) Digest with HN03 - HF - HC104, fuse residue with NaOH Mix sample and C powder (1 + 1) (REEs) Decompose by chlorination under pressure: Au) Reference S1847 S1850 S1870 S1888 s/901 S11106 S/C1147 S/C1148 s/c1150 SIC1151 SIC1 156 SIC1158 S/C1161 S/C1162 SIC1163 SIC1 165 SIC1 172 SIC1 175 SIC1176 SIC1177 SIC1178 S/C1180 S/C1182 SIC1 186 SIC1187 SIC1192 Biological, geological materials Trace levels AA; furnace - quartz T-tube, F, air - C2H,; S Major, minor and AE; ICP; L w2g g-' Trace levels AE; ICP; L trace levels AE; d.c.arc; S Coal fly ash Erbium oxide Geological material Uranium oxide Cation exchange: use HN03 as eluent Load sample into graphite cup; insert (REEs) horizontally, carrier distillation in tail region of ICP Fuse with LiBO;, - Li2B407, dissolve in acid, treat with HF, extract Fe" into IBMK; pass through resin and recover (Ag, Pd, Pt, Ta, Th and U) Review; future needs and prospects g-' AE; ICP; S Geological material Ultratrace levels AE; ICP; L Geochemical material Wide range Minerals, metal extracts Trace and AA; For ETA; ultratrace levels Lor S >20-100 ng 1-1 Trace levels MS; ICP; Lor S Wet chemistry Performance characteristics, capabilities Liquid - liquid extraction; ion-exchange chromatography; fire-assay separation and concentration Coal Environmental, geological materials Geological material Trace levels Trace levels AA or AE or XRF AA or AE; ICP; LorG Separatiodpre-concen tration methodology AA; ETA; L Zeeman background correction (Au, Ir, Pd, Pt, Rh and Ru) Pg Barite 40-400 pg g-1 AE; ICP; L Dissolve using cation-exchange resin at 80 "C for 24 h, then separate REEs by gradient HN03 technique (Ce, Eu, Gd and La) Comparison of automated, sequential AAS with ICP-AES Solvent extraction techniques using micro-volumes Interface operation and performance Geological material Single mineral grains Geological material, non-ferrous metals Rocks AA or AE; ICP; L AA; ETA; L MS; ICP; L Ultratrace levels >O.1 ng ml-1 Major, minor and trace levels AE AE AE ICP; L ICP; s ICP; L Digest in HF - HC104, evaporate to dryness, dissolve residue in HCI; add Sc as internal standard suspend 0.5 g in 25 g of suspension medium of glycerol - H20 (40 + 60 m/m) Grind until 90% of material is <44 pm; Spectral line atlas P y r 0- met allur gic a1 products Geological material Geological material Major and minor levels Minor and trace levels 0.1-1 .o pg g-1 AE; ICP; L Background correction by total difference computation for generalised standard additions method (Ce, Eu, Gd, La and Sm) (1 + 5 + 19) (REEs) Slurry in glycerol - propanol - H20 No separation or pre-concentration Fire assay procedure (platinum group metals, Combined fire assay/wet chemical procedure: Pb collection, HC104 parting, formic acid reduction - precipitation (Ag, Au, Pd and Au) Pt) Fuse with Na202 - Na2C03, dissolve with H2S04 - ascorbic acid - KI; extract into diantipyrylmethane - chloroform then obtain second organic phase using C6H6 (Ag, Au, Pd and Pt) Coal, coal ash, fly ash Rocks, minerals, concentrates Geological material Ores, concentrates AE; ICP; S MS; ICP; L MS; ICP; L AA; -; L Geochemical material, mill-tailings Trace levels AA; ETA; L188R JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, DECEMBER 1986, VOL. 1 Table 1.SUMMARY OF ANALYSES OF MINERALS AND REFRACTORIES-continued Technique ; atomisation; analyte form - Element Various (72) Various Various Various (9) (6) (10) Various Various Various Various Various Various Various Various Various Various (27) (11) Various Various Various (4) Various (12) Various Various Various Various Various Various (11) (21) (7) (15) Various Various Various Various Various Various (9) (14) (19) Various (36) Various (15) Various ( 5 ) Matrix Coal RMs Concentration - Sample treatment Preparation and analysis of 3 new RMs; statistical evaluation of results from 28 laboratories ICP (Y and REEs) Mg, Mn, Na, Si and Ti) study of matrix interferences with HN03 or HBr (Ag, Au, Bi, Cd, Sn andT1) Study of interference effects (Ba, Ca, Co, Cu, Fe, Mg, Mn, Ni, Sr and Zn) Chemical analysis of 3 standard rocks HPLC ion exchange on-line to nebuliser of Fuse with LiB02, dissolve (Al, Ca, Fe, K, Etching to separate thin layers (ca.1 pm), Reference SIC1194 Sl1227 86/33 86/35 86/75 86176 861115 86lC13 1 861C134 861C154 86/C162 86lC178 861196 861202 AE; ICP; L AA;-;L Geological material Silicate rocks Trace levels Major levels Trace levels Indium arsenide AA; ETA; L Major and trace Major, minor and ng ml-1 levels trace levels AA; F, air - C2H2; L - Clays, Mn ores, rocks Rock RMs MS; ICP; L Silicate rock RMs, water RMs Geological material Geological material Geological material Sulphide minerals Trace levels AE; d.c.arc; S Mix with buffer: graphite, Li2C03, NaC1, PTFE Trace levels AE; d.c. arc; S Study of factors affecting accuracy Trace levels MS; ICP; L AA or AE; ICP; L Initial studies Digest with acid mixture under pressure using Mixed acid and fusion, or graphite cup Powder <300 mesh mixed with binder to form Grind to pass 240 BS mesh, ignite at 815 "C, a microwave oven procedures pellet; laser ablation digest with HF in sealed container at 105-110 "C for 30 min, add H3BO3; use Ni as internal standard Discussion of capabilities Geological material Geological material Coal ash Major and trace levels >10 ng g-1 AE; ICP; Lor S MS; ICP; S Major and minor levels AE; ICP; L 861206 861233 861246 Geochemical material Silicate-based materials Basic and ultrabasic rocks AE; ICP; L AA; -; - Archaeological applications >0.001 mg kg-1 AE; F; L Decompose with LiOH - HN03 at 180 "C; pre-concentrate Cs and Rb by extraction with sodium tetraphenylborate in DIBK (Cs, K, Na and Rb) For GDL grind to 4 0 pm, heat at 600 "C, mix with Cu powder (1 + 4) and press; for ICP digest with H2S04 - HN03 - HF Slurry injection method Electron microprobe study 861265 AE; GDL or ICP; SorL Mediaeval glasses Trace levels Aluminous earth Archaeological glass Archaeological