摘要:

SECOND RIO SYMPOSIUM ON ATOMIC ABSORPTION S P E C T R O M E T R Y June 21-28 1992 Rio de Janeiro Brazil The Second Rio Symposium will be divided into two parts. In the first part the emphasis will be on furnace flame and hydride techniques and will be held at the Pontificia Universidade Cat6lica do Rio de Janeiro June 21-24 The second part will be devoted entirely to furnace atomic absorption spectrometry and will be held at the Hotel Nas Rocas in Buzios located 154 km north of the city of Rio de Janeiro June 26-28. Part I The programme will include invited lectures oral presentation of papers and posters covering the following topics introduction of samples coupling with flow injection; instrument development; analytical quality assurance; interference studies; application to environmental biological and industrial samples and speciation.Part II The programme with include invited lectures and presentation of papers covering the following topics atomization theories and mechanism; temperature and atom distribution; surfaces and substrate materials; combined techniques; chemical modification; solid and slurry sampling and new concepts. lnvi ted Lecturers The following scientists were invited to present lectures J. Alvarado (Caracas Venezuela) F. J. Krug (Piracicaba Brazil) Dm Batiston1 (auenos AireS Argentina) M.T.C. de Loos-Vollebregt (Delft Holland) D. Bradshaw (Lake Mary USA) B mVm L’vov (1 eningrad USSR) Km Dittrich (Leipzig Germany) N. Miller-lhli (Beltsville USA) 2. Fang (Shenyang China) G. Muller-Vogt (Karlsruhe Germany) G.Schlemmer (Uberlingen Germany) W. Frech (Umea Sweden) JmMm Harnly (Beltsville USA) M. Hinds (Ottawa Canada) W. Slavin (Nowalk USA) J.A. Holcombe (Austin USA) R. Sturgeon (Ottawa Canada) K.W. Jackson (Albany USA) D.L. Styris (Richland USA) G. Knapp (Graz Austria) 8. Welz (Uberlingen Germany) A Course on the determination of trace and ultratrace elements will be alsooffered. There will also be an exhibition and a social programme. Further information can be obtained from the organizers AmJ. Curtius Depto. de Quimica da PUC/Rio 22.453 Rio de Janeiro Brazil Phone (021) 529-9547 Telefax (021) 220-2305. B. Welz Bodenseewerk Perkin-Elmer Postfach 1 120 Uberlingen Germany Phone (07551) 81-3791 Telefax (07551) 1612.Ramon M. Barnes Editor Department of Chemistry GRC Towers University of Massachusetts Amherst MA 01003-0035 Telephone (41 3) 545-2294 fax 545-4490 0 bjective The ICP INFORMATION NEWSLETTER is a monthly journal published by the Plasma Research Group at the University of Massachusetts and is devoted exclusively to the rapid and impartial dissemination of news and literature information re- lated to the development and applications of plasma sources for spectrochemical analysis.Background ICP stands for inductively coupled plasma discharge which during the past decade has become the leading spectrochemi- cat excitation source for atomic emission spectroscopy. ICP sources also are applied commercially as an ion source for mass spectrometry and as an atom and ion cell in atomic fluorescence spectrometry. 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 of the ICP INFORMA 7lON NEWSLETTER in 1975.Other popular plasma sources i.e. microwave induced plasmas direct current plas- mas and glow discharges also are included in the scope of the ICP INFORMA TION NEWSLETTER. Scope As the only authoritative monthly journal of its type the ICP INFORMA TlON NEWSLETTER is read in more than 40 coun- tries by scientists actively applying or planning to use the ICP or other types of plasma spectroscopy. For the novice in the field the ICP INFORMA TlON NEWSLETTER provides a amuse and systematic source of information and background material needed for the selection of instrumentation or the development of methodology.For the experienced scientist it offers a sin- gle-source reference to current developments and literature. Editorial The ICP INFORMATION NEWSLETTER is edited by Dr. Ramon M. Barnes Professor of Chemistry University of Mas- sachusetts 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 viewpoints and developments. Dr. Barnes has been conducting plasma research on ICP and other dis- charges since 1968. He also serves as chairman of the Winter Conference on Plasma Spectrochemistry sponsored by the ICP INFORMA TION NEWSLETTER. Regular Features Original submitted and invited research articles by ICP Complete bibliography of all major ICP publications.Abstracts of all ICP papers presented at major US and inter- First-hand accounts of world-wide ICP developments. Special reports on dcp microwave glow discharge and other Calendar and advanced programs of plasma meetings. Technical translations and reprints of critical foreign-lan- Critical reviews of plasma-related books and software. and plasma experts. national meetings. plasma progress. guage ICP papers. Conference Activities The ICP INFORMA TlON NEWSLETTER has sponsored six international meetings on developments in atomic plasma spectrochemical analysis since 1 980 in San Juan Orlando San Diego St. Petersburg and Kailua-Kona. Meeting pro- ceedings have appeared as Developments in Atomic Plasma Spectrochemical Analysis (Wiley) Plasma Spectrochemistry and Plasma Spectrochemistry /I-IV (Pergamon Press) as well as in special issues of Spectrochimica Acta Part B and Journal of Analytical Atomic Spectrometry.The 1992 Winter Confer- ence on Plasma Spectrochemistry will be held in San Diego California January 6 - 11 1992; its proceedings will be published by Fall 1992. Subscription Information 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 17 runsfrom June 1991 through May 1992. Backissues beginning with Volume 1 May 1975 also are available. To begin a subscription complete the form below and submit it with prepayment or purchase information. For additional informa- tion please call (41 3) 545-2294 fax (41 3) 545-4490 or contact the Editor.Credit cards accepted. To order complete this section and send it to ICP Information Newsletter %Dr. Ramon M. Barnes Depart- ment of Chemistry Lederle GRC Towers University of Massachusetts Amherst MA 01 003-0035 USA. Start a subscription for the following issue 0 Volume(s)- (June 19- - May 19- ) or 13 19 (January - December). Enclosed 13 Prepayment 0 Check or money order OVISA 0 Mastercard Account No. (All 13 or 16 digits) D Purchase order (No. ) or D Send invoice. Date Cardholder Name Expiration date Cardholder Signature .Amount Due $ Mail to Name Organization Address City State/Country Z I P/ Po st alcode Telephone TeleNfax Note For each credit-card transaction a 3% service charge will be added reflecting our bank charges. Current subscription rates are $60 (North America) $85 (Europe South America) or $94 (Africa Asia Indian/Pacific Ocean Areas Middle East and USSR). Back issue rates available on request. All payments should be made with US dollars by draft on a US bank by international money order or by credit card. Foreign bank checks are not accepted. Circle 003 for further information

ISSN:0267-9477    

DOI:10.1039/JA99106BP022

出版商:RSC    

年代:1991

数据来源: RSC

摘要:

Journal of Analytical Atomic Spectrometry (Including Atomic Spectrometry Updates) JAAS Editorial Board* Chairman B L Sharp (Loughborough UK) J. Egan (Cambridge UK) D A. Hickman (London UK) J. Marshall (Middlesbrough UK) J. M. Mermet (Wleurbanne France) D. L. Miles (Keyworth UK) R. D. Snook (Manchester UK) *The JAAS Editorial Board reports to the Analytical Editorial Board Chairman A. G. Fogg (Loughborough UK) JAAS Advisory Board F C Adams (Antwerp Belgium) R M Barnes (Amherst MA USA) G M Hieftje (Bloomington IN USA) L Bezur (Budapest Hungary) G Horlick (Edmonton Canada) R F Browner (Atlanta GA USA) S Caroli (Rome Italy) A J Curtius (Rio de Janeiro Brazid L de Galan (Vlaardingen The Netherlands) J B Dawson (Leeds UK) R E Sturgeon (Ottawa Canada) K Dittrich (Leipzig Germany) W Frech (Umed Sweden) K Fuwa (Tokyo Japan) A L Gray (Egham UK) S Greenfield (Loughborough UK) B V L'vov (Leningrad USSR) Ni Zhe-ming (Belling China) N Omenetto (lspra Italy) T C Rains (Charleston SC USA) R Van Grieken (Antwerp Belgium) A Walsh K B (Victoria Australia) B Welz ( Uberlingen FRG) T S West (Aberdeen UK) Atomic Spectrometry Updates Editorial Board Chairman "D L J Armstrong (Dumfries UK) J R Bacon (Aberdeen UK) C Barnard (Glasgow UK) R M Barnes (Amherst MA USA) S Branch (High Wycombe UK) R Bye (Oslo Norway) J Carroll (Middlesbrough UK) M R Cave (Keyworth UK) *J M Cook (Keyworth UK) "M S Cresser (Aberdeen UK) H M Crews (Norwich UK) J S Crighton (Sunbury-on-Thames UK) J R Dean (Newcastle upon Tyne UK) *J B Dawson (Leeds UKI *J Egan (Cambridge UK) "A T Ellis (Oxford UK) J Fazakas (Bucharest Romania) D J Halls (Glasgow UK) *D A Hickman (London UK) "S J Hill (Plymouth UK) K W Jackson (Albany NY USA) R Jowitt (Middlesbrough UK) K Kitagawa (Nagoya Japan) J Kubova (Bratislava Czechoslovakia) "D Littlejohn (Glasgow UK) "J Marshall (Middlesbrough UK) Miles (Keyworth UK) H.Matusiewicz (Poznan Poland J. M. Mermet (Villeurbanne France) R. G. Michel (Storrs CT USA) T. Nakahara (Osaka Japan) Ni Zhe-ming (Beijing China) P. R. Poole (Hamilton New Zealand W. J. Price (Ashburton UK) C. J. Rademeyer (Pretoria South Africa) M. H. Ramsey (London UK) A. Sanz-Medel (Oviedo Spain) "B. L. Sharp (Loughborough UK) I. L. Shuttler (Uberlingen FRG) S. T. Sparkes (Plymouth UK) R. Stephens (Halifax Canada) J. Stupar (Ljubljana Yugoskwia) R.E. Sturgeon (Ottawa Canada) A. P. Thorne (London UK) G. C. Turk (Gaithersburg MD USA) J. F. Tyson (Amherst MA USA) *A. M . Ure (Aberdeen UK) S . J. Walton (Crawley UK) P. Watkins (London UK) B. Welz (Uberlmgen FRG). J. Williams (Egham UK) J. B. Willis (Victoria Australia) *A. Taylor (Guildford UK) *Members of the ASU Executive Committee Editor JAAS Judith Egan The Royal Society of Chemistry Thomas Graham House Science Park Milton Road Cambridge CB4 4WF UK Telex No 818293 Fax 0223 423623 Beltsville MD 20705 USA Assistant Editors Brenda Holliday Editorial Secretary Monique Warner US Associate Editor JAAS Dr J M Harnly US Department of Agriculture Beltsville Human Nutriton Research Center Telephone 0223 420066 BLDG 161 BARC-EAST Telephone 301 -344-2569 Paula O'Riordan Sheryl Whitewood Advertisements Advertisement Department The Royal Society of Chemistry Burlington House Piccadilly London W I V OBN UK.Telephone 071-437 8656. Fax 071-437 8883 Information for Authors Full details of how to submit materials for publica- tion in JAAS are given in the Instructions to Authors in Issue 1. Separate copies are available on request. The Journal of Analytical Atomic Spectrometry (JAAS) is an international journal for the publica- tion of original research papers communications and letters concerned with the development and analytical application of atomic spectrometric techniques The journal is published eight times a year including comprehensive reviews of specific topics of interest to practising atomic spectrosco- pists and incorporates the literature reviews which were previously published in Annual Reports on Analytical Atomic Spectroscopy (ARAAS) Manuscripts intended for publication must de- scribe original work related to atomic spectromet- ric analysis Papers on all aspects of the subject will be accepted including fundamental studies novel instrument developments and practical ana- lytical applications As well as AAS.AES and AFS papers will be welcomed on atomic mass spec- trometry and X-ray fluorescence/emission spec- trometry Papers describing the measurement of molecular species where these relate to the char- acterization of sources normally used for the pro- duction of atoms or are concerned for example with indirect methods of analysls will also be ac- ceptable for publication Papers describing the de- velopment and applications of hybrid techniques (e g GC-coupled AAS and HPLC-ICP) will be par- ticularly welcome Manuscripts on other subjects of direct interest to atomic spectroscopists in- cluding sample preparation and dissolution and analyte pre-concentration procedures as well as the statistical interpretation and use of atomic spectrometric data will also be acceptable for pub- lication There is no page charge The following types of papers will be consid- ered full papers describing original work Communicabons which must be on an urgent matter and be of obvious scientific importance Communications receive priority and are usually published within 2-3 months of receipt They are intended for brief descriptions of work that has -progressed to a stage at which it is likely to be valuable to workers faced with similar problems Reviews which must be a critical evaluation of the existing state of knowledge on a particular 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 elsewhere except by permission Submission of a manu- script will be regarded as an undertaking that the same material is not being considered for publica- tion by another journal Manuscripts (three copies typed in double spacing) should be sent tb Judith Egan Editor JAAS or Dr J M Harnly US Associate Editor JAAS All queries relating to the presentation and sub- mission of papers and any correspondence re- garding accepted papers and proofs should be directed to the Editor or IJS Editor (addresses as above) Members of the JAAS Editorial Board (who may be contacted directly or via the Editorial Office) would welcome comments suggestions and advice on general policy matters concerning JAAS Fifty reprints are supplied free of charge.Journal of Analytical Atomic Spectrometry IJAAS) (ISSN 0267-9477) is published eight times a year by The Royal Society of Chemistry Thomas Graham House Science Park Milton Road Cambridge CB4 4WF. UK. All orders accompanied with payment should be sent directly to The Royal Society of Chemistry Turpin Tractions Ltd. Blackhorse Road Letchworth Herts. SG6 1 HN UK Tel.+44 (0) 462 672555; Telex 825372 Turpin G; Fax +44 (0) 462 480947. Turpin Transactions Ltd. is wholly owned by The Royal Society of Chemistry. 1991 Annual subscription rate EC f309.00 USA $728.00 Rest of World f355.00. Customers should make payments by cheque in sterling payable on a UK clearing bank or in US dollars payable on a US clearing bank. Air freight and mailing in the USA by Publications Expediting Inc. 200 Meacham Avenue Elmont NY 11 003. USA Postmaster send address changes to Journal of Analytical Atomic Spectrometry IJAASI Publications Expediting Inc. 200 Meacham Avenue Elmont NY 11 003. Second class postage paid at Jamaica NY 11431. All other despatches outside the UK by Bulk Airmail within Europe Accelerated Surface Post outside Europe.PRINTED IN THE UK. 0 The Royal Society of Chemistry 1991. All rights reserved. No pact 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 permissiori of the publishers.Journal of Analytical Atomic Spectrometry (Including Atomic Spectrometry Updates) JAAS Editorial Board* Chairman L Ebdon (Plymouth UK) J Egan (Cambridge UK) D L Miles (Keyworth UK) D A Hickman (London UK) B L Sharp (Loughborough UK) J Marshall (Middlesbrough UK) R D Snook (Manchester UK) J M Mermet (Villeurbanne France) "The JAAS Editorial Board reports to the Analytical Editorial Board Chairman A G Fogg (Loughborough UK) F C Adarns (Antwerp Belgium) R M Barnes (Amherst MA USA) L Bezur (Budapest Hungary) R F Browner (Atlanta GA USA) S Caroli (Rome Italy) A J Curtius (Rio de Janeiro Brazid L de Galan (Vlaardingen The Nethei J B Dawson (Leeds UK) K Dittrich (Leipzig GDR) W Frech (Umes Sweden) K Fuwa (Tokyo Japan) A L Gray(€gham UK) JAAS Advisory Board S Greenfield (Loughborough UK) G M Hieftje (Bloomrngton IN USA) G Horlick (Edmonton Canada) B V L'vov (Leningrad USSR) Ni Zhe-ming (Belling China) N Omenetto (lspra /tala R E Sturgeon (Ottawa Canada) R Van Grieken (Antwerp Belgium) A Walsh K B (V,ctoria Australia) B Welz (Uberlingen FRG) T S West (Abderdeen UK) -lands) T C Rains (Charleston SC USA) Atomic Spectromery Updates Editorial Board Chairman "D.L. Miles (Keyworth UK) J. Armstrong (Dumfries UK) J. R. Bacon (Aberdeen UK) C.Barnard (Glasgow UK) R. M . Barnes (Amherst MA USA) S . Branch (High Wycombe UK) R. Bye ( Oslo Norway) J. Carroll (Middlesbrough UK) M . R. Cave (Keyworth UK) "J. M. Cook (Keyworth UK) "M. S. Cresser (Aberdeen UK) H. M. Crews (Norwich UK) J. S . Crighton (Sunbury-on-Thames UK) J. R. Dean (Newcastle upon Tyne UK) H. Matusiewicz (Poznan Poland J. M. Mermet (Villeurbanne France) R. G. Michel (Storrs CT USA) T. Nakahara (Osaka Japan) Ni Zhe-rning (Beijing China) P. R. Poole (Hamilton New Zealand W. J. Price (Ashburton UK) C. J. Rademeyer (Pretoria South Africa) M. H. Ramsey (London UK) A. Sanz-Medel,,( Oviedo Spain) I. L. Shuttler (Uberlingen FRG) S. T. Sparkes (Plymouth UK) R. -Stephens (Halifax Canada) J. Stupar (Ljubljana Yugoslavia) R. E. Sturgeon (Ottawa Canada) A.Taylor (Guildford UK) A. P. Thorne (London UK) G. C. Turk (Gaithersburg 11.10 USA) J. F. Tyson (Amherst MA USA) "A. M. Ure (Aberdeen UK) S. J. Walton (Crawley UK) P. Watkins (London UK) B. Welz (Uberlingen FRG) J. Williams (Egharr UK) J. B. Willis (Victoria Australia) "J. B. Dawson (Leeds UK) "L. Ebdon (Plymouth UK) "J. Egan (Cambridge UK) "A. T. Ellis (Oxford UK) "D. J. Halls (Glasgow UK) "D. A. Hickman (London UK) "S. J. Hill (Plymouth UK) J. Fazakas (Bucharest Romanla) K. W. Jackson (Albany NY USA) R. Jowitt (Middlesbrough UK) K. Kitagawa (Nagoya Japan) "D. Littlejohn (Glasgow UK) "J. Marshall (Middlesbrough UK) "Members of the ASU Executive Committee Editor JAAS Judith Egan The Royal Society of Chemistry Thomas Graham House Science Park Milton Road Cambridge CB4 4WF UK Telex No 81 8293 Fax 0223 423623 Assistant Editors Brenda Holliday Editorial Secretary M on iq ue Warner US Associate Editor JAAS Dr J M Harnly US Department of Agriculture Beltsville Human Nutriton Research Center Beltsville MD 20705 USA Telephone 301 -344-2569 Telephone 0223 420066 BLDG 161 BARC-EAST Paula O'Riordan Sheryl Whitewood Advertisements Advertisement Department The Royal Society of Chemistry Burlington House Piccadilly London W1 V OBN UK. Telephone 071 -437 8656.Fax 071 -437 8883 Information for Authors Full details of how to submit materials for publica- tion in JAAS are given in the Instructions to Authors in Issue 1 Separate copies are available on request The Journal of Analytical Atomic Spectrometry (JAAS) is an international journal for the publica- tion of original research papers communications and letters concerned with the development and analytical application of atomic spectrometric techniques The journal is published eight times a year including comprehensive reviews of specific topics of interest to practising atomic spectrosco- pists and incorporates the literature reviews which were previously published in Annual Reports on Analytical Atomic Spectroscopy (ARAAS) Manuscripts intended for publication must de- scribe original work related to atomic spectromet- ric analysis Papers on all aspects of the Subject will be accepted including fundamental studies novel instrument developments and practical ana- lytical applications As well as AAS AES and AFS papers will be welcomed on atomic mass spectro- metry and X-ray fluorescence/emission spectro- metry Papers describing the measurement of molecular species where these relate to the char- acterization of sources normally used for the pro- duction of atoms or are concerned for example with indirect methods of analysis will also be ac- ceptable for publication Papers describing the de- velopment and applications of hybrid techniques ( e g GC-coupled AAS and HPLC-ICP) will be par- ticularly welcome Manuscripts on other subjects of direct interest to atomic spectroscopists in- cluding sample preparation and dissolution and analyte pre-concentration procedures as well as the statistical interpretation and use of atomic spectrometric data will also be acceptable for pub- lication There is no page charge The following types of papers will be consid- ered Full papers describing original work Cornrnun/cations which must be on an urgent matter and be of obvious scientific importance Communications receive priority and are usually published within 2-3 months of receipt They are intended for brief descriptions of work that has progressed to a stage at which it is likely to be valuable to workers faced with similar problems Reviews which must be a critical evaluation of the existing state of knowledge on a particular 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 elsewhere except by permission Submission of a manu- script will be regarded as an undertaking that the same material is not being considered for publica- tion by another journal Manuscripts (three copies typed in double spacing) should be sent to Judith Egan Editor JAAS or Dr J M Harnly US Associate Editor JAAS All queries relating to the presentation and sub- mission of papers and any correspondence re- garding accepted papers and proofs should be directed to the Editor or US Editor (addresses as above) Members of the JAAS Editorial Board (who may be contacted directly or via the Editorial Office) would welcome comments suggestions and advice on general policy matters concerning JAAS Fifty reprints are supplied free of charge Journal of Analytical Atomic Spectrometry (JAAS) (ISSN 0267-9477) is published eight times a year by The Royal Society of Chemistry Thomas Graham House Science Park Milton Road Cambridge CB4 4WF UK All orders accompanied with payment should be sent directly to The Royal Society of Chemistry Turpin Tractions Ltd Blackhorse Road Letchworth Herts SG6 1 HN UK Tel +44 (0) 462 672555 Telex 825372 Turpin G Fax +44 (0) 462 480947 Turpin Transactions Ltd is wholly owned by The Royal Society of Chemistry 1991 Annual subscription rate EC f309 00 USA $728 00 Rest of World €355 00 Customers should make payments by cheque in sterling payable on a UK clearing bank or in US dollars payable on a US clearing bank Air freight and mailing in the USA by Publications Expediting Inc 200 Meacham Avenue Elmont NY 11003 USA Postmaster send address changes to Journal of Analytical Atomic Specrrometw UAASI Publications Expediting Inc 200 Meacham Avenue Elmont NY 11003 Second class postage paid at Jamaica NY 11431 All other despatches outside the UK by Bulk Airmail within Europe Accelerated Surface Post outside Europe PRINTED IN THE UK 0 The Royal Society of Chemistry 1991 All rights reserved No part of this publication may be reproduced stored in a retrieval system or transmitted in any form or bv anv means electronic mechanical photographic recording or otherwise without the prior permission of the publishers