ceramics Forensic materials Coal, fly ash Trace levels - AA; ETA; S AE; GDL; S 861C289 861C293 AE; d.c.arc; S Effects of additives: C, Li2C03, Li2B204, Li2B407 and LiF - Digest with HN03 - HF - HC104, add HCl 86/C294 AE; ICP; - AE; ICP; L 861305 861312 Coal ash AA;-;L Suspend in dilute HC1, treat with ultrasound for 30 min, filter and determine dissolved elements (Al, Ca, Fe, K, Mg, Na and Sr) Decompose with HF - HN03 at 110 "C for 1 h, heat with H3B03 Comparison of techniques 861313 Coal ash AE; ICP; L 8613 14 861337 861378 861379 861408 861424 - 10-'2-10-'0 g Trace levels Pg l3-l 1.4-3.6% as oxides Trace levels Dopant materials for semiconductor High-purity alumina Lutecium oxide AA or AE or MS; ETA or ICP; L AE; d.c. arc; S Arc between graphite electrodes Powder mixed with buffer (rare earths) (B, Ca, Cr, Fe, Mg, Mn, Pb, Si and Ti) AE; d.c.arc; S AE; ICP; L Light rare earth Lignite oxide mixtures Comparison with results by X-ray photoelectron spectrometry (rare earths) Dioxane extract fractionated to acid, base, neutral, C6H6-insoluble and petroleum spirit-insoluble fractions Discussion of element distributions AA or AE; ICP; L Sediments, manganese concretions Silicate rocks AA, NAA, XRF, colorimetric 861425 Major, minor and AE; ICP; L >1 ng g-1 AA; ETA; S trace levels Decompose with HNO, - HF - HC104 861435 861C455 Geochemical, environmental materials Improved atomiser design, 10-50 mg powdered sample (Ag, Bi, Cd, Pb and T1)JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, DECEMBER 1986, VOL. 1 189R Table 1. SUMMARY OF ANALYSES OF MINERALS AND REFRACTORIES-continued Technique; atomisat ion; analyte form Element Various Various Various Various (4) (17) (8) (17) Various Various ( 5 ) (8) Various Various (17) Various Various (10) Various Various Various (15) Various Various (44) (4) Various Various (33) Various Various Various (12) Various (4) Various Various Various Various ( 5 ) Matrix Environmental material Geological material Calcium phosphate Concentration Trace levels Sample treatment Reference 861C457 861C460 861C497 861C500 861C501 861C503 861C504 861C506 861C547 861C550 861C556 861C565 861C579 861C630 861C636 861C637 861C639 861C647 861678 861679 861682 861738 861C755 861C756, 861C864 861C759 AA; ETA; L AE; ICP; L Matrix interferences studied (Au, Eu, Pt and Use Sc as internal standard for major elements yb) Major, minor and trace levels 0.1-100 pg g-1 AE; d.c.arc; S AE; ICP; L Mix sample (1 + 1) with graphite - NaCl carrier (As, Ba, Cu, Fe, Mg, Ni, Pb and Zn) Either fuse with KHS04 and dissolve in (1 + 9) HN03 or decompose under pressure with HF - H2SO4 at 140-170 "C for 3-14 h, evaporate, dissolve in (1 + 9) HN03 Dissolve under pressure with HF - HCl- HN03 at 110 "C (Al, Ca, Fe, Si and Ti) Dissolve 2.5 g U or equivalent amount of compound in 5 N HN03, extract with 40% tributyl phosphate in CC14; evaporate to dryness and dissolve residue in 2 N HN03 (Dy, Er, Eu, Gd, Ho, La, Lu and Tm) Purification of silicon bar by partial fusion; transfer emission at plasma - slag interface by fibre optics to spectrometer for process AE; ICP; L AE; ICP; L AE; P, Ar - H2- 02, refining process; S Zirconia ceramics Trace levels Zirconium dioxide Minor and trace levels >0.02 vg g-1 Uranium, uranium compounds Silicon control oxalates with Y or Th carrier, from Mn as fluorides by HF - NH4F, fume with H2S04, neutralise, arc residue (REEs and Cd) Separate from Li by coprecipitation as Digest with mineral acids Li2S04, MnSO, , RMs for neutron cross sections Trace levels AE; d.c.arcin Ar - 0,; S Geological material Actinide compounds MS; ICP; L MS or AE; ICP; L Ultratrace levels Trace levels Single crystals less than 10 mg in solution or after separation and enrichment (Al, Ce, Co, Cr, Cu, Fe, Mn, Mo, Ni and Zn) - Mix powdered sample - graphite - CdF2 (2 + 2 + l), add Pd as internal standard Classification and systematic study of buffers for various applications (Mo, Si, Zr and Pt group) Preparation and analyses of new whole-rock phosphorite standard RM Treat rock powder with HN03 - HClO, - HF, dissolve residue in HC1; fuse ores with Na202, dissolve in HCl; coprecipitate with ferric hydroxide at pH 2.4 + NH,Cl, generate Hy (As, Sb, Se and Te) Digest with boiling aqua regia, extract using ascorbic acid - KI - hydroxylamine hydrochloride with tricaprylylmethyl- ammonium chloride in IBMK Ignite ca.3 g at 450 "C for 3 h, mix 100 mg (1 + 1) with NaF - graphite buffer, form into 30 mg compressed pellet Insert 50 mg of sample powder into graphite cup, drive horizontally into the plasma Either remove Fe by extraction with IBMK from HC1 medium, or reduce Fe*" to Fe" with ascorbic acid to minimise its extraction by IBMK; use aqueous or organic phase For XRFpre-concentrate by ion exchange and coprecipitate with Fe(OH)3 for thin-film preparation; comparison with ICP-AES (REEs) Decompose with HF - aqua regia and HBr - Br solution; 2-step solvent extraction with IBMK, from 0.1 M HBr medium (Au and T1) and from 3 M HBr + ascorbic acid (In and Te) Acid digestion (REEs) Correction for background and spectral interferences by chemometric technique to invert the matrix data insert above the top of the torch Place powdered sample in graphite cup and Study of matrix effects (Cd, Fe, Ni, V and Zn) Ca-rich rocks Granitic rocks Trace levels Trace levels - MS; ICP; L AE; a.c.arc; S AA; F, N20 - C2H2; L Various AE; Hy, ICP; L Catalysts Phosphate RM Major, minor and trace levels Ygg-' Silicate rocks, sulphide ores Geochemical material Trace levels AA; F, air or N2O - C2H2; L Stream sediments Major and trace levels AE; d.c.arc; S Silicate rocks Trace levels AE; ICP; S Geochemical material AA; F, air - GH2; L Rock RMs XRF or AE; ICP; SorL Rock, soil, stream sediment AA; F, air - C2H2; L Rock RMs Geological material Trace levels Trace levels AE; ICP; L AE; ICP; L Silicate rocks Trace levels Trace levels AE; ICP; S AE; DCP; L Geological material190R JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, DECEMBER 1986, VOL. 1 Table 1. SUMMARY OF ANALYSES OF MINERALS AND REFRACTORIEkontinued Element Various Various Various Various Various Various (23) Various Various Various Various Various Various (22) (15) (9) Various Various Various Various Various (16) (45) Various (10) Various Various Various Various Various (13) (8) Various Various (25) (60) Various Technique; atomisation; Concentration analyte form Trace levels AE; ICP; L Major and trace MS; ICP; L - AE; ICP; S levels Matrix Phosphorites Geological RMs Sample treatment Use acid-based solutions Correction for interferences Reference 861C760 861C790 86lC808 861C881 861C903 861C929 861C937 861C952 861973 8611013 861101 6 86/ 10 17 8611034 861 106 1 8611073 8611079 86/C1109 86/C1136 861C1137 86/C 1 139 86/C1180 861C1182 86/C1196 861C1200 861C1234 861C1246 Geochemical material Coal Laser ablation - AE; DCP; S Grind in 3 stages to pm-size particles, weigh into beaker, add 50 ml Of 0.5% surfactant solution, stir for 5 min Digest in HN03 - HF - HC104 Coal Trace levels - AE; ICP; S AA or AE; ICP; L Geological material Effects of particle size distribution, differential transport and thermochemical reactions with slurry injection or direct solid insertion - Geological, biological material Geological material Geological material RQck RMs - AA; furnace - F; S Major and trace levels SorL - AE; ICP; L XRF or AE; ICP; Comparison of techniques, 200 samples Study of causes and correction procedures for matrix effects by Ca Alkali fusion, digestion with HF - HC1- H202; interlaboratory study Decompose with HN03 - HCl- H20 - HF in sealed PTFE bomb Separate by cation exchange, collect on cation-exchanging paper from HCl medium at pH 1-2, ash and ignite (REEs) 150 "C for 5 h, add H3B03 solution; or with H2S04 at 230 "C for 16 h (Al, Ca, Fe, Hf, Mg, Mn, Na, Si andTi) Decompose under pressure with HF - HC1 at Major and minor AA; -; L Major, minor and AE; ICP; L levels trace levels Trace levels AE; -; S Geological material Rocks Zirconium oxide - AE; ICP; L Mediaeval glass Major and trace Trace levels AE; ICP; L AA or AE; -; L levels Phosphate minerals Dissolve in H2S04, filter and add H20 Data on 3 geochemical reference samples (REEs) Silicate rock RMs Major and trace Various Trace levels MS; ICP; L levels Limestone, manganese nodules Wide range Study of potential molecular interferences >0.1 pg 1-1 AE; ICP; S or L Design and application of a direct sample insertion system (Ag, As, Cd, Cu, Ge, In, Li, Pb, Sn and Zn) Slurry injection or direct solid insertion in graphite cup Support on conductive substrate, generate aerosol by high-voltage spark discharge Use HN03 in final stage to avoid molecular ion interferences Chemometric technique for deconvoluting background and spectral interference contributions to the analyte line aggregation of particles Slurry atomisation using dispersant to prevent - AE; ICP; S Geological material Ferromanganese nodules Geological material Geological material - AE; ICP; S Trace levels MS; ICP; L Trace levels AE; ICP; L Major, minor and AE; ICP or trace levels DCP; S Geological, environmental materials Corrosion resistant glass Major, minor and AE; ICP; L trace levels Dissolve using microwave oven, or in PTFE decomposition vessel; add fluoride complexer (Al, B, Ca, Co, La, Mg, Si and Sr) Homogenise coal, digest with acid; 3-year study of possible sources of acid precipitation Generalised scheme for decomposition and dissolution; acid attack with HF - HC104, flux fusion with Na2C03 .- Na2B407 (1 + 1); oxidisinglcomplexing agents added as required mathematical treatment for maximum accuracy micro-sampling technique by nebuliser starvation Time-saving methods for survey work; Digest with HF - HC104 - HNO,; Coal, acid rain Trace levels AA; ETA; L AE; ICP; L Major, minor and AE; ICP; L trace levels Glass, ceramics, refractories, ores Various - Geological material 86lC1247 86lC1258 Major, minor and AE; ICP; L trace levels Various - Geological material Trace levels AE; ICP; LJOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, DECEMBER 1986, VOL.1 Table 1. SUMMARY OF ANALYSES OF MINERALS AND REFRACTORIES-continued 191R Technique ; atomisation; analyte form AE; ICP; L MS; ICP; L MS; ICP; L AE; ICP; L Various AE; ICP; L AE; d.c.arc; S AE; ICP; S AE; ICP; L AA; F, N2O - C2H2; L AA or AE; ICP; L AE; ICP; L AA or AE; -; S Element Various Various Various Various Various Various Various Various Various (12) (12) (11) ( 5 ) (48) (12) (23) (8) Various Various Various (6) Various Various Various Various (29) Various Various (4) ( 5 ) Various Various Various Various Various (9) (20) Various (23) Various (4) Various (9) Various (6) Matrix Concentration Trace levels Sample treatment Reference 86lC1259 86lC1260 86lC 1264 861C1266 8611276 8611288 8611295 8611297 8611298 8611308 8611323 861 1326 8611328 8611371 86/14 16 86/1432 8611442 8611443 8611466 861C1475 86lC1536 861C1555 86lC1569 86lC1583 8611630 8611636 8611 670 Digest with HF - HC104 Obsidian artifacts Silver, geological material Mineral fluid inclusion Ferromanganese deposits Sulphide ore CRMs Geological material Pyrite, pyrrhotite >0.3 pg g-1 Dissolve 3-15 mg sample in HN03, dilute Use FI and/or electrothermal volatilisation Separate by ion-exchange chromatography See Au, ref. 86/1276 (Ag, Au, Cu, Fe and S) to 50 ml for fluid inclusion leachates (REEs) Trace levels Trace levels Major and trace Minor and trace levels levels >4% g-l Fuse rock sample with Li2B407, dissolve in glycerine - HC1 Excite at 11 A in arc Geochemical material Cement, geological material Minor and trace Major and minor levels levels Direct introduction of 25-40 mg sample with grain-size 200-300 mesh Dissolve under pressure with H20 - HF - aqua regia at 160 "C for 45 min, cool and treat with H3B03 solution (Al, Ca, Fe, K, Mg, Na, Si and Ti) Decompose under pressure with acid mixtures Ores, slags, oxidic Granites material Trace levels Digest with acid mixture (Be, Li, Mo, Nb, Sn and W) Pre-concentrate on S-containing polymer, decompose at 650 "C, mix residue with CuO (Au, Pd, Pt, Rh and Ru) Mix sample (1 + 2) with graphite powder containing 3% NaCl Separate by adsorption on polyamide plastic soaked with PMBP at pH 2-6; dry, ash, mix with spectrographic buffer (REEs) Use 3 different solutions for major, trace and rare earth elements Grind in swing-mill, pass through 325-mesh sieve, prepare slurry; study of mass transport losses in the spray chamber using laser measurement technique suspension with xylene HCl, filter and use filtrate (Cu, Fe, Ni and Pb) Li2B407 (Cd, Cr, Cu, Ni and Zn) Rapid, direct analysis by injecting as Fuse with Na2C03, dissolve in concentrated Digest with HN03 - HClO,, or fuse with Catalysts, grogs, ceramics, wastes Trace levels Rocks, minerals Trace levels AE; d.c.arc; S AE; ICP; S Rocks Igneous rocks Major and trace levels AE; DCP; L Coal AA; F, N2O - C2H2; S Zeolite AE; ICP; S AA;-;L Silica Trace levels City waste incinerator ash CRM Ore concentrate CRM Geological material Bauxite, Bayer mud Geological material Trace levels AE; ICP; L MS; ICP; L AE; ICP; L AE; ICP; L AE; ICP; S Study of accuracy of isotope ratio Dissolve with HF - HC104 - HC1 (Cd, Co, Cr, Fuse with Li2B407 on a Claisse Fluxer VI, Study of slurry injection problems: matrix measurements Cu, Mn, Ni, Pb, V and Zn) dissolve in dilute HN03 match textural, mineralogical and chemical compositions Material less than 200 mesh used to fill glass columns; leach by buffers at pH 3, pH 5 and pH 8 and collect effluent at 10-h intervals over 3-month period (V relative to other elements) Digest with HN03 - HClO, - HF, evaporate and dissolve in HCl(1 + 1); or fuse ores with Na202; precipitate analytes with Fe(OH)3 at pH 2.4 in presence of NH4C1 solution (As, Sb, Se and Te) Fuse with LiB02 in PtlAu crucible, dissolve in dilute (1 N) HN03, add Sc as internal standard (Al, Ca, Fe, Mg, Mn, Si, Ti, U and zr> Digest with HF - HCl - HC104, heat to dryness, then with HCl - HClO,; add HN03 - HCl to hot residue (Er, Ho, Lu, Pr, Tb and Tm) 1-2000 pg g-1 Major and minor levels - AA; ETA; Land proton-induced X-ray emission Weathered fly ash Trace levels Silicate rocks, sulphide ores AE; Hy, ICP; G Yo levels AE; ICP; L Silicate rocks containing U and Zr Trace levels MS; ICP; L Rocks192R JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, DECEMBER 1986, VOL. 1 Table 1. SUMMARY OF ANALYSES OF MINERALS AND REFRACTORIES-continued Technique ; atomisation; Matrix Concentration analyte form Sample treatment Reference Element Unm Various - Coke Trace levels AE; d.c. arc; S Various - Various - Cu ore, Ni ore 0.13-38 pg g-1 AA; F, Solids - AA; -; S (4) ( 5 ) concentrates air - CzHz; L Various - Glass, feldspathic - AA; F; L sand, CRMs ( 5 ) Electroslag - AA or AE; F; L Various - (8) remelting slags Various - Sediment CRM Trace levels AE; ICP; L (13) Mix sample with 2-5% NaF as buffer 8611723 Review with 458 references 8611725 Coprecipitate with Cu sulphide, dissolve 8611747 precipitate in (3 + 1) HC1- HN03; add CdS04 solution, dilute with 2 M HCl (Au, Pd, Pt, Rh and Ru) Study of interference suppressants: Al, Fe, La, Sr, NH4C1 or 8-hydroxyquinoline (Ba, Ca, Cr, Mg andTi) (Cu , Ni , Ti and V) 8611767 8611789 Grind to pass 200 mesh, dry, fuse with Na2C03 - K2S207 (3 + 1) for 15 min at 750 "C then 15 min at 1000 "C; cool and add HCl(1 + 1), warm to dissolve cake (Al, Ca, Cr, Fe, Mg, Mn, Ni and Si) Dissolve by conventional methods, separate using cation exchange (REEs) 8611804 LOCATION OF REFERENCES The references cited in this Update have been published as follows: Sll-Sl1234, J. Anal. At. Spectrom., 1986, Supplement, 1S-49S. 8611-861265, J. Anal. At. Spectrom., 1986, 1( 1) 19R-28R. 86/C26&86/709, J. Anal. At. Spectrom., 1986, 1(2), 45R-59R. 86171~8611030, J. Anal. At. Spectrom., 1986, 1(3), 75R-85R. 86/1031-8611460, J. Anal. At. Spectrom. 1986, 1(4), 107R-120R. 8611461-8611834, J . Anal. At. Spectrom., 1986, 1(5), 155R-168R. Glossary of Abbreviations Whenever suitable, elements may be referred to by their chemical symbols and compounds by their formulae. The following abbreviations are used extensively in the Atomic Spectrometry Updates. a x . AA AAS AE AES AF AFS APDC ASV CMP CRM cw d.c. DCP DMF DNA EDL EDTA ETA FAAS FAES FAFS FI GC GDL HCL h.f. HPLC IBMK alternating current atomic absorption atomic absorption spectrometry atomic emission atomic emission spectrometry atomic fluorescence atomic fluorescence spectrometry ammonium pyrrolidinedithiocarbamate (ammonium tetramethylenedithio- carbamate) anodic-stripping voltammetry capacitively coupled microwave plasma certified reference material continuous wave direct current d.c. plasma N, N-dime t h ylformamide deoxyribonucleic acid electrodeless discharge lamp ethylenediaminetetraacetic acid electrothermal atomisation flame AAS flame AES flame AFS flow injection gas chromatography glow discharge lamp hollow-cathode lamp high-frequency high-performance liquid chromatography isobutyl methyl ketone (4-methylpentan- 2-one) ICP IR LC LTE MECA MIP MS NAA NaDDC NTA OES PMT p.p.b. p.p.m. PTFE r.f. REE RM RSD SBR SEM SNR SSMS TCA TLC TOP0 u.h.f. uv VDU vuv XRF inductively coupled plasma infrared liquid chromatography local thermal equilibrium molecular emission cavity analysis microw ave-induced plasma mass spectrometry neutron-activation analysis sodium diethyldithiocarbamate nitrilotriacetic acid optical emission spectrometry photomultiplier tube parts per billion parts per million polytetrafluoroethylene radiofrequency rare earth element reference material relative standard deviation signal to background ratio scanning electron microscopy signal to noise ratio spark-source mass spectrometry trichloroacetic acid thin-layer chromatography trioctylphosphine oxide ultra-high-frequency ultraviolet visual display unit vacuum ultraviolet X-ray fluorescence