ISSN:0267-9477    

DOI:10.1039/JA99106FX029

出版商:RSC    

年代:1991

数据来源: RSC

摘要:

JASPE2 6(8) 587-678 283R-340R ( 1 99 1 ) December 199 1 Journal of Analytical Atomic Spectrometry I n c I u d i n g Atom ic S pect ro m e t ry U pd at es CONTENTS NEWS AND VIEWS 587 Conference Report 588 Conference and Meetings 589 Courses 589 Papers in Future Issues PAPERS 591 601 605 609 61 5 623 627 631 637 643 647 653 661 669 673 675 677 Matrix Interferences From Methacrylic Acid Solutions in Inductively Coupled Plasma Mass Spectrometry-J Marshall J Franks High Speed Photographic Study of Plasma Fluctuations and Intact Aerosol Particles or Droplets in Inductively Coupled Plasma Mass Spectrometry-Royce K Winge J S Crain R S Houk Minimization of Non-spectroscopic Matrix Interferences for the Determination of Trace Elements in Fusion Samples by Flow Injection Inductively Coupled Plasma Mass Spectrometry-Jiansheng Wang E Hywel Evans Joseph A Caruso Determination of Uranium and Thorium in Aluminium With Flow Injection and Laser Ablation Inductively Coupled Plasma Mass Spectrometry-Peter van de Weijer Peter J M G.Millings Wilhelmina L. M Baeten Wim J M de Laat Flow Injection On-line Separation and Preconcentration for Electrothermal Atomic Absorption Spectrometry. Part 2. Determination of Ultra-trace Amounts of Cobalt in Water-Michael Sperling Xuefeng Yin Bernhard Welz Slurry Sampling and Fluorination-Electrothermal vaporization Inductively Coupled Plasma Atomic Emission Spectrometry for the Direct Determination of Molybdenum in Food-Hu Bin Jiang Zucheng Zeng Yun'e Cold Vapour Atomic Absorption Method for the Determination of Mercury in Iron(iii) Oxide and Titanium Oxide Pigments Using Slurry Sample Introduction-lgnacio Lopez Garcia Maria Jeslis Vizcaino Martinez Manuel Hernandez Cordoba Tandem Sources Using Electrothermal Atomizers Analytical Capabilities and Limitations-Heinz Falk Determination of Geographic Origin of Agricultural Products by Multivariate Analysis of Trace Element Composition-Robert S Schwartz Le T Hecking Immobilized Alga as a Reagent for Preconcentration in Trace Element Atomic Absorption Spectrometry-Hayat A M Elmahadi.Gillian M Greenway Determination of Zinc in Human Milk by Electrothermal Atomic Absorption Spectrometry-Josiane Arnaud Alain Favier Josette Alary Direct Determination of Cadmium and Lead in Geological and Plant Materials by Electrothemal Atomic Absorption Spectrometry-Franci Dolingek Janez Stupar Vinko VrEaj Determination of Selenium by Electrothermal Atomic Absorption Spectrometry.Part 1 . Chemical Modifiers-Hana DoEekalova Bohumil DoEekal Josef Komarek Ivan Novotny Combination of Chemical Modifiers and Graphite Tube Pre-treatment to Determine Boron by Electrothermal Atomic Absorption Spectrometry-Milagros Luguera Yolanda Madrid Carmen Camara Effect of the Matrix on the Determination of Some Impurities in Europium(iii) Oxide by Flame and Electrothermal Atomic Absorption Spectrometry-Vera Spevackova Karel Kratzer Ma'ja Cejchanova Sulphur Contamination From Synthetic Materials in the Argon Gas Supply in Inductively Coupled Plasma Atomic Emission Spectrometry-A P M de Win CUMULATIVE AUTHOR INDEX I NTER-LABORATORY NOTE ~ ATOMIC SPECTROMETRY 283R Industrial Analysis Metals Chemicals and Advanced Materials-John Marshall UPDATE John Carroll James S.Crighton 323R References Typeset by Burgess & Son (Abingdon) Ltd (1 Printed in Great Britain by PAGE BRos Page Bros NorwichSTANDARD 7YPE S. 81. Jm JUNIP 7 Potter Street Harlow Circle 001 for further information . Atomic Spectroscopy Group and North East Region of The Royal Society of Chemistry Productivity Enhancement in Atomic Spectroscopy A one day meeting to be held at York University York UK Wednesday February 5,1992 The speakers will include SJ. Haswell M.H. Ramse y C.L.R. Barnard Data Handling Connection Collection and Control G. Hibberd M. Ingham A.N. Eaton J. Marshall The Development of a Continuous Flow Microwave Digestion Method for On-line Sample Preparation Appropriate Precision Matching Analytical Precision Specifications to the Particular Application AA or ICP-Which to Choose? Operational and Quality Control Procedures in a High- ICP-MS-Variations on a Theme Expert Systems for Improving Eficiency in Atomic throughput XRF Laboratory Spectroscopy For further details contact Dr. J. Marshall ICI plc. Wilton Materials Research Centre Room D125 P.O. Box 90 Wilton Middlesbrough Cleveland TS6 8JE UK. Telephone 0642 432029; Fax 0642 437277.

ISSN:0267-9477    

DOI:10.1039/JA99106BX031

出版商:RSC    

年代:1991

数据来源: RSC

摘要:

JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRYy DECEMBER 199 1 VOL. 6 283R ATOMIC SPECTROMETRY UPDATE-INDUSTRIAL ANALYSIS METALS CHEMICALS AND ADVANCED MATERIALS John Marshall* and John Carroll ICI plc Wilton Materials Research Centre P.O. Box 90 Middlesbrough Cleveland TS6 8JE UK James S. Crighton 8P Research Centre Chertsey Road Sunbury on Thames Middlesex TW16 7LN UK Summary of Contents 1 Metals 1 .l. Ferrous Metals and Alloys 1.2. Non-ferrous Metals and Alloys Table 1. Summary of Analyses of Metals 2 Chemicals 2.1. Petroleum and Petroleum Products 2.1.1. Crude oil and fractions 2.1.2. Lubricating oils 2.2. Organic Chemicals and Solvents 2.2.1. Chemicals 2.2.2. Solvents 2.3. Inorganic Chemicals and Acids 2.3.1. Chemicals 2.3.2. Acids 2.4. Nuclear Materials 2.5. Process Analysis and Automation Table 2.Summary of Analyses of Chemicals 3 Advanced Materials 3.1. Polymers and Composites 3.2. Semiconductor Materials 3.3. Glasses Ceramics and Refractories 3.3.1. Glasses 3.3.2. Ceramics and Refractories Table 3. Summary of Analyses of Advanced Materials This Atomic Spectrometry Update is the third to appear under the title of ‘Industrial Analysis’. The structure of the review is the same as that used in previous years. The subject matter covered in this review is so diverse that it is difficult to discern broad themes in application or technique development. However pressures continue to be exerted on industrial laboratories to provide information with greater structural content (both of a chemical and physical nature) while at the same time demands are made for higher sample throughput and improved sensitivity.A wide range of techniques are now available for the direct characterisation of solids allowing the integrity of the sample to be maintained. However the issue of response calibration is central to the debate concerning the study of solid structures and a variety of theoretical and empirical methods have been proposed to obviate such difficulties. The determination of chemical structure has become increasingly important as the advantages of using atomic spectometric techniques for chromatographic detection are realised. In order to satisfy demand for greater sensitivity preconcentration and/or extraction procedures continue to be developed and the use of flow injection for automating such procedures is growing.There are also encouraging signs of the development of atomic spectrometric techniques for process control which should lead to a reduction of the amount of routine analysis required. It remains to be seen whether the instruments developed over many years for laboratory work will evolve to meet this challenge. 1. METALS This section of the review covers the analysis of ferrous and non-ferrous metals and alloys by analytical atomic spectro- metry. A summary of analytical methods for the analysis of metals is given in Table 1. in these areas were related to improvements in sample preparation methodologies rather than in method develop- ment for the analytical techniques in question. This perhaps reflects the necessity of presenting the samples to the instruments in solution form and to some extent to the 1 .l.Ferrous Metals and Alloys maturity of these techniques. Details of these procedures are summarised in Table 1. Both AAS and ICP-OES continue to enjoy widespread use in metallurgical analysis. The majority of abstracts received * Review Co-ordinator to whom correspondence should be addressed. The number of applications describing the use of ICP- MS for both ferrous and nonferrous metals analysis show a marked increase compared with those received in previous years reflecting the increasing acceptance of this technique in the metallurgical field. Development of analytical proce-284R JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY DECEMBER 199 1 VOL. 6 Table 1 SUMMARY OF THE ANALYSES OF METALS Technique; atomization; analyte form* AA;F;L ZAA;ETA,S AA;F;L Element Matrix Ag Copper-based alloys Ag Copper metal Ag Copper alloys Reference 9111330 9 112509 9 1/25 1 9 Sample treatmentlcomments Ag separated from matrix using HPLC Calibration against solid standards 2 g of alloy mixed with 15 ml of 50% HNO and boiled to remove NO and cooled; 2 ml of 1% Hg(NO,) solution were then added to prevent interference from chloride and the resulting solution diluted to 100 ml prior to analysis Samples dissolved in H,SO MgSO employed as a chemical modifier Sample decomposed in a quartz reaction vessel using a mixture of HCl HNO H,SO and H,PO acids Inert sample introduction system employed to prevent high B blanks due to HF attack Indirect method based on the formation and extraction of the Cd(o-phenanthroline),(BF,) complex Study of inter-element effects Micro-hydride generation with 20 p1 of sample and 15 pl of NaBH solution introduced to reaction cup; 8-hydroxyquinoline added to remove interference by nickel and cobalt Bi3+ coprecipitated with iron hydroxide followed by the formation of Cu(NH,),2+; the precipitate was recovered and dissolved in HCl Optimization of continuous hydride system for Bi determination based on S/N ratio described 0.1-1 g of sample dissolved in 10 ml of HNO acid ( l + l ) 5mlof2moldm-3KBraddedand solution then diluted to 50 ml; Bi was extracted with 0.05-0.1 mol dm- dodecylamine in CHCl and back extracted from the organic phase with 1-5 ml of 4.4% ammonia solution and 4.4% seignette salt Sample dissolved in HNO excess of HNO expelled by use HCHO and the interference by iron eliminated by the addition of citric acid- triammonium citrate solution Sample heated with mixture of HCl-H,PO then HNO (HF for tungsten steels) and HClO were added and solution was heated at 245 "C until cessation of fuming then diluted dissolution of solid alloy samples prior to AA analysis is described between 2-pyrilideniminobenzohydroxamic acid and iron in MIBK Specific method for monitoring chromium plating and polishing solutions; validity of the method supported by data from 6 years of testing Comparision of solution and solid sampling for determination of Ga in aluminium alloys. Discussion of matrix effects and the use of graphite powder as a chemical modifier Ga was extracted from acidic solutions (pH 0.5-2.0) into xylene by complexation with potassium xanthantes An on-line flow injection procedure for electrolytic Method based on extraction of complex formed No details given in abstract A1 Carbon steel samples AA;ETA,l B Boron-alloyed steel AE;ICP;L B Titanium metal MS;ICP;L B Steel AA;-;L 9014027 91/1541 9 11C16 19 9112575 911C27499 911131 B Iron and cobalt alloys AE;ICP;L Bi Steel- and nickel-based alloys AA;Hy;L Bi Copper powder AA;Hy;L 911137 Bi Low-alloy steels Bi Brasses AE;Hy:L AA;ETA,L 9 111078 9113257 Steel AA;F;L 9 112994 Ca c o Iron and steel AA;F;L 9111 117 AA;-;L AA;FL AA;F;L AA;ETA;S c u Alloy samples 9 112 142 Fe High tensile brass 9 1/708 Fe Chromium plating solutions 9113375 9 1/86 Ga Aluminium alloys Aluminium alloys AE;ICP;L 9113030 Ga Copper-manganese- Ferrosiliconzirconium nickel alloys AE;spark;S 9 1 I894 911320 9 11C 1 727 Ge Hf Hf AE;ICP;L 0.5 g of sample digested in HNO,-HF-H,SO acid mixture and diluted in HC1 prior to analysis 0.5 g of sample spiked with 179Hf and dissolved in HF-H,SO,.The isotopically altered Hf was separated from the matrix by cation-exchange chromatography the solution evaporated out of pure spectral carbon which was then homogenized and pressed into electrodes solutions were employed for calibration Sample dissolved using HF-HNO,. Matrix matched Zirconium metal IDMSspark source;S In Nickel alloy AA;ETA;L 911950JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY DECEMBER 1991 VOL. 6 285R Table 1 SUMMARY OF THE ANALYSES OF METALS-co Technique; atomization; analyte form* AA;ETA,L Element Matrix In Tin alloys Ir Platinum metal K Potassium molybdenum bronze Mn Manganese high-alloy steel P Tungsten metal Pb Aluminium alloys Pb Nickel-based alloys Pb Nickel-based alloys Pb Copper metal Pb Steel Pd Titanium alloys S Steel Si Aluminium-silicon and aluminium-silicon-copper alloys Sn Lead-tin solder leachate Te Cast iron Tl Nickel-based alloys V Steel W Cobalt-titanium intermetallic compound Various (1 0) Platinum and palladium metal AA;F;L EDXRF;-;S AA,F;L AE;ICP;L AA;ETA;S AA,ETA,S AFETA,S PAA,-;S AA;ETA;L AA,F;L 1DMS;thermal ionization$ XRF-iS AA;ETA;L M,ETA,L AF;ETA;S AA;F;L AE;ICP;L AA;ETA;L lntinued Sample treatmentlcomments Tantalum lined graphite tube was used 8-fold improvement in sensitivity over pyrolytic coated tube claimed and improved tolerence to interference effects also reported Ir separated from the matrix by liquid chelating exchanger (RCHOCH,CH,) (R =C,H,,) Identification of K compounds in predominant phases of samples prepared by solid state reactions Matrix matched standards required to avoid interferences due to iron 0.4 g of sample was dissolved in 40% HF-concentrated HNO,. The solution was evaporated and the residue boiled in 2.5 mol dm-3 NaOH.To the solution were added 0.5 mol dm-3 H,BO 4 mol dm-3 acetic acid to mask the tungsten and 5 mol dm-3 HNO followed by treatment with ammonium vanadate and molybdate and the resulting phosphovanadomolybdate complex was extracted on a micro-column using a diol sorbent and eluted with solution (0.7-1 mol dm-9 KOH Graphite cup furnace employed for the direct analysis of solid samples.Standard reference alloys were used as both solid and solution calibration standards Direct analysis of solid samples calibration was achieved by the method of additions using Pb(NO,) standard solution Analysis of single-alloy chips (0.5-2.0 mg) RSD in the range 7-20% reported Samples were irradiated with a 23 MeV proton beam for 1-3 h. The sample was etched using 14 mmol dm-3 HNO and dissolved in 6 mol dm-3 HN03. The solution was then passed through Dowex 1- X8 anion exchanger and sample eluted with 0.5 mol dm-3 H,SO,. Pb was determined from the 803.1 and 88 1 .O keV gamma rays of ZwBi steel dissolved in HN0,-HCl; matrix matched standards were employed for calibration Unalloyed steel was dissolved in HNO and alloyed No details given in abstract S determined in four NIST SRMs. Enriched "S was Sample was fused and the melt homogenized by used as an internal standard stirring under a mixture of molten salts (alkali metal and aluminium chlorides and fluorides) and cast into beads (NH,),HPO solution (0.5 ml) 5% Mg(N0)2 solution (0.1 ml) and 10% HNO solution,(0.2 ml).The resulting solution was diluted to 10 ml prior to analysis. Tungstate impregnated tubes were used for the analysis 5 ml aliquot of leachate treated with 10% Ni employed as chemical modifier Analysis of single-alloy chips (0.5-2.0 mg) RSD in the range 7-20% reported Sodium dodecyl sulphate was added to overcome interference effects of several elements Sample was dissolved in a mixture of HN0,-HF and H,S04 was then added and the solution heated until fuming.Tartaric acid was added to prevent hydrolysis of W. Carbon present due to added tartaric acid was employed as an internal standard studied using various types of graphite tubes and a L'vov platform Influence of matrix on analyte atomization was Reference 9112500 911144 9 112 18 1 911958 9111 10 91187 911419 911 1426 9111578 9 I I2580 9111472 9 1 I826 9111 15 9 112438 9 111 468 9 111 426 9112423 9 11 1 608 9014 146286R JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY DECEMBER 199 1 VOL. 6 Table 1 SUMMARY OF THE ANALYSES OF METALS-continued Element Matrix Various ( 10) Aluminium alloys Various (6) High-purity aluminium Various (3) Copper metal various (2) Various (30) Various (4) Various (4) Various ( 5 ) Various (8) Various ( 5 ) Various (1 2) Nickel -aluminium alloy Tungsten metal Calcium metal Stainless steel Cast iron High-purity tantalum Molten iron Silicon and aluminium alloys Various ( 5 ) Molybdenum metal Various (4) Silver-based alloys Various (6) Zirconium alloys Various (7) Stainless steel Various (4) Alloy steel Various (4) Copper metal Various (1 9) High-purity chromium Various (9) High-purity mercury Technique; atomization; analyte form* Sample treatmentlcomments AE;ICP;L AA;ETA;Sl AA;ETA,L AE;ICPL AE;ICPL AA;F;L XRF;-;S AE;ICP;L AE;ICP;L AE;-;L AE;ICP;L AE;Hy;L AA;FL AE;ICP;L MS;ICP;L AE;ICPL AE;ICP;Hy AE;ICPL ZAA;ETA;L Analytes preconcentrated with chelating ion exchanger for Cd Co Cr Cu Fe Mg Mn Ni Ti and Zn determined in alloys by spark ablation of samples and dispersion in water before introduction into the graphite furnace 0.10- 1 .O g of sample was dissolved in 20 ml of HNO (1 + 1).The pH of the sample was adjusted to 1-2 with NH,OH; Bi Sb and Sn were coprecipitated with MnO by addition ofi(Mn0 and MnZ+ and was dissolved in a mixture of HNO,-H,O and diluted to 50 ml Alloy fused with Na202 and the cooled melt dissolved in 5% HCl A study of spectral interferences in the determination of 30 elements in a tungsten matrix reported The sample was dissolved in HC1 and the analyte elements extracted with sodium dieth y ldithiocarbamate-CHC13 (internal standard) and 8 ml of aqua regia. A 0.25 ml portion of the digest was applied to filter paper which was then dried Three correction methods for the elimination of interference by the iron matrix were employed and the relative merits of each approach compared removed using an anion exchanger analysis of molten iron NaOH and a few drops of H,O,. On cooling the solution was treated with 10 ml of H,O followed by 20 ml of HC1 (1 + l) boiled with several drops of H,02 cooled and diluted to 10 ml with 5% HCl.Finally the solution was diluted 5-fold with 5% HCl Hydride forming elements in higher oxidation states were separated from the matrix by coprecipitation with lanthanum hydroxide. Optimization of analytical conditions and control of interferences were also discussed Sample treated with dilute HCl to separate the matrix by precipitation Zr matrix removed as ZrCl by chlorination using HCl at 330 "C. The residue was dissolved using a mixture of 3 ml of 6 mol dm-3 HCl-0.5 ml of concentrated HN03-0.2 ml of concentrate H,SO Extended range calibration employed for analysis of varying composition.Interferences due to common background polyatomic ions are also discussed Spectral interference of alloying elements on analyte elements was studied Mathematical experimetal design techniques employed for selecting optimum and compromise conditions for generation of As Sb Bi and Sn h ydrides oxidized with HClO or alkaline H202; trace elements were then precipitated and collected on cellulose loaded with indium hydroxide or on cellulose-H yphan Mercury sample vacuum distilled in a silica boat and the residue dissolved in 3 mol dm-3 of HC1 and diluted to 5 ml with H,O Trace elements (Cu Fe Mg Mn Pb and Zn) 0.1 g of sample was heated with 1 ml of ZnC1 I Sample dissolved in a mixture of HN0,-HF matrix Q-switched pulse laser excitation employed for direct 0.25 g of sample was dissolved in 10 ml of 20% Chromium powder was dissolved in HCl and Reference 91116 91145 91184 911129 911184 911375 911427 911982 9111 172 9111 173 9 111479 9 11 1486 9111522 91/1610 9 1 IC 1 732 91/22 18 9112250 9 1 I2464 9 112495JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY DECEMBER 199 1 VOL.6 287R Table 1 SUMMARY OF THE ANALYSES OF METALS-continued Technique; atomization; Element Matrix analyte form* Various Non-ferrous metals 9 9 . . -- and alloys Various (2 1) W AE;ICPL Various Tool steels AE;ICP;L Various (5) High-purity copper MS;ICPL Sample treatmentlcomments Review with 15 references on trace element analysis of non-ferrous metals and alloys by AAS and ICP- OES Study of spectral line interferences in the determination of trace elements in tungsten metal Closed vessel microwave dissolution for tool steels was studied and its dissolution speed and reliability compared with those of hot-plate dissolution 1 g of sample dissolved in 8 ml of 7 mol dm-3 HNO 10 mg of La solution were added and the resulting solution adjusted to pH 9-10 by addition of 0.3 mol dm-3 NH,.The solution was filtered and the precipitate dissolved in hot HCl and diluted to 20 ml before analysis by ICP-MS *Hy indicates hydride generation and S L G and S1 signify solid liquid gaseous or slurry sample introduction. Other abbreviations are listed elsewhere. Reference 91/3148 9 1/3192 91/3429 90/4 167 dures for the determination of various elements in steel samples at the low- to sub-ppm level have been reported (9 l/C2804).Polyatomic ion interferences caused by the iron matrix were discussed and detection limits given. Determination of trace elements in three different