ISSN:0267-9477    

DOI:10.1039/JA986010169R

出版商:RSC    

年代:1986

数据来源: RSC

摘要:

JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, DECEMBER 1986, VOL. 1 193R ATOMIC SPECTROMETRY UPDATE REFERENCES The address given in a reference is that of the first named author and is not necessarily the same for any co-author. 8611835. 8611836. 8611837. 8611838. 8611839. 8611 840. 8611841. 8611842. 8611843. 8611 844. 8611845. 8611846. 8611847 I Wittman, P. K., Mitchell, J. W., Ultrapurification of nitrogen monitored by metastable transfer emission spec- troscopy, Appl. Spectrosc., 1986, 40, 156. (AT & T Bell Lab., Room lD-239,600 Mountain Ave., Murray Hill, NJ 07974, USA). Parisi, A. F., Hieftje, G. M., Fundamental studies in the ICP using a sinusoidally modulated power input, Appl. Spectrosc., 1986, 40, 181. (Dept. Chem., Indiana Univ., Bloomington, IN 47405, USA). Coxon, J.A., Roychowdhury, U. K., A spectrometric technique for monitoring [02(a1Ag)] in the gas phase, Appl. Spectrosc., 1986,40,203. (Dept. Chem., Dalhousie Univ., Halifax, Nova Scotia B3H 453, Canada). Wichman, M. D., Fietkau, R., Fry, R. C., Simplified slurry method for direct flame emission determinations of dietary salt in processed meat, Appl. Spectrosc., 1986, 40, 233. (Dept. Chem., Kansas State Univ., Manhattan, KS 66506, USA). Pyen, G. S., Long, S. E., Browner, R. F., Determination of arsenic, selenium and antimony, using hydride genera- tion introduction to an inductively coupled plasma, Appl. Spectrosc., 1986,40,246. (US Geological Survey, 6481-H Peachtree Industrial Blvd., Doraville, GA 30348, USA). Burton, L. L., Blades, M. W., A comparison of excitation conditions between conventional and low-flow, low-power inductively coupled plasma torches, Appl.Spectrosc. , 1986, 40, 265. (Dept. Chem., Univ. British Columbia, Vancouver, BC V6T 1Y6, Canada). Mitchell, P. G., Sneddon, J., Radziemski, L. J., A sample chamber for solid analysis by laser ablation - DCP spec- trometry, Appl. Spectrosc., 1986, 40, 274. (Dept. Chem., New Mexico State Univ., Las Cruces, NM 88003-0004, USA). Broekaert, J. 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M., Masking, chelation and solvent extraction for the determination of sub-parts-per-million levels of trace elements in high iron and salt matrices, Anal. Chem., 1986, 58, 1541.(Los Alamos Natl. Lab., Los Alamos, NM 87545, USA). Boguszewska, Z., Krasiejko, M., Palmowska-Kus, B., Application of platinum gauze activated by hydrogen to the adsorption separation of silver traces and their determination by AAS or spectrophotometry, Talanta, 1986,33, 155. (Dept. Anal. Chem., Tech. Univ. Warsaw, 00-664 Warsaw, Poland). Rettberg, T. M., Holcombe, J. A., Direct analysis of solids by graphite furnace atomic absorption spectrometry using a second surface atomiser, Anal. Chem., 1986, 58, 1462. (Dept. Chem., Univ. Texas, Austin, TX 78712, USA). Donaldson, E. M., Wang, M., Determination of silver, antimony, bismuth, copper, cadmium and indium in ores, concentrates and related materials by atomic absorption spectrophotometry after methyl isobutyl ketone extraction as iodides, Talanta, 1986, 33, 233.(Mineral Sci. Lab., Canada Centre for Mineral and Energy Technol., Dept. Energy, Mines and Resources, Ottawa, Canada). Pettersson, J., Hansson, L., Olin, A, Comparison of four digestion methods for the determination of selenium in bovine liver by hydride generation and atomic absorption spectrometry in a flow system, Talanta, 1986, 33, 249. (Univ. Uppsala, Dept. Anal. Chem., PO Box 531, S-751 21 Uppsala, Sweden). Lajunen, L. H. J., Kubin, A., Determination of trace amounts of molybdenum in plant tissue by solvent extraction - atomic absorption and direct current plasma emission spectrometry, Talanta, 1986, 33, 265. (Dept. Chem., Univ. Oulu, SF-90570 Oulu, Finland). Roy, N. K., Das, A. K., Determination of tungsten in rocks and minerals by chelate extraction and atomic absorption spectrometry, Talanta, 1986, 33, 277. (Geol. Survey of India, 27 J. L. Nehru Rd., Calcutta 700016, India).200R 8612032. 86/2033 I JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, DECEMBER 1986, VOL. 1 Cardarelli, E., Cifani, M., Mecozzi, M., Sechi, G., Analytical application of emulsions. Determination of lead in gasoline by atomic absorption spectrophotometry, Tuluntu, 1986, 33, 279. (Dept. Chem., Univ. “La Sap- ienza” of Rome, Rome, Italy). Fujita, K., Takada, T., Effect of temperature on genera- tion and decomposition of the Group Vb element hydrides and estimation of the kinetic stability of gaseous bismuth hydride by atomic absorption spectrometry, Tuluntu, 1986, 33, 203. (Dept. Chem., Coll. Sci., Rikkyo (St Paul’s) Univ., Nishi-Ikebukuro, Toshima-ku, Tokyo 171, Japan). Papers 861C203486/C2038 were presented at the Atomic Spectrometry Updates Symposium, Sheffield, UK, 15th April, 1986. 861C2034. Mermet, J. M., Trends in inductively coupled plasma spectrochemistry, (Laboratoire des Sciences Analytiques, Bit. 308, UniversitC Claude Bernard-Lyon I, 69622 Villeurbanne Cedex, France). 86/C2035. Welz, B., Abuse of the analyte addition technique in atomic absorption spectrometry, (Dept Appl. Res., Bodenseewerk Perkin-Elmer und Co. GmbH, D-770 Uberlingen, FRG). 86lC2036. Thompson, M., High precision analysis by ICP-OES (Appl. Geochem. Res. Group, Imperial Coll. Sci. and Technol., London SW7 2BP, UK). 86K2037. Halls, D. J., Achieving faster analysis by electrothermal atomic absorption spectrometry, (Trace Metals Unit, Dept. Biochem., Glasgow Royal Infirmary, Castle St., Glasgow G4 OSF, UK). 86/C2038. Ebdon, L., Evans, K., Hill, S., Jones, P., The determina- tion of tributyltin at the nanogram per litre level by coupled high performance liquid chromatography - atomic absorption spectrometry, (Dept. Environmental Sci., Plymouth Polytechnic, Drake Circus, Plymouth P14 8AA, UK). 8612039. McLaren, J. W., Mykytiuk, A. P., Willie, S. N., Berman, S. S., Determination of trace metals in sea water by inductively coupled plasma mass spectrometry with pre- concentration on silica-immobilised 8-hydroxyquinoline, Anal. Chem., 1985, 57, 2907. (Anal. Chem. Section, Chem. Div., Natl. Res. Council of Canada, Ottawa, Ontario K1A OR9, Canada). I

ISSN:0267-9477    

DOI:10.1039/JA986010193R

出版商:RSC    

年代:1986

数据来源: RSC

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JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, DECEMBER 1986, VOL. 1 401 Obituary Professor J. M. Ottaway It is with deep regret that we announce the sudden death of Professor John Otta- way on 20th October 1986. Amongst John’s many and varied achievements he was Chairman of the JAAS Editorial Board and was the principal driving force behind its conception and initial success. His endless enthusiasm and optimism had been a constant source of inspiration to me as Editor over recent years and he will be dearly missed by his friends and colleagues on the JAAS Board and around the world. Our heartfelt sympathy goes to his wife Barbara. A full obituary will be published in the next issue. Editor

ISSN:0267-9477    

DOI:10.1039/JA986010401b

出版商:RSC    

年代:1986

数据来源: RSC

摘要:

JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, DECEMBER 1986, VOL. 1 403 The Evolution of the ICP as an Ion Source for Mass Spectrometry Alan L. Gray Department of Chemistry, University of Surrey, Guildford, Surrey, GU2 5XH, UK The origins of a new instrumental tech- nique for spectroscopic analysis usually arise well before its engineering develop- ment becomes economically practicable, and may often be traced back to a time well before the development of the cur- rent established technique with which it eventually begins to compete. This is certainly true of the use of the ICP as an ion source for mass spectrometry, which owes its conception to a market need for the next generation but one of atomic spectrometers that was felt in the late 1960s. Inductively coupled plasma atomic emission spectrometry was at that time developing rapidly in research labora- tories around the world, some years before the launch of commercial ICP- AES systems in 1974.The need was defined during a market- ing meeting in 1970 at the UK branch of Applied Research Laboratories where the author was Head of Research. The eventual product was envisaged as a mass spectrometer capable of accepting solid mineral samples and providing multi-ele- ment analyses at levels down to 10 ng g-1 in an analysis time of a few minutes. The specification was formulated around the performance attainable by spark-source mass spectrometry, which, however, had two severe drawbacks, a need for skilled and time-consuming interpretation of the photoplate readout and an analysis rate of only one or two samples per day.A search for an improved ion source had involved the author in a study of the development of solid sample ion sources during the preceding two or more decades but most of the types considered involved difficulties of sample introduction and high vacuum operation. The most promis- ing were felt to be high current arc, ion bombardment or sputtering discharges but the report prepared in December 1970 also contained the following paragraph. “An additional method, which as far as is known has not yet been tried, could possibly be based on a version of the aerosol generator. This is a very con- venient technique for producing a submic- ron particulate aerosol from a large con- Fig. 1. Mass analyser housing, vacuum vessel and capillary arc of original CAP-MS system ducting sample compact in a suitable carrier gas stream. This is then injected into a plasma arc which vaporises and ionises the particles. It should thus be possible to extract from this plasma neu- tral and ionised atoms representative of the sample.The successful use of the method as an optical emission source demonstrates the presence in the arc of atoms representative of the sample, at concentrations which are high by mass spectrometric standards. The problem then of sampling the plasma at approxi- mately atmospheric pressure . . . is similar to that of studying high temperature gas phase chemical reactions and electrical discharges and a number of inlet stages have been designed for these. Some of these are based on a series of differ- entially pumped chambers and as such require rather extensive pumping systems.. . .” Immediately after this report was pre- pared discussions were held with Knew- stubb and Hayhurst who had been exten- sively involved with Sugden at Cambridge in the mass spectrometry of atmospheric pressure flames. 1-3 They considered that a high temperature plasma would be very suitable as an ion source for subsequent analysis by a quadrupole mass analyser and it was decided to proceed with a feasibility study. Although the aerosol generator and capillary arc combination, developed by ARL as the AG-CAP for remote analysis of steel samples in stock yards, was initially proposed, this was partly because it was already available in prototype form in the laboratory concer- ned.It was realised however that other sample introduction methods such as sol- ution nebulisation and laser ablation could also be used and that other plasmas could be more suitable than the capillary arc, so in the patent application filed in March 1971,4 these were all covered, including the ICP and MIP. By June that year a feasibility study was started at the University of Liverpool under J. L. Mor- ruzzi. He designed and built the original ion sampling system based on Hayhurst’s work3 which eventually grew into the404 ocw JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, DECEMBER 1986, VOL. 1 - k research system at the University of Sur- rey. Readers who have seen this will note the resemblance to the original arrange- ment shown in Fig. 1 where the capillary arc unit is shown in front of the sampling aperture at the top right.The aerosol generator is seen at the bottom left. Although many problems had yet to be overcome, this work showed that mass spectra could be produced in this way from metal samples, and the system was transferred at the end of the year-long study to the ARL plant at Luton. Here the author and his colleagues D. Hagger and R. J. Anderson, developed the system further, introducing solutions by a nebuliser, and during the period up to 1975 obtained good spectra, low detection limits and useful isotope ratio results. The first report of this work was made to a meeting of The Society for Analytical Chemistry in April 1974.5 The detection limits reported then are shown in Table 1 from the publication of that presentations and a spectrum of Mg in solution at 1 ng ml-1 from another paper6 in Fig.2. Other publications from this period are listed as references 7-10. It was clear that such a system did provide the basis of an analytical instrument although the origi- nal proposal had met with considerable scepticism from mass spectroscopists used to more conventional ion sources. The capillary arc, as might be expected from its relatively low gas temperature of about 3500 K, proved to be a very limited ion source. Not only did it show severe non-linearity on elements in solution at more than about 10pgml-1 but it also showed serious matrix effects and poor ionisation efficiency for elements of ionisation energy above about 10 eV. Most of this was attributed to the combi- nation of low gas temperature and the difficulty of introducing more than a small fraction of the sample into the hot core of the plasma, where it would be properly dissociated and ionised. It was clear that, although a relatively simple plasma for use in a feasibility demonstration, the capillary arc had to be replaced by a more suitable type, of which the ICP was the obvious contender.Brief consideration had been given earlier to the possibility of Table l.* Elemental detection limits (2a) Detection limit/ Element pg ml-1 Ag . . . . . . . . . . As . . . . . . . . . . Cd . . . . . . . . . . c o . . . . . . . . . . c u . . . . . . . . . . Hg . . . . . . . . . . Mg . . . . . . . . . . Mn . . . . . . . . . . Pb . . . . . . . . . . Se . . . . . .. . . . Zn . . . . . . . . . . 0.004 0.004 0.003 0.0003 0.0008 0.14 0.001 0.00009 0.00004 0.1 0.008 * Data from reference 5 using capillary arc. 13 Na “Mg 1 I m/e Fig. 2. Spectrum showing magnesium at ca. the 0.001 pg ml-1 level, from the capillary arc6 (Re roduced from Proc. Anal. Div. Chem. sot? using an MIP but it was clear that this offered little advantage over the CAP, except possibly a high ionisation temper- ature, but the gas temperature was even lower, about 2000K, in the types avail- able at that time. By this stage considerable interest in the potential of the system, especially for isotope ratio measurements, was being shown by S. H. U. Bowie, then Director of the Institute of Geological Sciences in Gray’s Inn Road, London, (now the British Geological Survey) and his col- league P.J. Moore. With their active support and encouragement a proposal was prepared in June 1975 for them to submit to the European Economic Com- munity for a joint research programme to develop the system further using an ICP. By October of that year this was agreed in principle by the EEC although formal proposals for the work would not be submitted for some time. At just the moment this encouraging news was received the company suffered one of those upheavals in policy which affect the best regulated organisations from time to time and it was decided to drop mass spectrometry from the future product range. The work in the UK thus stopped temporarily. In the meantime the publication of the work in The Analyst7 arid elsewhere had aroused interest abroad and early in 1976 The Ames Laboratory, with support from the EPA, started a project to extend the method to an ICP, R.S. Houk being the research worker involved. By late 1977 Professor V. A. Fassel wrote to the author telling him that the Ames system had now been built and should soon be operating. Almost at the same time the IGS-EEC funding was agreed for the project to restart in the UK so the potential for a race was generated. At this time Robert Craig, of