types of stainless steel by ICP-MS were presented. The extended dynamic range of the technique (20 ng 1-'-20 mg 1-l) was demonstrated and interference by common polyatomic ions discussed (91lC1732). Major and minor elemental constitu- ents were determined in steels following sample dissolution in HCl-HN03 which was evaporated to dryness and the residue dissolved in HN03 prior to analysis. Adoption of this sample preparation procedure was claimed to reduce polyatomic ion interferences.Memory effects due to the iron matrix have also been studied (91K1643). The interference of polyatomic ions as a function of acid dissolution procedure has been investigated (9 11C1723). The effect of polyatomic ions containing F on ICP-MS spectra resulting from the dissolution of alloy steels by HF was reported. The ability to analyse metal samples directly continues to be of great interest and research to achieve this aim is being pursued in most areas of atomic spectrometry. A simple and rapid method for the determination of trace elements in steels based on ETAAS employing a spark ablation for sampling has been described (91/45). The procedure in- volved spark induced ablation of metal samples and dispersion of the material in water prior to introduction into the furnace.Stabilized temperature platform furnace conditions were employed and simple aqueous standards were used for calibration. The direct analysis of molten iron by laser emission spectrometry has been evaluated (91/1173). In this study C Mn P S and Si were determined by employing Q-switched pulsed laser excita- tion at 1.06 pm. Analyte emission was measured following the intense continuum emitted after initial irradiation of the sample. The analysis was not affected by fluctuations of the surface level tilt angle or temperature of the molten iron. The molten iron was analysed continuously at a skimmer of the blast furnace. A review of alternative methods of sample introduction to ICP-OES for metals analyses discussed sampling techniques which avoid disso- lution of the sample prior to analysis (91K2783). Grinding or electrodispersion procedures were employed to provide suspensions of metallic particulates which could be directly introduced into the ICP. However such methods were found to be limited by the fact that the particle size must be in the pm range to ensure efficient atomization of the sample.When the metal was used as an electrode in pure water the electrically dispersed particles were in the sub-pm range. Consequently results obtained using this sample preparation technique were found to be more reliable than those produced by grinding. Other procedures suggested for solid sampling involved direct ablation of the metal. Spark sources may be used for this purpose but these do not provide any spatial information.However laser ablation permits a scan of the surface which provides local informa- tion. The influence of laser characteristics on crater shape the amount of material ablated the size of the particles produced and the type of plasma formed above the surface of the material were discussed in this overview (91K2783). Analysis of low-alloy and stainless steels using spark ablation-ICP-OES has been reported (9 1 /46 1 ). Eleven ele- ments in low-alloy steel were determined. Samples were eroded by a controlled spark and the resulting metal aerosol introduced to the ICP. The precision and accuracy of the analysis was investigated by determination of certified standards. In another application this technique was used for the analysis of free-cutting steels (91/2974).The samples were etched using HCl to remove non-conductive inclusions thus rendering the surface sufficiently conduct- ing to support the spark discharge. Results obtained compared favourably with analysis of the same samples after dissolution. A new technique was reported for normalizing laser power fluctuations in laser ablation plasma AES (9 112373). The technique involves measuring light loss caused by scattering of the ablated material as it flows through a specially designed cell. The variation in absorbance was used to correct for variations in the amount of ablated material. This approach was compared with conventional internal standardization employing a matrix element as internal standard. Three excitation sources for AES namely the Ar ICP Ar MIP and He MIP coupled with laser ablation were compared.The over-all performance was reported to be best for the Ar ICP although in some cases the lower background produced by the MIP produced better results. The spectra were collected with a photodiode-based spectrometer designed for simultaneous multichannel de- tection. This allowed acquisition and subsequent back- ground correction of transient signals produced during ablation. The ability of this detection system to deal with288R JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY DECEMBER 1991 VOL. 6 complex spectra produced from cast iron was discussed. The role of internal standardization in AE analysis using laser-produced micro-plasmas has been studied (9013998). Temperature changes were found to occur in the plasma as a result of the variation in the amount or composition of laser ablated material introduced.Thus an internal stan- dard was employed to compensate for changes in signal intensity due to this temperature variation. Iron-chromium alloy was used as the test material. Results which were independent of the plasma temperature and the ablation characteristics were reported for the major components (Cr and Fe). However for elements with varying vaporization rates such as Cu and Zn it was found necessary to select an appropriate measurement time after the initial laser pulse to ensure complete atomization of the sample in order to produce satisfactory data. The application of a non-uniform magnetic field to stabilize a d.c. arc prior to introduction of a laser ablation sample introduction has been reported (9 1/3058).Limits of detection were improved by factors of 3-6 compared with the unstabilized arc for the analysis of steel samples. The & of glow discharge sources for direct analysis of metals cdntinues to generate great interest. Considerable research effirt is currently being expended to investigate glow dzscharge processes with a view to translating this knowl- edge into improvements in the design of instrumentation and analytical methodology. The performance character- istics of a jet-assisted glow discharge lamp for use in emission spectroscopy have been described (9 1/2845). A conventional Grimm lamp was modified to produce jet- assisted sputtering by drilling jet channels (0.2 and 0.5 mm) in the restrictor and reversing the gas flow through the lamp.Using this system ablation rates were increased up to a factor of 4 compared with conventional lamp designs. The kinetics of sputtering of pure metals and alloys has been investigated (911C1655). The sputtering rate of pure metals and alloys and pressed powders were calculated and the specimens examined by electron microscopy. The sputtering kinetics were shown to be dependent not only on the sample composition but also on the type of microstruc- ture exhibited by the sample. The effect of a supplementary microwave discharge on excitation conditions in a Grimm discharge has also been investigated (9 11C2789). A dual-cathode glow discharge lamp was used in the sputter modulation mode for the determination of Cr and Mn in steel (9113069). Calibration was achieved by the use of iron-manganese and iron-chromium binary alloy stan- dards and was linear to 3.36Oh for Cr and 2.14Oh for Mn. Results obtained showed good agreement for certified reference standards.A novel hollow cathode glow discharge system employing laser ablation sampling has been de- scribed (9013973). A Q-switched Nd:YAG laser was used to ablate sample material which was introduced into the discharge by means of an Ar gas flow. A photodiode array detector was used to acquire spectral data and spectral intensity profiles of atomic lines in the cathode bore. Optimization of operating parameters such as lamp fill pressure flow rate of Ar gas and discharge current was studied. Laser ablation has also been investigated as a means of sample introduction of metals for ICP-MS.The possibility of using this technique for the determination of elements in steel from ppm to percent. levels using a single analytical method was investigated (911C1642). The accuracy of the method was determined using a variety of steel reference standards. A review of laser ablation ICP-OES as a means of analysing solid samples for a variety of metals and alloys has been published (9 113404). X-ray fluorescence spectrometry remains a widely em- ployed technique within the iron and steel industry and developments in instrumentation and methodology con- tinue to be reported. A field-portable microprocessor- controlled X-ray analyser for rapid alloy identification has been described (9 113496).The radioisotope analyser em- ployed modified Lucus-Tooth-Price intensity corrections for quantitative multi-element analysis. The performance of the instrument was demonstrated for the determination of S in carbon steels and Ni and Ti in stainless steels. An on- line XRF spectrometer for the determination of Ni and Zn in plating bath solutions employed in the electroplating of sheet steel for the car industry has been reported (9 1/3496). The analyser consists of an energy-dispersive XRF spectro- meter and an associated liquid sampling system. Plating process solution was continuously supplied to the spectro- meter. The analyser employed an energy discrimination method utilizing filters. The instrument was reported to have carried out fully automated analyses with good performance over a 9 year period. The use of XRF spectrometry as control analysis in the melting of alloy steels has also been outlined (911428).1.2. Non-ferrous Metals and Alloys As in previous reviews the bulk of the abstracts received concerned the analysis of aluminium and copper metals and alloys. However an increase in the number of abstracts relating to the determination of nickel-based alloys pure transition metals and precious metals was noted. A review on the trace element analysis of non-ferrous metals and alloys by AAS and ICP-OES has been published (9 113 148). The direct determination of Pb in solid aluminium alloy samples by ETAAS has been reported (91/87). Certified aluminium alloys were employed as solid standards. Sam- ple and standards were introduced into a pyrolytic graphite coated graphite cup atomizer.Relative standard deviation values obtained for standards were of the order of 5-6Oh and limits of detection based on 100 mg sample sizes were in the pg g-l range. The same workers reported the use of this system for the direct determination of Ga in aluminium alloys. The use of graphite powder as a chemical modifier was discussed (9 1/86). Inductively coupled plasma OES was also employed for the determination of Ga in aluminium alloys after solvent extraction of the analyte with potas- sium xanthates. Results produced were in good agreement with reference values (9 113030). A method for preconcen- tration of trace elements from aluminium alloys prior to determination by ICP-OES has been described.A chelating ion-exchange resin was employed to separate the elements of interest from the aluminium matrix. Recoveries were 100% for most of the elements studied and the accuracy of the method was determined by reference to ALCAN and NIST reference materials. The preconcentration method can be run in both batch or flow injection mode (91116). In another application B was determined in aluminium by ICP-OES after autoclave dissolution of the sample with hydrochloric acid (9 113259). Other applications of ICP- OES reported included the determination of trace REEs in Si-A1 alloys (91/1479) Ni and Ru in Ni-A1 powders (9 1 / 1 129) and the quantification of main components in A1 bronzes (9111484). In a study of the eflect of sample surface integrity on XRF analysis of A1 alloys 11 surface preparation techniques were evaluated. The technique that caused the most damage and lowest surface integrity was high speed lathe turning under dry conditions.Diamond ultra-turning and diamond micro-milling under lubricated conditions caused the least damage. The effective thickness of the specimen layer necessary to measure analyte-line radiation was shown to be dependent on the analyte atomic number and ranged from a few to several hundred micrometres (9 1/50). Other XRF applications included the determination of Si in Si-A1JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY DECEMBER 1991 VOL. 6 289R alloys (91/1156) and the detection of Cr and Mn in aluminium wires and sheets (91/3 139). The production and certification of reference standard material for the analysis of aluminium has been documented (9 1/1288).The analysis of copper and its alloys continues to generate applications for atomic spectrometric techniques. A series of papers concerning the determination of trace elements in a high-purity copper cathode Cu-Cath-1 has been published by the British Standards Institute. Part 1 (91/3112) consi- dered the sample preparation and subsequent AAS determi- nation of Cr Co Fe Ni and Zn. Part 2 (9 1/3 1 12) outlined methods for the determination of Cr Co Fe Ni and Zn by discrete volume-nebulization AAS. In another application FI methodology was applied to the determination of Se in copper metal by hydride generation AAS. Aflow injection manifold incorporating a mini-cation exchange resin was employed for continuous matrix isolation to ensure removal of interfering elements prior to analysis.The developed system was claimed to allow the routine determination of Se at ppb concentrations in the presence of copper matrix levels of 1000 ppm. Inductively coupled plasma MS has also been applied to the analysis of copper metal and alloys. The technique was applied to the analysis of high-purity copper (911C2066). In this method the matrix was removed by electrodeposition onto a Pt cathode. This pre-treatment reduced the level of copper in the sample to below 10 ppm. The electrode potential was set to the point where only Au Ag Bi Cu Hg and Pt were electroplated on the cathode. Losses of analyte elements from the solution other than those mentioned above were reported to be negligible.In order to improve precision and accuracy isotope dilution calibration was employed with spiked isotopes added prior to the separa- tions. The optimized separation procedure and limits of detection obtained together with results for the analysis of NIST reference materials were reported. The determination of trace amounts of As Bi Pb Sb and Sn in high-purity copper by ICP-MS has also been investigated (90/4167). The analyte elements of interest were coprecipitated with La and the precipitate was then dissolved in hot nitric acid and diluted prior to analysis. The remaining applications for copper and copper alloy analyses are documented in Table 1. A number of applications were described in connection with the analysis of precious metals and associated alloys.A comprehensive review discussing the development of selec- tive extractives for precious metals and their application in analytical chemistry has been published (90/400 1). The selectivity efficiency and mechanism of extraction and re- extraction were considered with respect to the effects of substituents attached to the metal binding groups. Enrich- ment of trace amounts of Au Ag Pd and Pt metals by a precipitate floatation has also been described (90/40 1 5). A number of abstracts were received which were devoted to the analysis of silver metal. A direct method for the determination of Au Pd and Pt in fine silver using ETAAS with solid sampling was evaluated (9 K2007). Two methods of solid sampling were considered.The first method involved in situ dissolution of a solid sample by addition of 25% nitric acid in a cup-in-tube atomizer. A high gas flow was required to remove matrix components from the furnace volume during the atomization stage. The second method involved dissolution of the silver sample in nitric acid and agitation of the solution to suspend undissolved elements present in particulate form. In each case calibration was achieved using aqueous standards containing a matching amount of dissolved silver. Results for both procedures were compared with a third method in which the analyte elements in question were extracted from the matrix prior to analysis. A method for the determina- tion of 28 impurity elements in high-purity silver by AES was also described (91/3336).Finally other applications which may be of interest included the determination of trace metals in gold by laser ablation ICP-MS (9 1/C1630) the separation and determi- nation by AAS of trace elements in high-purity platinum and palladium materials (9 1/455) a separation method for trace elements from high-purity rhodium and iridium (9 1/459) and the determination of metallic impurities in platinum and palladium by ETAAS (90/4 146). 2. CHEMICALS This part of the review covers industrial applications of atomic spectrometry to the analysis of a wide variety of materials loosely referred to as ‘chemicals’. Some natural products such as petroleum are included where there is clear synergy with the products produced. The structure of the review is therefore generally similar to that of previous years (see J.Anal. At. Spectrom. 1990 5 323R). One notable exception is that catalysts are now covered in section 3 (Advanced Materials) in view of the similarity of analytical techniques with those used for characterization of refractories (often used as catalyst supports). A summary of publications over the review period relating to analysis of chemicals is given in Table 2. 2.1. Petroleum and Petroleum Products A summary of papers received during the review period which dealt with applications of atomic spectrometry within the petroleum industry is given in Table 2. A general review (472 references) of methods for determination of trace metals in petroleum and related products has been pub- lished by Kaegler (9 1 /345 1 ).2.1.1. Crude oil and fractions The distribution of biomarkers (sterane and triterpane) and sulphur heterocycles (dibenzothiophenes) as determined for example by GC-MS has traditionally been used to characterize crude oils for exploratory and environmental purposes. However it is increasingly being realized that valuable information may also be contained within the trace element constituents of the oil. Price et al. (91lC1645) have shown that trace elements determined using ICP-MS provided a fingerprint which could clearly distinguish between eight North Sea crudes even though the fields were geologically very similar. Changes to the fingerprint during initial stages of weathering were also studied. In a separate study concentration ratios of V:Ni V:Cu Ni:Cu and some composite indices determined using XRF were found to offer good geochemical markers for Miocene and Lower Cretaceous crude oils (9 1/1387). Further information can be obtained if the chemical form of the trace elements in the crude oil can be determined.Zaki et al. (91/21) have used AAS to determine trace elements in heavy distillates and crude oil after extraction with DMF to establish the porphyrin (extract) and nonporphyrin (residue) fractions. A290R JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY DECEMBER 1991 VOL. 6 Table 2 SUMMARY OF ANALYSES OF CHEMICALS Technique; atomization; analyte form* Sample treatmentlcomments Reference 911373 Element Matrix PETROLEUM AND PETROLEUM PRODUCTS- A1 Lubricating oil AA;ETA;L Sample (5-10 g) ashed in nickel crucible and then fused with 1.5 g of NaOH and 0.5 g of Na,O at 380 "C for 10-1 5 min. Cooled melt dissolved and diluted to 25 ml with 5% HNO,.(Recovery 94- 1 12%) Study of effects of heating rate and maximum temperature on redistribution of As Hg and Se between shale oil retort water and offgas of a 6 kg bench scale retort Application of fundamental parameter software to on- line XRF analysis Flow injection AAS analysis of emulsions of lubricating oils Study of effect of viscosity index (VI) improvers [styrene-isoprene styrene-butadiene poly(alkylmethacry1ate) and ethylene-propylene] on Ca response methods for determination of C1 in crankcase oils hydraulic and metalworking oils fuel oils and oil fuel blends with used oils determination of Fe in complex organic mixtures using FAAS and ETAAS.Use of ETAAS after dilution in IBMK is recommended approach Samples diluted with xylene and analysed using ETAAS. (Concentration range 0.000 18-0.0023% m m As for As Interlaboratory comparison of XRF with chemical Comparison of sample treatment procedures for Quantification of Hg in various hydrocarbon mixtures using ETV-ICP-MS. Decreased recovery reported when at least 14 carbon atoms present in the compound FI into petroleum spirit followed by aspiration into a flame photometer. (Concentrations up to 20 ppm) Common gasoline additive (methylcyclopentadieny1)manganese tricarbonyl is determined down to 0.6 ppm using GC with flame photometric detection porcelain crucible until sulphopolymer obtained. Latter is then calcined at 850 "C for 7 min prior to analysis.(LOD 0.01% m/m) Samples diluted with solvent and analysed using ETAAS. Calibrated using standard additions As for Br Determination of alkyllead compounds in environmental samples using ICP-MS Gasoline and water emulsified using surfactant (Tween 60) and introduced directly to flame using ultrasonic nebulizer Petroleum product mixed with H,SO (1 + 1) in Direct analysis using FAAS with no fuel gas Fuel oil (0.8-1 g) and 4-fold by mass paraffin (m.p. 60-62°C) melted thoroughly mixed and moulded onto a disc for analysis using WDXRF. (Concentration range 20 ppm to 4% mlm) SEM with energy dispersive X-ray (EDX) analysis used to study the influence of elemental S and thiols on the corrosion of Cu strips in ASTM D- 130 test British Standard (BSI) for determination of S in petroleum products using ED-XRF with 55Fe source.(Concentration range 0.0 1-5 % mlm) 9 11C 1807 9113452 As Shale oil retort samples AEMIP,G XRF NAA;L S 911124 XRF-iL AA;FL AA;F;L 911143 9112590 9113575 Br Gasoline Ca Lubricating oils Ca Lubricating oils c1 Used oil and fuel oil XRF-;L 911351 1 Fe Petroleum and products AA;F or ETA,L 9 1/3 135 Fe Petroleum and products AA;ETA;L 9113545 911124 9 11296 1 Hg Shale oil retort samples AE;MIP;G AA;F;G Crude oil and naphtha MS;ICPL XRF NAA;L,S K Gasoline and lubricating oils AE;FL Mn Gasoline additives AE;FL 91/1500 9112458 N Petroleum products AE;-;S 9 111 292 Ni Petroleum products AA;ETA,L 911C565 XRF;-;L M S; I CP; L 91J143 911C557 Pb Pb Gasoline Alkyllead Gasoline AA;FL 9 1 I3468 Pb Pb S Gasoline Fuel oil AA;F;L XRF;-;S 9113558 9 1 /426 Copper Hydrocarbons SEM-EDX;S XRF-;LJOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY DECEMBER 1991 VOL.6 291R Table 2 SUMMARY OF ANALYSES OF CHEMICALS-continued Element Matrix Se Shale oil retort samples Si Lubricating oil V Petroleum coke V Petroleum products V Petroleum coke Zn Lubricating oils Various ( 5 ) Crude oil distillates Various Lubricating oil (additive elements) Various ( 15) Lubricating oil Various (7) Petroleum products Technique; atomization; analyte form* AE;MIP;G AA;ETA;L XRF NAA;L S XRF-$5 AA;ETA;L AA; ETA L XRF-;S AA;F;L AA;F;L XRF-;L XRF-;L AE;MIP;G Various (4) Lubricating oils AA;FL Various (1 3) Lubricating oils and additives AE;ICP;L Various Crude oil and heavy residues AA;FL AA ETA; L Various (7) Crude oil XRF-;L Various Crude oil MS;ICP;L Various (8) Oil products AE;ICP;L Various Various (wear metals) Various (wear metals) Various Various Crude oil and naphtha Lubricating and hydraulic oils Lubricating oils Hydrocracker feed Oils AE;MIP;G AE;MIP;L AE;arc;L AF1CP;L AE or MS;ICP;L ORGANIC CHEMICALS AND SOLVENTS- As Organic arsonium cations AA;F;G Sample treatmentlcomments As for As Oil diluted with IBMK and analysed directly using Radioisotope XRF analysis without standards As for Ni Acid extraction of V from petroleum coke samples using microwave heating for 15 min.XRF analysis of extracted solids confirmed total extraction of V from samples ETAAS. (Recovery 92-106%) As for Ca Determination of distribution of Cu Fe Na Ni and V between various fractions of heavy distillates using direct mineralization dilution with organic solvent and solvent extraction (DMF) line XRF analysis Application of fundamental parameter software to on- Sample ( 5 g) of ultrasonically homogenized oil placed in 40 mm diameter cup with 2.5 pm Mylar window.Measured using Philips PW 1480 with He atmosphere and Rh side window tube. (Limits of detection 0.2-3.3 ppm) products. LODs for C S 'H 2H C1 N and 0 are 1 2 4 4 40 50 and 120 pg s- * respectively. Dynamic ranges are > 5 x lo3 Dry ashing in the presence of a porous inert material (silica gel) to reduce loss of analyte by volatilization or sputtering. Tested for Cr Fe Mg and Pb but not appropriate for the last element Samples ashed and then digested with HN03 and HZO2. RSDs were 2.2-12.8% for additives and 3.9-8.1% and 2.5-12.0% for fresh and used lubricating oils respectively Review on determination of metals in crude oil and heavy residues using FAAS and ETAAS XRF used to determine Ca Cr Cu Fe Mg Ni and V in 10 Middle Eastern crude oils.Element ratios and indices shown to provide good geochemical markers. (Concentrations 0.2-36 ppm) North Sea crudes diluted with solvent and analysed using ICP-MS. Measured metal concentration fingerprints allowed clear discrimination of the eight crudes studied against aqueous standards using ICP-OES. LODs for Al Cr Cu Fe Mg Ni Pb and S ranged from 0.003 to 0.1 ppm Advanced data processing algorithm for interference correction in GC-AES analyses. Applicable down to ppb levels Sample introduction system consisted of an ultrasonic nebulizer heated spray chamber condenser and H2S0 absorption cell Electrode configuration and sample delivery modified to improve efficiency of wear particle detection in lubricants Comparison of results obtained by direct analysis in organic solution with those after mineralization New high pressure hydraulic nebulization system permitting direct analysis of undiluted oils Multi-element GC-AES analysis of petroleum Oil samples formed into emulsions and analysed Determination of arsenobetaine arsenocholine and tetramethylarsonium cations by HPLC-FAAS using thermochemical hydride generation.(LODs 13.3 14.5 and 7.6 ng respectively) Reference 911124 911373 911333 91lC565 9 1 I907 9113575 91121 911143 9 11223 911473 911828 91/963 9111 126 9111387 IC 1645 IC 1749 lC1884 9 1 x 2 15 1 9112573 9 1 lC2767 91lC2786 9 llC2805 911157292R JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY DECEMBER 199 1 VOL.6 Table 2 SUMMARY OF ANALYSES OF CHEMICALS-continued Element Matrix Cd Organic acid solutions (Cd) Chlorodiazepoxide C1 (Ag) Organosilicon compounds c o Organic chelates 0) Vitamin B,2 (CU) Aliphatic amines (CU) Chlorhexidine 2H GC eluents Mg Organic acid solutions Sn Alkyltin compounds Yb Organic complexes Yb (Sulphosalicylic acid) Technique; atomization; analyte form* Sample treatmentlcomments AA;F;L AE;MIP;G AE;ICP;L AA;ETA;L AA;F;L AA;F;L Zn Organic acid solutions AE;ICP;L Zn Mercaptomethyl- AA,F;L (Zn) Chlorodiazepoxide AA;F;L prop ylproline Zn Pharmaceutical preparations AA;F;L Various Solvents AE;ICP;L Various (14) Cd alkyl compounds AE;-;S Various Volatile solvents AE;ICP;L Various ( 5 ) Solvents Various Solvents Various Solvents Various Emulsified solvents AE;DCP;L MS;ICP;L AE;ICP;L AA;FL AE;ICP;L AA;F;L Study of effects of organic acids on solvent introduction and plasma excitation conditions Indirect FAAS determination of chlorodiazepoxide in pharmaceutical preparations by reduction on Cd or Zn columns.(Concentrations 1-25 pg ml-l) CH30Na-CH30H and Cl preconcentrated by precipitation as AgCl. C1 determined indirectly by measurement of Ag using FAAS. (Concentrations in the ppm range) introduction to FAAS. Complex with trifluoroacetylacetone gave highest sensitivity Indirect determination of vitamin B in pharmaceuticals using FAAS. LOD is 0.2 pg ml-I and RSD (8% at 10 pg ml-1 formation of dithiocarbamate derivatives followed by extraction in chloroform of the Cu" chelates.Cu is measured by FAAS after mineralization AA;FL Organosilicon compounds decomposed with AA;F;G Comparison of chelates for direct vapour-phase AA;FL AA;F;L Indirect determination of aliphatic amines by (HNO3) pharmaceutical preparations using FI-AAS. Sample injected into ammoniacal Cu solution precipitate retained on filter then eluted with HNO Determination of deuterium in GC eluents using atmospheric pressure MIP emission detector with tangential flow torch. (RSD for 2H:1H ratio=2%) Indirect determination of chlorhexidine in As for Cd Several organopalladium complexes tested as chemical modifiers for determination of alkyltin compounds in ethyl acetate-hexane (3 + 2 vlv).20-fold enhancement obtained compounds which can form stable complexes with Yb and their use to depress interferences from other rare earth elements and inorganic acids Sensitivity of Yb increased 23.6 times in presence of sulphosalicylic acid and NaCl and interferences from acids and rare earth elements greatly depressed Sensitivity enhancement effects of organic As for Cd Indirect determination as for Cd Sample (0.5 g) digested with 5 ml HCl evaporated to about 0.5 ml then made up to 10 ml in 10% HC1. Analysed using air-C,H flame at 21 3.9 nm Samples dissolved in mixed solvent containing H20 HCl EtOH and 2-butanone (air-C2H2 flame) Electronic device for control of solvent plasma load using Peltier cooling Samples decomposed to CdO and mixed with NaC1 graphite powder and Floroplast.Some impurities preconcentrated on partially precipitated hydroxide. [LODs 1 x 10-4-3 x lop6% mlm (3 x 10-6-1 x m/m with enrichment] desolvation to improve plasma stability and limits of detection. (LODs ranged from 0.2 pg 1-I for Fe to 5 pg 1-I for Pb) Optimization of FI system. (LODs in ng ml-I B 21; Cu 14; Mo 28; W 120; and Zn 20) Effect of organic solvents on polyatomic ion interferences Comparison of desolvation effects with aqueous and organic sample introduction Study of effect of organic solvents and non-ionic surfactants on profiles of Ca Cr Cu and Fe in C,H2-air flame using dual nebulization system Use of ultrasonic nebulization with cryogenic Reference 9013965 91112 9113417 9117 9 11937 9 11709 9112189 911862 9013965 9113348 911186 9113001 9013965 91112 911377 9113392 9013976 9013991 9013995 9014006 911852 911871 9 1 I942JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY DECEMBER 199 1 VOL.6 293R Table 2 SUMMARY OF ANALYSES OF CHEMICALS-continued Element Matrix Various Solvents Various Solvents Various Diethyl ether Various Organic chemicals Various (23) Organic chemicals Various Ethanol Technique; atomization; analyte form* Sample treatmentlcomments AA;F;L AA;F;L MS;ICP;L AE;MIP;G AE or MS;ICP or DCP;L AE;MIPG AE or AFICP;L Various (1 2) IBMK AE;ICPL Various (12) IBMK AE;ICP;L Various Organic compounds AA;FL Various Aqueous-organic mixtures AE;ICP;L Various (6) Alcohol solutions AE;ICP;L Various Organic solutions Various (1 1) Penicillin G Various Organic solutions Various (7) Organic solvents Various (9) Tetramethyltin AE;ICP;L AE;ICP;L AE;ICP;L AE;ICP;L AE;-;S Various Organic solvents and AE;ICP;L volatile compounds Various Pharmaceuticals Various (7) Pharmaceuticals INORGANIC CHEMICALS AND ACIDS- A1 Concentrated salt solutions XRF;-;- AA;-;- AE;ICP;L Mixture of butanol and ethyl acetate proposed as alternative to IBMK for extraction of metal complexes for AAS Ionization suppression for organic solutions by on- line addition of KC1 in aqueous solution using a branched capillary Optimization of plasma conditions for analysis of diethyl ether using ICP-MS and comparison of sample introduction techniques Review of plasma spectrometric detectors for GC and HPLC Review of recent GC-AES applications to petroleum environmental pesticide and aroma samples. Accuracies of 5% or better claimed for quantification using compound independent calibration Study of effect of ethanol addition to aqueous solutions in ICP-OES and ICP-AFS.REE detection limits improved in ICP-OES and tendency to form refactory oxides reduced in ICP- AFS Effect of operating parameters on S/B of analytical lines and excitation temperature for analysis of IBMK in an air-Ar ICP. 50% and 10% air optimum for atomic and ionic lines respectively As above but study of carbon molecular bands. 