Vacuum Genera- tors, a major mass spectrometry company in the UK, became very interested in the technique as a possible alternative to spark-source mass spectrometry and a joint visit to the Ames Laboratory was made. Collaboration was agreed to be better than competition and so it was arranged.By June, Houk had produced the first spectra of the major ions, Ar, H and 0 from the ICP. During that summer the author spent a time working with Houk at Ames and they succeeded in producing the first spectra of analyte ions, albeit at 50pgml-1, from an ICP.11 Somewhere about this time also Douglas and French at The University of Toronto started work on an MIP system using their Targa atmospheric pressure sampling mass spectrometer. This work eventually formed the basis of the system now marketed by Sciex. In the UK it was decided to base the work at The University of Surrey. With funding. eventually arriving the project started early in 1979. ARL willingly co- operated by transferring the original equipment and the work started on strip- ping and re-building this system, which had been out of use for almost four years, by the author and his colleague A.R. Date. Date had been seconded to the project from IGS, where he had extensive experience of arc emission spectrometry. The rebuilt system is shown in Fig. 3. The opportunity to obtain hands-on experience at Ames of an ICP system and its peculiar problems of interfacing to a mass spectrometer was of considerable value to the reborn project and this was extended by further collaboration on visits in both directions in the following year. Seven months after the start of the project the first spectra were obtained at Surrey and from then on progress was rapid. Both at Ames and Surrey, however, serious limitations were experienced with the apertures used to extract ions from the centre of the plasma flame.In the original work, using the CAP, apertures of 70 ym diameter had proved adequate to induce continuum flow into the first vacuum stage, and when drilled in platinum had proved quite durable. The gas tempera- ture in this system, however, was about 3500K. The gas temperature of the cen- tral channel of the ICP was much higher, probably close to 6000 K and apertures of this size were too small to prevent the formation of a boundary layer across them which thus imposed a cooler inter- mediate plasma region between the ICP and the mass spectrometer, in which a variety of undesirable chemical recombi- nation reactions occurred. Extraction through these apertures still occurred by continuum flow from the gas within the boundary layer however, and excellent spectra and high sensitivity wereJOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, DECEMBER 1986, VOL.1 Fig. 3. Reconstructed system at the University of Surrey obtained.12 The establishment of true continuum flow from the bulk plasma of the ICP, using large diameter apertures having usable lifetimes, was first achieved at Surrey in the latter half of 1980. The developments of the following year enabled for the first time a performance characteristic of that to be expected from the almost ideal nature of the ICP as an ion source to be seen,13 although much remained to be done to produce a useful trace element technique. A more detailed discussion of this stage of the work appears in reference 14. From this point the evolution of the ICP ion source accelerated with startling rapidity.l4 From their early experiments with an ICP, based on microwave plasma sampling with large apertures,15 Douglas and his colleagues in Toronto developed the elegant centre tapped load coil solu- tion to the problems created by the plasma offset potential. This was subse- quently incorporated in the Sciex “Elan” (TM), the first commercial ICP-MS instrument shown in public at the 1983 Pittsburgh Conference. The VG Plasma Quad (TM), based on the second instru- ment built at Surrey for Date to use at the BGS London, had however been announ- ced but not exhibited as a commercial instrument at the International Mass Spectrometry Conference in Vienna in the summer of 1982 and at the 1st Biennial National Atomic Spectroscopy Sympo- sium in Sheffield, July 1982.This was first exhibited in May 1983 in the USA, at the ASMS meeting in Boston. Although it was some time before either of these instruments were installed in a customer’s laboratory and still longer before the first reports of their operation began to appear, a total of about 100 instruments supplied by the two manu- facturers are now in use, and several other commercial systems are rumoured to be on the way. No atomic spectrometry conference is felt to be fully representa- tive without an ICP-MS session and increasing numbers of publications are appearing in the scientific literature. Nevertheless, although the technique is still in the early stages of growth, it does now seem expected to show an unusual degree of maturity for such an infant, well beyond those achieved at a similar age by the preceeding developments of flame and furnace AA and ICP-AES.This is perhaps a consequence of the simplicity of its underlying principle and the evident power of detection in ideal circumstances. In common with many infant prodigies some early experiences have generated both unqualified rapture and unjustified condemnation, both of which owe much to the joint inexperience of early users and the manufacturers. Understanding is growing, particularly in the light of better instrument perfor- mance and reliability, that the power to do multi-element analysis at levels hitherto only oljtainable in a single- element role, imposes responsibilities on the analyst NM times greater, where N is the number of elements observed and M may well be >l.The earliest users have needed to learn hard lessons about labor- atory, atmospheric, blank, solvent and standard contamination hitherto only fully realised in laboratories doing ultra- trace certification work, itself a slow and meticulous process. The sudden increase in the number of analysts able to enter this area has led to a wider understanding of the problems involved in high throughput ultratrace multi-element analysis. Early users who have come to terms with this are now reporting excellent results that really do begin to show evidence of the early promise. The cross disciplinary nat- ure of the technique has led to problems of understanding in both traditionally 405 trained mass spectrometrists and atomic spectrometrists and perhaps the most urgent problem now facing the champions of the method is one of education rather than instrument development.This has inevitably had to await the maturity in instrumental hardware now being more widely seen, and the realisation that the technique is more than another labora- tory toy. As it becomes more firmly established in the accepted range of analy- tical tools, more need and more oppor- tunity will arise for this educational pro- cess to take place. A fuller and more extended role for short courses and work- shops in conference programmes in the future is to be welcomed. However this occurs in detail there seems little doubt that this healthy youngster ICP-MS has an important role to play in the future. The author is happy to acknowledge the contribution of the colleagues and asso- ciates mentioned in the text and of the many people who have also contributed to the development of ICP-MS but are not acknowledged by name.No method such as this is evolved in isolation from other workers even though their contribution may have been no more than to start a train of thought. The development of the technique at The University of Surrey would not have been possible without the encouragement and financial support of The British Geo- logical Survey (NERC) and Directorate General for Science, Research and Deve- lopment (DGXII) of The European Eco- nomic Community. 1. 2. 3. 4. 5. 6 . 7. 8. 9. 10. 11. 12. 13. 14. 15. References Knewstubb, P. F., and Sugden, T. M., Proc. R. SOC., 1960, 255, 520. Sugden, T. M., in Reed, R. I., Editor, “Mass Spectrometry,” Academic Press, London, 1965. Hayhurst, A. N., IEE Trans. Plasma Sci., 1974, PS.2, 115. British Patent 1371 104, 1971. Gray, A . L., Proc. SOC. Anal. Chem., 1974, 11, 182. Gray, A . L., Proc. Anal. Div. Chem. SOC., 1975, 12, 94. Gray, A. L., Analyst, 1975, 100, 289. Gray, A. L., Anal. Chem., 1975, 47, 600. Gray, A. L., Hagger, D . , and Ander- son, R. J . , Proceedings of XVIII Collo- qium Spectroscopicurn Internationale, Grenoble, 1975,II, 482. Anderson, R. J., and Gray, A. L., Proc. Anal. Div. Chem. SOC., 1976, 13, 284. Houk, R. S . , Fassel, V. A., Flesch, G. D., Svec, H. J . , Gray, A. L., and Taylor, C. E., Anal. Chem., 1980, 52, 2283. Date, A. R., and Gray, A. L., Analyst, 1981, 106, 1255. Date, A. R., and Gray, A. L., Spectro- chim. Acta, Part B, 1983,38,29. Gray, A . L., Spectrochim. Acta, Part B , 1985,40, 1525. Douglas, D. J . , Quan, E. S. K., and Smith, R. G., Spectrochim. Acta, Part B , 1983,38, 39.