50% air found optimum for suppression of bands Review of indirect procedures for determination of organic compounds using AAS Effect of cellosolve and ethanol concentrations in aqueous solutions on intensities and backgrounds of ICP-OES lines solutions on S/B of atom and ion lines of Cu Mn Ni Pb Sr and Zn.Increase of outer gas flow can reduce plasma changes conventional Ar plasma for analysis of organic solutions. Suppression of molecular bands at 50% air mixture Direct analysis of sample solutions (1 5% d v ) against matrix matched standards prepared from high- purity penicillin. (ppb limits of detection) thermospray nebulizer from C CN N and NO powder evaporated to dryness and 0.5% NaCl added. Residue treated with 0.5 ml of HCl dried and analysed using AES (Al Ca Cu Fe Mg Mn Pb Te and Zn) Modified direct injection nebulizer for introduction of organic solvents to ICP. Reduced effects of selective volatilization compared with Meinhard nebulizer pharmaceutical analysis various pharmaceuticals using AAS Influence of alcohol concentrations in aqueous Performance of air-Ar ICP compared with Transport efficiency improved (30-40%) using Oxygen added to plasma to reduce band interference Sample (2-6 ml) mixed with 50 mg of graphite Review with 55 references on use of XRF for Determination of Cr Cu Fe Mn Ni Pb and Zn in System for continuous extraction of A1 (complex with cupferron) into xylene phase separation using membrane and analysis of organic phase using ICP-OES.(ppb concentrations) Reference 9 1 /999 91/1463 91/C1646 9 1/C2086 91/C2087 91/C2122 9 l/C2 1 30 9 l/C213 I 9 1/2240 9 1/2408 9 1/C2722 91/C279 1 91/C2840 91/C2876 9 1 /C2907 9 1/C2909 91/3 173 9 1/3282 9 1/3472 91J3473 9 1/C29 13294R JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY DECEMBER 199 1 VOL.6 Table 2 SUMMARY OF ANALYSES OF CHEMICALS-continued Technique; atomization; analyte form* AA;F;L Sample treatmentkomments Reference 9 1 /927 Indirect determination of NH3 by reduction of Ag ions in the presence of Mn". Unconsumed Ag in solution is measured using AAS. (Concentration range 20-200 jg of NH,) Performance of FAAS using N,O-C2H2 for high salt solutions improved using jaw-type burner with large opening and microsampling technique As extracted with solution containing 2% KI and 0.4% SnC1 in 4-methylpentan-2-one (pH 3-4) then back extracted into 0.4 mol dm- HNO,. Determination using ETAAS with Ta coated device in 8-10% H,-Ar. (0.46-3.35 pg ml-I) PH,-camer gas (H or Ar) mixtures used in manufacture of semiconductor components Sample mixed with concentrated HNO 2.5% La solution and 50 ml of HzO heated to 65 "C aqueous NH added and La(OH) containing coprecipitated As filtered off.Precipitate dissolved in HN03 solution and analysed using ETAAS interference from Ca Na and Sr in DCP-OES and FAAS (N,O-C2H2). (Concentration range 1-500 Pug ml-') 9 111490 9 1 /450 Determination of trace amounts of ASH in 91/1339 9 113053 Mg (5 mg ml-I) added to samples to reduce Preconcentration by crystallization from an aqueous salt eutectic solution. (Detection limit 5 x d m ) Battery sawed opened with tweezers and the contents extracted with HCl-HNO (2+ 1) at room temperature for at least 16 h. (RSD 2.1% LOD 0.0001% d m ) Cd extracted from alkaline aluminium chloride using 6 mol dm-' H3P04-2 mol dmP3 KI and IBMK.Determination using FAAS with air-C,H flame added to mask interference from Fe. (Detection limit 1 ppb) Study of changes in Co K/?/Ka intensity ratios with calcination of CoCO at different temperatures. Large change in ratio possibly due to effect of molecular structure Comparison of results obtained using spectral peak fitting programme with traditional approach Calcium removed from solution by extraction with a mixture of ammonium di(2-ethylhexyl) dithiophosphate (0.5 rnol dm-9 and tributyl phosphate (2 rnol dm-9. Cs determined in aqueous phase after removal of NH,C1 by sublimation 5 ml of 2% APDC added to 10 ml of sample. Cu complex extracted into 10 ml of IBMK and determined using FAAS. (LOD 0.01 pg ml-l) Cu extracted from aqueous solution (pH 4.5) using 5 x 10-3 rnol dm- pivaloyltrifluoroacetonate.(Concentration range 0.0 1-0.0037% m/m) Round robin analysis of N 10-P 34Oh liquid fertilizer. (Concentration range 0.05-O.S0h) Determination of Cu in saline to hypersaline waters containing high Fe concentrations by coprecipitation with FeO(0H). Also applicable for Al Mn and Ni determinations Inteiferences from mineral acids compensated and precision improved using Myers-Tracy internal standardization procedure calibration using standard additions On-line extraction into IBMK using 0.2% APDC. KI 5 ml of 0.5 rnol dm- ammonium citrate solution and Analysis carried out in 2 rnol dm- HCI with As for Cu Element Matrix (45) Ammonia A1 High salt solutions AA;F;L As Phosphoric acid AA;ETA;L As Phosphine AS Copper sulphate electrolytes and electrolytic copper AA;ETA;L Ba Formation water AE;DCP;L AA;F;L 9112775 Caesium iodide Dry batteries XRF-;S 9113027 9014 1 73 Br Cd AA;FL Aluminium chloride Fertilizer Cobalt carbonate AA;FL AA;FL XRF;-;S 9 1/33 I 7 9 113583 90/4 157 Cd Cd c o Cr c s Liquid fertilizer Calcium chloride brines AE;ICP;L AA;FL 9112791 9111366 c u Sodium chloride AA;F;L 9 11948 c u Cobalt oxide AA;F;L 9 11969 9111290 9 112635 c u Liquid fertilizer cu Fe rich brines AA;F;L AA;F;L AE; ICP; L 9 113208 cu Mineral acids AA;F;L AA;FL 9113558 9113538 c u Barium titanate Fe Barium titananteJOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY DECEMBER 199 1 VOL.6 295R Table 2 SUMMARY OF ANALYSES OF CHEMICALS-continued Technique; atomization; analyte form* AA;ETA;L Element Ge Hg Hg I (Hg) Mg Mn Mo P Pb Pb Pb Pb Pd Pt Matrix Mineral acids Sample treatmentlcomments Palladium nitrate added as chemical modifier.For HCl Ge is extracted with toluene and back extracted with tetramethyl ammonium hydroxide. (LOD 0.1 ng g-l) formation of Hg vapour using KMnO and NaBH,. (RSD 4.3% LOD O.OOOl% d m ) Inorganic Hg compounds reduced to vapour using NaBH or Sn". Mercury trapped on gold coated wall of graphite cuvette and then released electrothermally in AAS. (Concentration range As for Cd but determination of Hg carried out after 5- 100 ppb) Indirect determination of I- by measurement of decrease in Hg emision intensity in cold vapour MIP-OES due to interference effect of I- complexes. (Concentration range 2-100 ng ml-1) Study of distribution of magnesium stearate lubricants on the surface of sodium chloride tablets using imaging and static SIMS As for Cu Round robin analysis of N 10-P 34% liquid fertilizer.(Concentration range 0.005-0.1%) A C1,SiH vapour introduction system is described for use with ICP-OES. Calibration for P established using PH On-line preconcentration on PTFE micro-column of Spheron Oxin 1OOO. Column washed with water and analyte eluted with 1 mol dm-3 HNO directly into graphite tube. (Detection limit 0.1 ng ml-I) Preconcentration by electrodeposition on a W electrode (30 s,-0.6 V versus SCE) followed by insertion in graphite cup for ETAAS analysis. (Concentration range 0.4-50 ng ml-I) As for Cu As for Cd Determination of Pd in ammoniacal-Trilon solutions utilized in the electrodeless coating of metals and alloys.(Concentration range 0.01-10 g 1-I) Thermogravimetric and XRD analyses showed H2PtC16 in ETAAS is broken down to volatile PtC12 before being converted into metallic Pt whereas cis-Pt(NH,),Cl is converted into metal in a single step. Could explain why ETAAS response is different for the two compounds As for Cs Sample preparation by membrane coating needs only about one tenth amount of sample compared with conventional pressed tablet. Simultaneous determination of different valancies of S. (Concentration range 0.001-30% d m ) Tandem on-line continuous separation involving reaction with KI to form Sb13 extraction into xylene and then H,Sb vapour generation 5 ml of sample solution treated with 2 ml of H2S04 (1 + 1). Calibration using standard additions Extraction with 0.5 mmol dm- 33- dibromosalicylaldehyde 2- benzothiazoylhydrazone-CHCl solution in the presence of zephiramine at pH 3.8 followed by backextraction into 3.5 mol dm-3 HCl. (Linear up to 300 ng of V) manifold for spectrophotometric determination of Zn.(Concentration range 0.2-60 g 1-I) As for Mo. (Concentration range 0.05-2.0%) As for Cu Application of chemical modification in direct Samples diluted by dialysis prior to injection into FI insertion ICP-OES. Best results obtained using 10 pl spike of 0.25 mol dm-3 NaF to the sample cup Reference 91lC1729 73 14 9 1/90 9 112356 9 113208 9 11 129 1 91/77 90140 12 9 112498 9 112635 9 1/33 17 9 112478 911 1072 Dry batteries M,cold vapour;G 9014 9 112 Mineral acids AA;ETA,G Sea-water and brine AE;MIP;G Sodium chloride tablets SIMS-;S Mineral acids Liquid fertilizer AE;ICPL M,F;L AE;ICPG Trichlorosilane Sodium chloride M,ETA;L Potassium bromide AA;ETA;L Fe rich brines Aluminium chloride Metal coating solutions AA;F;L AA;F;L XRF;-;L H2PtC1 and cis-Pt(NH,),Cl AA;ETA;L Rb S Calcium chloride brines M F L Sulphur sorbents and coal ash XRF-;S 9111366 91/31 77 Sb Zn electrolysis solutions AE;ICP;G 91/C2912 sc V Titanium white sulphate Common salt AE;ICP;L AA;ETA;L 9 11369 91/3479 Zn Hydrometallurgical process streams Spectrophoto- metric;L 911458 Zn Liquid fertilizer Zn Fe rich brines Various Inorganic chemicals M F L M F L AE;ICP;S 9111291 9112635 901395 7296R JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY DECEMBER 199 1 VOL.6 Table 2 SUMMARY OF ANALYSES OF CHEMICALS-continued Technique; atomization; analyte form* AA;F or ETA,L Element Matrix Various (24) Ammonium perrhenate Sample treatmentlcomments Reference 9014008 Ca K Mg Na and Si determined directly in aqueous solution.Other elements (except Mo) determined after separation of dithiocarbamate complexes. Mo extracted with benzoin oxime Determination of Bi Cu and Zn and Cu Fe and Pb in concentrated sodium chloride and ammonium fluoride solutions respectively ml of HNO (1 + 1) for 2 h in sealed bottle (65-70 "C). Fluorides complexed with boric acid prior to ICP-OES determination of Al Ca Fe Mg Mn Na P Si and Ti 2 g sample treated with H20 decomposed with HCl (1 + 1) and diluted to 100 ml. LODs improved using concentric nebulizer and adding methane as reductant (5- 10 ml min-I) Short pre-oxidation using sodium nitrate prevents losses of S by volatilization and of metals into the platinum crucibles during fusion of mineral sulphides preconcentration of Ag Bi Cd Cu Fe Mo Pb Sb and Zn.Best results obtained with HCl- trioctylmethylammonium chloride-0.002 mol dm-3 APDCIIBMK Changes in state of arc plasma followed with Ba Ca Mg and Mn carbonates as functions of composition of carbon powder mixtures and arc current preconcentrated by matrix removal (5- 10 g) at 180 "C in the presence of 50 mg of powdered graphite. (LODs 3 x 10-*-2 x Review of methods for determining trace impurities in S Se and Te Determination of Ba Ca Fe Mg Ni and Si using axially viewed ICP-OES with direct nebulization using concentric tubular device with bell mouth to prevent clogging.(LODs 0.01 0.003 0.04 0.003 0.2 and 0.5 pg ml-l respectively) tetraborate in ratio 100+97+3 and placed in graphite electrode for spectrographic analysis vacuum distillation over carbon collector in Mo glass ampoules. (LODs 2 x 1O-Io- 6 x lo-* % m/m) Comparison of atomic spectrometric methods for determination of trace elements in saturated brines. (Concentration range 1-50 pg 1-I) On-line preconcentration of trace metals by chelating ion exchange Correction for effects of salt concentration on analyte response by measurement of Sc atom to ion line ratios. Eliminates need for matrix matching of standards Review of determination of trace components of sea- water including trace metals inorganic anions and organic compounds and Pb determined using AAS.Hg determined by ashing at 850-900 "C in 02 trapping Hg vapour in an amalgam and then releasing into AAS by heating. (LODs 0.3-5 pg g-]) Determination of Fe Ni Pb and Zn after electrolytic removal of Cu matrix. (RSDs are 1.8-6.9% in the concentration range 0.0001-0.01%) 90140 10 500 mg digested with 2 ml of HF (50% m/m) and 2 9014 1 62 Comparison of extraction systems for Co Cr Cu Fe Mg Mn Ni Pb and V % d m ) Sample mixed with carbon powder and sodium Preconcentration involving matrix removal by Samples digested with hot HN03-HCl and Cd Cr Various (6) Concentrated salt solutions AA,F;L Various ( 10) Coal AEICPL Various (1 1) Lithium carbonate Various ( 5 ) Sulphides Various (9) High-purity Ni salts AF,ICP;L XRF;-;S AA;F;L 911183 911205 9 11237 Various (4) Carbonates AE;arc;S 911288 Various (9) Ammonium hydrogen fluoride AE;arc;S 911341 Various Chalcogens Various (6) Brine Various AE;ICPL 9 11342 911368 Various (1 3) Sb203 Various (19) Boron bromide Various Brine AE;-$ 911416 9 1 I470 AE;arc;S AE or MS;ICP;L 9 1x745 MS;ICP;L AE;ICP;L 91lC777 9 1lC786 Various Brine Various Sea-water and formation water Various Sea-water Various 9 11949 9111009 Various (4) Fertilizers AA;F or ETA L or G Various (4) Copper oxide AA,F;L 9 11 1477JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY DECEMBER 1991 VOL.6 297R Table 2 SUMMARY OF ANALYSES OF CHEMICALS-continued Technique; atomization; analyte form* Element Matrix Sample treatmenthmments De-ionized water added dropwise to weighed sample at low temperature. HNO added and sample heated in microwave oven at low power.HF is then added to complex elements such as Nb Si Ta Ti and W Laser ablation ICP-MS analysis of samples prepared as pressed powders and glass discs. In20 used as internal standard for determination of Ba Fe Mg Mn Sr and Pb dryness and reconstituted in less acidic media. For volatile analytes sample is diluted 10-fold in water. LODs improved using ultrasonic nebulizer ICP-OES analysis of 1-2.5% NaCl solutions using FI Determination of Ag Au Co Cu Fe Pb Pd Pt Sb and Zn in formation waters to provide information on origin and migration history Determination of trace metallic impurities in N2 H HCl NH B,H SiH ASH and PH by flameless AAS For non-volatile elements acid is evaporated to Precision improved and matrix effects reduced in Review of use of XRF in cement plants Review of spectrochemical methods for analysis of high-purity volatile inorganic hydrides halides and organometallic substances Optimization of FI-ICP-OES system.(LODs 0.033-7.6 pg ml-I; RSDs 0.58-2.9%) Determination of Cd Co Cu Fe Mn Ni and Zn in high-purity ammonium and sodium molybdate after extraction into IBMK with 2-(2- benzoxazoly1)cyanoacetaldehyde of mineral acids and some common concomitants during determination of Ca Cd Cu Fe K Li Mg Mn Pb and Zn using ICP-AFS Study of effects of low concentrations ( HCl HNO and HClO.,). Enhancement from HCl suppression from HClO but no significant effect from HN03 composition of mixed carrier ( 5 + 1 AgCl-SrF2). (Detection limits 0.1-50 ppm) Comparison of three techniques (flame with and without preconcentration and ETA) for AAS determination of Cd Cr Cu Ni and Pb in concentrated CaCIJNaCI solutions.ETAAS was best Study of interferences caused by low concentrations A d.c. arc carrier distillation technique with 12% Introduction to use of XRF in fertilizer industry Sample dissolved and Cd Cu Fe Ni and Pb extracted into IBMK using APDC. Al Ca Co Cr Mg and Mn determined in aqueous phase after Zn extracted into CHC1 using trioctylmethylammonium chloride Reference 9 1lC 163 1 9 1 IC 1 637 9 11c 19 12 Various (58) Lithium and lithium hydride AE or MSICPL Various (6) Calcium carbonate Various Mineral acids MS;ICP;S AE;ICPL Various Brine AE;ICP;L :2 128 12555 12624 911 9 9 Various (10) Formation waters AA;ETA;L Various High-purity gases AA;ETA;G Various Cement Various High-purity gases XRF-;S Various 9 112683 9 112689 Various Sodium chloride Various (7) Molybdates AE;ICP;L M F L 9112693 9112704 Various (1 0) Mineral acids AFICPL 9 1 lC2 86 5 Various Acids Various (22) Thorium oxide Various ( 5 ) Concentrated salt solutions AE;ICP;L AE;arc;S M F or ETA,L 9 112980 9113158 9113455 Various Fertilizers Various (1 1) Zinc salts XRF AA;FL 9 113456 9113581 NUCLEAR MATERIAU- B Nuclear materials B Uranium metal or oxide AE;ICP;L AE;arc;S Enhancement of sensitivity of B lines by addition of Sample dissolved in HN03 Mannitol added and He to Ar camer gas in ICP-OES boron separated from matrix by cation exchange.Boron solution evaporated to dryness redissolved in solution containing NaF and Be internal standard and evaporated to dryness on carbon electrode Matrix separation using extraction chromatography with levextrel-TBP resin.Mg(NO,) used as chemical modifier. (Detection limit 1 ppb) 9 1lC548 9 112607 Be U308 M,ETA,L 9112373298R JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY DECEMBER 199 1 VOL. 6 Table 2 SUMMARY OF ANALYSES OF CHEMICALS-continued El emen t Matrix c o Uranium solutions Ga Plutonium Mn Uranium solutions 23up EfAuent Ru Fuel reprocessing solutions Tc Spent fuel reprocessing streams 99TC Effluent U NaCl leaching solutions Various (1 5) Uranium tetrafluoride Various (7) Uranium oxide Various (70) Radioactive materials Various (7) Process plant d u e n t s Various (30) Uranium compounds various Various Various Various Various Various Low-level radioactive waste Low-level radioactive waste Pu recovery streams Nuclear fuels Nuclear materials Pure As Fe or Ni Technique; atomization; analyte form* AE1CP;L XRF;-;L AE;ICP;L MS;ICP;L M;F;L AEICPL MSICPL AE1CP;L AE1CP;L M,F or ETA,L AE or MS1CP;L MS;ICPL AE;ICPL AEICPL or M,ETA,L AE;ICP;L Mycold vapour,G AE;ICP;L AEarc;S AE1CP;L AA;ETA,L MS;ICP;L or S MS;ICP;L Sample treatmentlcomments Least-squares fitting of pure component spectral curves to spectral regions of solutions containing 10 000 mg 1-1 of uranium. (LOD 0.25 mg 1-I) Ascorbic acid added to 6 mol dm-3 HCl solution of plutonium and Ga separated on anionexchange column.Analyte eluted with 0.02 mol dm-' HC1 and Zn added as internal standard. (Concentration range 0.2-1% m/m) As for Co. (LOD 0.05 mg 1-I) Samples acidified and internal standard solution added Direct determination using FAAS with air-C,H flame.(Concentration range 20-80 pg ml-I). Spectrophotometric methods given for lower concentrations Tc separated from other fission products and heavy metals by precipitation of latter in alkaline medium. (RSDs 2.2% at 9 pg ml-I and 4.9% at 0.9 pg ml-I) scintillation counting adsorption on strongly basic AGlX 8 anion- exchange resin. I and Te also determined using ion chromatography and liquid scintillation respectively NH,OH and HN03 and then passed through TBP modified poly(trifluoroviny1 chloride) stationary- phase column. (Concentration range 0.1-1 pg ml-I) evaporated to dryness and 3 ml of 1 mol dm-3 HN03 and 0.5 g of ascorbic acid added. Solutions passed through column of GDX-301 beads pre- treated with trialkylphosphine oxide.(Determination of Cay Cu Cry Fe K Mg and Mn) separation. Other elements determined using ICP- OES after matrix separation. (Concentration range PPm) Determination of various fission activation and nuclear fuel actinides (e.g. I3Cs lZ9I 9s'c and isotopes of N Th and U) in nuclear plant effluents nuclear waste materials and environmental waters. (LODs 10- 100 ppt) Impurities separated from uranium matrix using tri(2ethylhexyl) phosphate coated columns Removal of U and Th using trioctylphosphine oxide extraction. Determination of Ag As Bay Cd Cry Ni Pb and elements associated with waste treatment using ICP-OES and Hg Se and Tl using AAS Determination of contaminants in process streams of low-level waste water treatment plant.Hg determined using cold vapour AAS Determination of impurities in Pu recovery process streams. Samples prepared using ion-exchange membranes and acid matrix matching Comprehensive methods for determination of trace metals in Tho UO PuO (U,h)O graphite (U,Pu)C (Pu-Al) and (U-Al) alloys Methodologies for analysis of nuclear materials using ICP-MS. Includes application of laser ablation for solid samples and coupled ion chromatography for interference removal and speciation products in samples of pure As Fe and Ni. (Concentration range ppm) As for 23Up. Results compared With liquid Uranyl ions separated from excess of NaCl by Sample converted into U0,(N03) using HzO 0.5 g of sample dissolved in 3 ml of HN03 Actinides determined using ICP-MS with no matrix Determination of total impurities and transmutation Reference 911C541 911454 911C541 9 1 IC 1 647 9 112677 9013952 9 1lC 1647 91J1374 911435 911439 911C542 9 1lC544 911C546 911C547 911C550 9 l/C55 1 9 1 I944 9 1lC 1 632 9 1lC 1648JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY DECEMBER 199 1 VOL.6 299R Table 2 SUMMARY OF ANALYSES OF CHEMICALS-continued Element Matrix Various Plutonium Various (4) Environmental samples Various Nuclear fuels (REEs) Various Uranium Various Uranium (REEs) Various (5) Uranium solutions Various Fuel reprocessing liquids AEICPL AEICP;L XRF;-;L XRF;-;L Technique; atomization; analyte form* Sample treatmedcomments Reference MS;ICP;L FI sample introduction (100 pl loop). No matrix 91lC1649 MS;ETA;G 9 1 I2290 separation required Determination of Gd Pu Tc and U using RIMS with three tunable dye lasers pumped by copper vapour laser and time-of-flight mass spectrometer.(Detection limit about 1 x lo7 atoms) Two separation methods used. First based on TBP extraction second involved separation of REEs on alumina column coprecipitation with lanthanum oxalate redissolution and determination using ICP-OES Degradation of detection limits for trace elements in solutions containing high (4%) concentrations of U reduced by Kalman filtering of the spectra obviating the need for chemical separation REEs separated from matrix by adsorption of U on 71 1 anion-exchange resin and further preconcentrated by adsorption on levextrel-PMBP resin. REEs eluted from resin using 1 mol dm-3 HCI. (Limits of detection 0.006-0.07 pg g-I) Direct determination of Dy Er Eu Gd and Sm in uranium solutions using matrix matched standards EDXRF with preliminary selection of energy range of radiation from sample (around Pd Ka line) allows monitoring of Mo Pd Rh Ru and Zr at mg ml-I concentrations AE;ICP;L 9 llC2729 9 llC2885 91/31 30 9113294 9 113401 *Hy indicates hydride generation and S L G and S1 signify solid liquid gaseous or slurry sample introduction respectively.Other abbreviations are listed elsewhere. higher degree of speciation can be achieved through coupling of atomic spectrometry to chromatographic tech- niques. Sullivan (91/C1884) and Firor (91/473) have re- ported application of a commercial GC-MIP-AES system for speciation of trace levels of organometallic compounds in crude oil and non-metallic impurities in naphtha and other petroleum products. The potential benefits of obtain- ing information on the chemical form of elements in petroleum and products particularly at trace levels are clearly very high and so it seems certain that many more applications will be reported in future years as instruments of this type become more widely utilized.Crude oils and naphthas can contain hazardous concen- trations of Hg capable of causing embrittlement of alumi- nium piping and heat-exchange equipment. Electrothermal vaporization ICP-MS has been used to determine soluble and suspended mercurials in petroleum with a limit of detection of around 3 ppb (ng g-*) (91/2961). However decreased recoveries were obtained with compounds containing a larger number of carbon atoms (e.g.14 or more) and so calibration using standard additions was recommended. Similarly the corrosive properties of naphthas are gener- ally governed by their content of S compounds. This is routinely tested by studying the tarnishing of copper strips placed in a naphtha sample for a prescribed time under controlled conditions (ASTM D-130). Scanning electron microscopy with energy dispersive X-ray detection of S has been used to provide a more quantitative assessment of the degree of corrosion on the strips than the subjective visual comparison usually employed (91K1807). The degree of corrosion was found to be independent of the hydrocarbon composition but did depend on the concentration and chemical form of the S compounds.For example the corrosion produced by elemental S was 3.7 times higher than the equivalent concentration of S present as ethylmer- captan and for mercaptans with six carbon atoms the corrosive effect followed the order thiophenob hexane- thiobcyclohexanethiol. Determination of metals in crude oil and heavy residues has been reviewed by Lang et al. (91/1126). Release of heavy metals into the environment can be a serious concern during production and processing of some petroleum products. Olsen et al. (91/124) have used a combination of atomic spectrometric techniques for the measurement of As Hg and Se in the product streams of a bench scale inert gas oil shale retort. Zeeman-effect AAS and MIP-OES were used to monitor the off’s stream and XRF NAA and cold vapour AAS were employed to analyse the raw and spent shales retort water and shale oil.Most of the Hg was found to volatilize into the off’s whereas As and Se preferentially redistributed into the shale oil and retort water. Alkyllead compounds have traditionally been used in anti-knock formulations for gasoline. Several standard (e.g. ASTM) atomic spectrometric methods exist for the determi- nation of total Pb in gasoline using XRF or AAS. However techniques using solution nebulization for sample introduc- tion (e.g. AAS) exhibit widely different responses depend- ing on the chemical form of the Pb compounds involved and their relative volatility. This problem is normally overcome by reaction of the alkyllead compounds with halogens (e.g. ICl 12) prior to analysis.Two groups of workers have reported methods for direct determination of Pb in gasoline using FAAS. Yulin et al. (91/3468) formed an emulsion using the surfactant Tween-60 prior to nebuliza- tion using an ultrasonic nebulizer while Lavrinenko et al. (91/3558) used the gasoline itself in place of fuel gas in the AAS flame. It is not clear from the abstracts whether these approaches completely eliminate the problems of selective300R JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY DECEMBER 1991 VOL. 6 volatilization. For environmental samples the extra sensi- tivity afforded by ICP-MS can be particularly useful. Shelton (9 11C557) has discussed the determination of total organic Pb in water soil and organic liquid using this technique. Other gasoline additives containing K and (methylcyclopentadieny1)manganese tricarbonyl have been determined using FI-FAES (9 11 1500) and GC-FPD (9 1/2458) respectively.As mentioned in last year's review there are several advantages to be gained by introducing petroleum and product samples to ICPs as aqueous emulsions rather than by diluting with an organic solvent. Borszeki et al. (9 1 1C 1 749) have adopted this approach for determination of S and heavy metals in oils and oil products using ICP-OES. Calibration was carried out using simple aque- ous standards. Readers may also be interested in a method for the determination of microamounts ( 10-200 ppm) of oil in water using an atomic absorption spectrometer (911434). The oil was extracted with petroleum ether and determined by monitoring the absoption at 256 nm.2.1.2. Lubricating oils This year has seen a marked reduction in the number of papers reporting the direct determination of wear metals in used lubricating oils reflecting the maturity of this type of analysis. However all atomic spectrometric techniques commonly used for these direct determinations suffer from particle size limitations. Saba (9112573) has modified the electrode configuration geometry and sample delivery to improve wear particle detection efficiency in an arc emis- sion spectrometer. Another development which may be of interest is a hydraulic high pressure nebulizer for ICP or AA spectrometry (9 llC2786 9 11C2805). The nebulizer was operated by forcing solution through a special nozzle of 10 20 or 30 pm under a pressure of 100-400 bar (1 0-40 MPa) provided by an HPLC pump. Aerosol was produced by impact of the resulting solution jet with an impact bead.The aerosol production efficiency was found to be very high (60%) giving rise to increased sensitivity and it was possible to nebulize undiluted oils directly. However the small diameter orifices and filters used will probably prohibit application to used oil analysis in view of the likelihood of blockage by particulates in the oil. In order to overcome the particle size limitations some form of sample degradation is normally required. This usually involves ashing of the sample. Barbooti et al. (911828) reported that more rapid dry ashing could be carried out in the presence of a porous inert material (silica gel). The silica gel was found to prevent sputtering and volatilization of the sample but some very volatile elements (e.g.Pb) were still lost during the ashing procedure. A similar approach has been adopted for determination of A1 in lubricating oil using GFAAS (911373). In this case a folded ashless filter-paper with the conical tip removed was placed in the sample (5- 10 g) in a nickel crucible and the oil was gently boiled and inflamed. The crucible was then transferred into a 750 "C muffle furnace cooled and the residue fused with NaOH and Na202. Baohu (911963) has also reported the determination of 13 elements in lubricat- ing oils using ICP-OES after ashing and digesting the samples in HNO and H202. X-ray fluorescence was among the techniques used in an interlaboratory comparison of methods for the determination of C1 in crankcase hydrau- lic metalworking and fuel oils (91135 1 1).The determination of additive elements (e.g. Ca and Zn) in lubricating oils using AAS can suffer from interferences due to the presence of polymers added to oil formulations as viscosity index (VI) improvers. The effect of various concentrations of the VI improvers styrene-isoprene styre- ne-butadiene poly(alkylmethacry1ate) and ethylene-pro- pylene has been studied (9 113575). Direct determination of Ca in lubricating oil by FI-AAS using emulsions has also been reported (9112590). 2.2. Organic Chemicals and Solvents This section of the review covers the analysis of organic chemicals reagents and solvents. Methods involving pre- concentration by extraction into organic solvents are not included in this section since most of the applications reported have been concerned with the analysis of high- purity inorganic compounds.This work is therefore re- ported in section 2.3. A summary of the analysis of organic chemicals and solvents is given in Table 2. 2.2.1. Chemicals As noted in last year's review (see J. Anal. At. Spectrom. l990,5,323R) few of the papers now being published deal solely with the determination of elements in specific organic chemicals reflecting the extensive literature which already exists in this area. Instead most of the work being reported is concerned either with speciation of trace elements or indirect methods for the determination of organic com- pounds using atomic spectrometry. One notable exception is in pharmaceuticals where atomic spectrometry can be used to replace standard visual-colorimetric methods for the determination of heavy metals giving improved accu- racy sensitivity and selectivity (9 11C2876).Application of XRF (9113472) and AAS (9113473) to pharmaceutical analysis has been reviewed. The determination of Zn in pharmaceutical preparations using AAS with a mixed solvent system (9 113392) and multi-element trace analysis of Penicillin G using ICP-OES have also been reported (9 K2876). Another area that has attracted some interest is sensitivity enhancement and matrix eflect suppression in AAS by complexation with organic compounds. Sensitivity en- hancements for Yb in FAAS (911186 91/3001) and Pd in GFAAS (9113348) have been reported.In both cases sensitivity was improved by about a factor of 20. Castillo et al. (9117) have reported a novel approach for improving sensitivity of Co determination in FAAS by the formation of volatile chelates (providing much higher transport efficiency than conventional solution nebulization). The most effective chelate was found to be trifluoroacetylace- tone. Two simple volatilization systems which could be adapted to conventional instrumentation were reported. The use of atomic spectroscopic detection in separation science has been reviewed by Uden (911C2086). These detectors are increasingly being used for speciation of trace elements using both gas and liquid chromatography. For GC helium MIPS and surfatrons have proved to be effective for both metal and non-metal detection with applications including halogen detection in environmental GC dual-element detection involving B and Fe derivatiza- tion for diols GC of organotin and Se and determination of Ni S and V complexes in petroleum products.Wylie (911C2087) has claimed that the MIP-OES response is nearly independent of molecular structure (within 5% or better) offering the possibility of compound independent calibration for quantitation and determination of empirical formulae. However more studies are required with a wider variety of compound types to assess the general validity of this assumption. The use of GC-MIP-OES for element selective determination of deuteriated compounds has been discussed in a recent publication (9 1/862). This can play an important role in determination of the function and structure of organic and biological compounds (e.g.deter- mination of metabolites in body fluids and tissues arising