ISSN:0267-9477    

DOI:10.1039/JA9860100403

出版商:RSC    

年代:1986

数据来源: RSC

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406 JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, DECEMBER 1986, VOL. 1 Conference Reports 69th Canadian Chemical Conference: 1st-4th June, 1986, University of Saskatchewan, Canada The University of Saskatchewan was the 1986 host of this annual conference of the Chemical Institute of Canada, which covers all aspects of chemistry. The organisers were delighted that the analy- tical chemistry programme turned out to be the biggest in the history of the conference, with 83 invited and contri- buted papers and 9 posters. It is fashion- able for conference organisers to aim for a spectacular opening in the form of light shows, etc., but this time nature obliged during the pre-conference evening mixer with a brilliant thunderstorm and atten- dant tornadoes. Fortunately, the perfect weather which accompanied the remainder of the conference presented this beautiful campus at its best.Cer- fainly , the friendly, informal atmosphere that pervaded during the analytical ses- sions was more in keeping with this weather than the opening storm! Most of the atomic spectrometry presentations were in two symposia: “Microsampling Techniques in Atomic Spectrometry,’’ and “Recent Develop- ments in Plasma Spectrometry.” It was appropriate that the Fischer Scientific Award in analytical chemistry went to Shier Berman of the NRC, who has made outstanding contributions in the areas of both symposia. His award lecture was the opening event of the analytical pro- gramme. The symposium on microsam- pling techniques was concerned mainly with electrothermal atomic absorption spectrometry, reflecting its high level of activity in Canada.Ralph Sturgeon presented the opening lecture on the fundamentals of atomisation, and this was followed by a balanced programme of fundamental and applied papers, includ- ing contributions from both Canada and the USA. A recurring theme was the direct analysis of solids, which is un- doubtedly an area of increasing interest. Also covered was the introduction of microsamples into ICPs, in Gary Hor- lick’s invited presentation. The plasma spectrometry symposium followed and mostly retained the same compact (and lively) audience. Papers were about evenly divided between ICP-AES and ICP-MS, and the strong interest in the latter is hardly surprising as one of the only two instrument manufacturers is a Canadian company.Gary Horlick and Jim McLaren both presented a substantial amount of data, which confirmed that ICP-MS is already approaching maturity as a technique ready for routine use. The speakers on ICP-AES included Mike Blades. Delegates able to drag themselves away from the symposia could visit the impres- sive analytical facilities of some of the Government research stations located on campus. These include the Plant Bio- technology Institute of the National Research Council, the Animal Pathology Laboratory of Agriculture Canada, and the Saskatchewan Research Council, which recently acquired the first ICP-MS instrument in the Province. Kenneth W. Jackson University of Saskatchewan, Saskatoon, Sask., Canada Federation of Analytical Chemistry and Spectroscopy Societies (FACSS): 13th Annual Meeting, 28th September-3rd October 1986, St.Louis, MS, USA Unlike the well known quantum phe- nomenon whereby the act of observation perturbs the system being studied, obser- vation of the FACSS conference perturbs only the observer. With nearly 700 oral presentations delivered over four and a half days in 10 or 11 parallel streams, for the 1500 delegates to listen to, not to mention a sizeable exhibition, 8 half-day or one-day short courses and the employ- ment bureau, it is not possible for one person to have fully covered all aspects of a conference of this size. While I am apologising for the somewhat less than comprehensive coverage I have been able to provide, I have to confess that I sneaked out of some of the atomic spec- troscopy sessions to listen to contributions from electrochemists and flow injection analysts. For most delegates, I imagine, there were some clashes of interest.This meant that some careful planning was needed the night before in order to map out the next day’s schedule. Given the complexity of the programme, some kind of com- puter based optimising strategy is really needed and my recommendation to next year’s organisers is to issue the pro- gramme on floppy disk, together with a modified simplex or critical path analysis sub-routine. I also have to admit that I was viewing ,this conference through the eyes of someone who had never attended a con- ference in the USA before and, in fact, had not set foot on American soil since the first American set foot on the moon.Being of a conscientious disposition, I was able to resist the alternative attractions of rain-soaked, downtown St. Louis, such as they were, and spent most of the working day in the convention centre. As a venue for a conference, this seemed ideal. All the lecture halls were right next to each other and right next to the exhibition hall and the whole lot was very close to the hotel accommodation. Despite there Gateway Arch, St. LouisJOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, DECEMBER 1986, VOL. 1 being no time allocated for “change over,” there was no problem in getting from one lecture stream to another in time to hear the start of the next lecture. With most of the presentations allocated a total of 20 minutes including questions, it was quite important not to miss the opening few sentences.Atomic spectroscopists have no cause for complaint as every conceivable aspect of the subject was covered in one way or another. Monday saw a morning sympo- sium devoted to “Calibration and Curve Fitting for Atomic Spectroscopy,” one of the streams jointly organised with the RSC. Most of the work was done by my co-organiser, Dr. Nancy Miller-Ihli from the US Department of Agriculture. Our session clashed with one on “Lasers and Mass Spectrometry,” one on “Emission Spectrochemical Analysis, Sources and Signals,” a stream which appeared to feature papers about techniques contain- ing two of everything, “Dual ICP-AES” and “Tandem Flame Atomic Spectro- scopy” from groups at Wayne State and North Carolina State Universities, respectively.This stream also featured the first of no less than 18 contributions from Professor Gary Hieftje’s group at Indiana. Also that morning were a smat- tering of “Hyphenated Techniques in Separation Science,” which included liquid chromatography hyphen any atomic spectroscopy technique you care to name. The afternoon saw the continua- tion of the “Lasers and Mass Spec- trometry” sessions and another of the symposia that the RSC had been involved in. This time it was “Furnace Atomic Emission Spectroscopy” organised jointly by the late Professor John Ottaway and Dr. Jim Harnly (also from the US Depart- ment of Agriculture). This session included contributions from two of the small band of Europeans, Dr. Erik Lund- berg from the University of Umei, Sweden, and Dr.Heinz Falk from the Central Institute for Optics and Spectro- scopy, East Berlin, DDR. Tuesday morn- ing saw the same pair of organisers in action again with a symposium on “Back- ground Correction in Atomic Absorp- tion.” In amongst the contributions that might be expected, was one relatively new technique namely the use of a photodiode array for ICP-AES, described by Dr. Piet van der Plas from Delft University of Technology, The Netherlands. This symposium clashed with one on “ICP- MS.” The afternoon contained a rather mixed bag in “Atomic Absorption Spec- troscopy,” which clashed with “High Cur- rent Emission Spectroscopy Sources.” The early evening contained the poster session, to which delegates were enticed by the offer of some cheese and wine.Again a lot of atomic spectroscopy, but this time mainly applications to real sam- ples that ranged from spruce needles to renal fluids. This was the only aspect of the conference that was not done as well as at a European conference. On the whole, the posters contained too much information that could only be read from a distance of six inches. Wednesday morning kicked off at 8.40 a.m. (as did many of the sessions) with “ICP Excitation Mechanisms,” just the thing to aid the digestion of what the “Burger King” thinks is fit for consump- tion at breakfast time. This theme was continued in the afternoon with “Dis- charge Excitation Mechanism and Scien- tific Fundamentals,” which clashed with “Solids Analysis with Hollow Cathodes, Glow Discharges and Microdischarges” ; this session contained a couple of papers describing the use of a glow discharge source in which considerable increase in the atomic population could be achieved by impacting the surface with a gas jet.It 407 appeared as though the device was avail- able from a company called Analyte Corp. and had been developed at Oregon State University. Running throughout the day was the third symposium that the RSC had helped to organise, “Multi-dimensional Fluores- cence” put together by Professor Jim Miller and Professor Isiah Warner from Emory University. Thursday had an all-day session on “Atomic Fluorescence and Laser En- hanced Ionization Spectroscopies .’, This clashed with both “Solids Analysis with ICP-MS and Spark Discharges” and “Fundamentals of Electrothermal Atomi- sation.” This latter stream was probably the most international with contributions from Sweden (Professor Anders Ceder- gren), West Germany (Drs. Bernhard Welz and G. Miiller-Vogt), the UK (the late Professor John Ottaway), East Ger- many (Dr. Heinz Falk) and Canada (Professor Ken Jackson and Dr. Ralph Sturgeon), Inductively coupled plasma mass spectrometry was also getting more good coverage in a stream entitled “New Methods and Techniques: ICP-MS and Others. ” The last half day of the conference contained “Applications of Electrother- mal Atomisation,” “Applications of Atomic Spectroscopy” and one of the very few mentions of X-ray methods in a rather heterogeneous stream entitled “Surface, X-ray and Miscellaneous Methods.” The resulting free afternoon just allowed enough time for delegates to visit the amazing Gateway Arch before staggering off to the airport and unwind while watching the TV monitors for announcements about the delayed flights home. Julian Tyson Loughborough University of Technology, UK

ISSN:0267-9477    

DOI:10.1039/JA9860100406

出版商:RSC    

年代:1986

数据来源: RSC

摘要:

JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, DECEMBER 1986, VOL. 1 407 ASU Highlights The length of the ASU Review on “,Minerals and Refractories” that appears in this issue of JAAS is directly related to the review perod being 21 months. This lengthy period is a consequence of chang- ing an annual publication, Annual Reports on Analytical Atomic Spectro- scopy, into one which is spread between the six issues of JAAS appearing in one year. Subsequent reviews on this topic will cover the research papers and confer- ence presentations abstracted during 12- month periods. Papers relating to the analysis of min- erals far outnumber those on refractories. Whilst much valuable work is being car- ried out, and published, on the applica- tion of AAS and ICP-AES, as well as spectrographic techniques, to the analysis of geological material, anyone working in this area is likely to be keenly interested in the developments that are occurring in ICP-MS.The various advantages of ICP- MS that are discussed in this review show it to be a technique particularly suited to the analysis of mineral material, enabling rare earth elements to be determined with ease and isotopic ratios to be measured. Although it is encouraging that advances are being made in alternative methods of sample introduction, such as slurry injection, laser ablation and the insertion of solids, for the more establi- shed techniques of AAS and ICP-AES, a new approach to sample preparation will be required if ICP-MS is to realise its full potential. Much effort, however, is still being expended in optimising acid decom- positions and flux fusions for geological material, and the topic of sample prepara- tion is covered quite extensively in this review. David Hickman The Metropolitan Police Forensic Science Laboratory, London, UK

ISSN:0267-9477    

DOI:10.1039/JA9860100407

出版商:RSC    

年代:1986

数据来源: RSC