from the use of a deuteriated drug). For HPLC argon ICPsJOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY DECEMBER 199 1 VOL. 6 301R or DCPs are generally used with OES or MS detection for applications such as the determination of phosphinates polyphosphates and organomatallic cations. Sensitivity can be enhanced using a direct injection nebulizer which also gives a more uniform response for compounds having widely differing volatility (91/3282). In an alternative approach to improving sensitivity Blais et al. (9 111 57) have used a novel coupled HPLC-AAS system with thermo- chemical hydride generation for determination of arseno- betaine arsenocholine and tetramethylarsonium cations.The methanolic HPLC eluent was nebulized using a thermospray pyrolysed in a methanol-oxygen kinetic flame and the analytes were thermochemically derivatized to hydrides in the presence of excess of hydrogen. The volatile derivatives were then transported to a cool diffusion oxygen-hydrogen flame atomizer for AAS measurement. The absolute limits of detection for arsenobetaine arseno- choline and tetramethylarsonium cations were 1 3.3 14.5 and 7.6 ng respectively. It is perhaps surprising that there have been few reports on the use of plasma spectrometric detectors for supercritical fluid chromatography (SFC) in view of their inherent suitability for this application. However these will undoubtedly feature strongly in future reviews as SFC techniques become more widely accepted.A particularly innovative approach to speciation of trace elements has been described by Caruso and co-workers (91/860). By varying the power of a low-pressure helium MIP within the expansion stage of a VG PlasmaQuad ICP- MS instrument varying degrees of fragmentation of the analyte molecules was achieved. As the power was in- creased changes in the fragmentation pattern occurred eventually resulting in elimination of the parent ion. This approach permitted structural information to be obtained for compounds with mass within the range of the quadru- pole. Several alkanes and aromatic compounds with mass less than 160 were examined. The potential of using nitrogen as the plasma gas to obtain fragmentation was also studied.The indirect determination of organic compounds using AAS was reviewed by Kucova (9 1/2240). Procedures based on extraction of ion pairs formation of chelate complexes precipitation reactions or redox reactions were described. An indirect method for the determination of aliphatic amines was among those reported in the year under review (9 11709). The method was based on formation of dithiocar- bamate derivatives by reaction with carbon disulphide in basic medium followed by extraction in CHC13 of the copper@) dithiocarbamate. Applications of indirect mea- surement in the pharmaceutical field included FI determi- nation of chlorohexidine by precipitation with copper@) (9 112 189) and the determination of chlorodiazepoxide by zinc or cadmium reduction in a continuous system (9 1 / 12).The latter method which is selective towards the N-oxide group has a sampling frequency of 150 per hour. The high selectivity and sensitivity of AAS can allow indirect determination of many compounds in pharmaceutical preparations at ppm concentration levels. The methods are relatively cheap extremely rapid and can be readily automated and so are particularly suitable for quality control type applications. It therefore seems likely that applications in this area will continue to attract attention for some time. 2.2.2. Solvents Most of the papers published within this review period have been concerned with the eflect of organic solvents on ICP sources for OES and/or MS. In some cases the work concentrated on the benefits that can be gained by for example adding organic solvents to aqueous solutions while others were concerned with reducing matrix effects caused by introduction of solvents to the plasma. The influence of organic solvents added to aqueous solutions on ICP-OES spectral lines and background is a complex function of the nature of the solvent mixture composition excitation conditions and presence of matrix elements (9 112408).Most workers have reported increased transport efficiency in the presence of organic solvents possibly due to production of a smaller droplet size distribution. However the effect on plasma temperature and spectral line intensities depends on the nature of the solvent and the plasma operating conditions. Blades et al.(90/3965) found that for organic acids the temperature in the lower region of the central ICP aerosol channel was increased relative to H20 solutions giving rise to higher ion to atom line ratios. Conversely for alcohols Steffan and Vujicic (91/C2722 91/C2791) reported a cooling of the analyte channel of the plasma resulting in an increase in S/B ratios for lines with excitation potential less than 5 eV but a decrease in SIB ratio for lines (atomic and ionic) with higher excitation potential. Irrespective of the mechanism addition of organic solvents to aqueous solutions can be beneficial. For example by adding ethanol to sample solutions and using desolvation detection limits for ICP- OES determination of rare earth elements were improved by an order of magnitude (91K2122).Addition of ethanol to the sample solution can also reduce the tendency of elements to form refractory oxides in the ICP tail plume. This is beneficial when the ICP is used as an atomizer for AFS. Thus a limit of detection of 24 ng ml-l for the determination of Eu in yttrium oxide was obtained. Addition of organic solvents to aqueous solutions can also be beneficial for ICP-MS. Evans and Ebdon (911852) showed that dramatic reductions in polyatomic ion interfer- ences (ArCl Ar2 and C12) were achieved by adding about 10% propan-2-01 in water. However similar benefits were also obtained by adding a small amount (about 0.03 1 min-l) of N2 to the nebulizer gas and so the latter approach was recommended. Most of the work on analysis of organic solvents carried out during the review period has been concerned with the effects of volatile solvents in ICP spectrometry.Ebdon and co-workers (9 1/C778 9 1/C1646) have compared the effects of different interfaces spray chambers and aerosol desolva- tion procedures for introduction of organic solvents to the ICP. One of the most criticial parameters appeared to be desolvation. Plasma excitation temperatures were observed to decrease with increasing solvent vapour loading when controlled with a variable temperature condenser (9 1/87 1). It was suggested that the main impact of desolvation with organic solvents was to reduce the C2 species population in the plasma which in turn strongly influenced plasma temperature and reduced band interferences in ICP-OES. An electronic device based on Peltier cooling was described which was used to control the solvent plasma load in ICP spectrometry (90/3976).The device was found to be more convenient than an aerosol cooling tube immersed in a liquid cooling bath and offered potential for automation of solvent load experiments. Weiderin et al. (90/3995) have clearly demonstrated the benefits which can be gained in ICP-OES by employing aerosol desolvation. A two-step desolvation system was used for continuous ultrasonic nebulization of organic solvents. The aerosol was first heated above the b.p. of the solvent with vapour subse- quently removed in two condensers kept at - 10 and about - 80 "C respectively. Limits of detection were comparable with those obtained by ultrasonic nebulization of aqueous solutions (0.2-5 pg l-l) even for 'difficult' volatile solvents such as methanol acetone acetonitrile or ethanol.Band emission from C2 was found to be about 25 times less302R JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY DECEMBER 199 1 VOL. 6 than when the aerosol was partially desolvated using only a condensation temperature of - 10 “C. An alternative approach to reducing band interference in ICP-OES analysis of organic solvents is to oxidize the molecular species (e.g. C,) by addition of oxygen or air to the plasma. Tang et al. (91/C2840 91/C2130 911C2131) have reported that molecular bands due to organic solvents could be greatly depressed (or even eliminated) using a 50% v/v air-argon cooled ICP. Several atomic lines also showed optimum S/B ratios at this concentration of air but ionic lines showed maxima at 10% v/v air at which concentration the CN band emission was very intense.Nevertheless detection limits for 12 analytical lines were lower in a 50% v/v air-argon cooled ICP than in a conventional argon cooled ICP. However in a study involving addition of oxygen to the plasma it was found that CN C2 N2 and NO bands were reduced but not completely eliminated and that background noise was increased (9 1 /C2909). Aerosol desol- vation is therefore probably the preferred approach espe- cially in view of its effect on plasma temperature. Other approaches to the introduction of organic solvents to ICPs which have been reported include use of a thermospray nebulizer (911C2907) and a modified direct injection nebulizer (9 113282).The latter approach is particularly useful for samples which contain volatile analyte species since the system gives a more uniform response to com- pounds having widely different volatilities. A few papers have been published concerning the introduction of organic solvents in FAAS. Bagdi et al. (9 1/942) studied the atomization processes in FAAS analy- sis of oganic liquids while Watling et al. (9 1 / 1463) observed on-line ionization suppression in organic solutions using a non-miscible aqueous suppressant (KCl solution). For any workers who have difficulty obtaining IBMK a 1+1 mixture of butanol and ethyl acetate has been reported to be an acceptable alternative for extraction of metal complexes for subsequent AAS analysis (9 1/999). Miscibility with water can be reduced by adding a small amount of AI(NO3h.23. Inorganic Chemicals and Acids This section of the review covers analysis of inorganic chemicals and acids. However those chemicals generally regarded as exhibiting material functionality are not in- cluded since these are covered in section 3 of the review. The structure of the review this year differs from previous years in that analysis of catalysts is also included in the later section in view of the fact that many catalyst support materials are refractories and that many of the techniques used for characterization of catalyst surfaces are similar to those used for other ‘advanced materials’. Since the boundary between the categories is somewhat arbitrary however readers should also refer to the later section and Table 3 for comprehensive coverage of analysis of ‘inor- ganic chemicals’ and catalysts.2.3.1. Chemicals Analysis of solutions containing high salt concentrations continues to attract considerable attention in view of its importance in several industrial applications. In the chlor- alkali industry trace elements even at very low concentra- tions can cause blockages of the sensitive membranes employed in the electrolytic production of sodium hydrox- ide (9 1/C745) while in the petroleum industry determina- tion of trace elements in sea- and formation waters is important for prediction of scaling problems and to aid reservoir diagenesis studies (91/2555 91/2775,91/2929). A review with 165 references has been published covering the determination of trace components (metals inorganic anions and organics) in sea-water and salts (91/949).Inductively coupled plasma emission spectrometry is an attractive technique for the determination of trace elements in view of its multi-element capability good sensitivity and ease of operation. In solutions containing high levels of dissolved solids however the precision and accuracy of the technique can be severely degraded by salt deposition on the nebulizer orifice and evaporation-atomization-excita- tion effects in the ICP. The former problem can be overcome by using an appropriate nebulizer e.g. Pan et al. (911368) have reported the direct determination of trace elements in brine using an axially viewed ICP-OES instru- ment with a bugle-shaped concentric nebulizer.The latter problem can be more difficult to resolve and matrix matching of standards and samples is the conventional approach. This may not be possible if the sodium content of the samples is not known. Thomsen (911C786) has there- fore adopted a novel approach in which the sodium concentration in the sample was estimated by measuring the Sc atom to ion line ratio and correction factors applied to compensate for the matrix effect. Presumably the same result could be achieved by measuring the sodium concen- tration directly using its emission line. Precision and accuracy of determinations can be improved using FI (91/C2128 9112693) but in order to obtain the best performance some form of matrix separation is generally required. Chelating ion exchange has been shown to be a convenient method for on-line preconcentration of trace metals and matrix removal prior to ICP-OES or ICP-MS analysis (9 1 1C7 77).Determination of trace elements in solutions containing high levels of dissolved solids can also be carried out directly using FAAS with suitable modifications. Gruber et al. (9 1 / 1490) reported the determination of Al (dinitrogen oxide-air-acetylene flame) in salt solutions using a jaw-type burner with a large opening while Bekzharov (9014010) used a dosage device which employed the dosage scheme ‘washing solution-sample-washing solution’ for analysis of 30% NaCl and 30% NH4F solutions. As with ICP-OES however better results are generally achieved if some form of matrix separation is employed. Generally elements of interest were separated from Group I elements (Na) by coprecipitation (9 1/2635) or by extraction into organic solvent using a chelating agent (91/948,9 113479).However the reverse separation can also be utilized. Samoilov et al. (9111366) have developed a method for the determination of Rb and Cs in calcium chloride brines after extraction of Ca into heptane using a mixture of ammonium di(2- ethylhexyl) dithiophosphate and tributyl phosphate. Methods for the determination of Cd Cr Cu Ni and Pb in concentrated calcium chloride1sodium chloride including FAAS with and without preconcentration and ETAAS have been compared (9113455). Electrothermal AAS was found to be most satisfactory although on-line preconcen- tration has also been reported to reduce matrix interfer- ences using this technique (90140 12).This year has seen something of a renaissance in the use of AAS with preconcentration techniques for analysis of high-purity inorganic compounds. At first sight this may seem somewhat surprising in view of the increasingly widespread availability of rapid multi-element techniques with high sensitivity such as ICP-MS. However although the latter technique performs exceptionally well for many elements those below mass 80 can suffer from severe interferences from argon and polyatomic ions necessitating combined use of ICP-MS and ICP-OES to achieve compre- hensive elemental coverage (9 1 /C 163 1). For determination of the lighter elements use of AAS with preconcentration may offer a cheaper and more attractive alternative. The most popular preconcentration technique reported in-JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY DECEMBER 199 1 VOL.6 303R volved extraction into IBMK using a complexing agent such as APDC and this approach has been applied to the determination of a large number of elements in high-purity nickel (911237) and zinc salts (91/3581) ammonium per- rhenate (9014008) and aluminium chloride (91133 17). Sub- ppm Osg g-l) detection limits were generally achieved using this approach. Other chelating agents which have been used include pivaloyltrifluoroacetonate for the determination of Cu in cobalt oxide (9 1/969) and 2-(2-benzoxazolyl)cyanoa- cetaldehyde for the determination of trace elements in molybdates (9 1 12704). Preconcentration using electrolysis (9112498) and co-precipitation with LL~(OH)~ (9 113053) have also been used for the ETAAS determination of Pb in high-purity potassium bromide and As in copper sulphate electrolytes and electrolytic copper respectively.Precon- centration by extraction into organic solvents can also be used with ICP-OES provided that the solvent employed is not too volatile. Two on-line separation systems utilizing extraction into xylene have been reported for the determi- nation of ultra-trace (ppb) levels of Al in concentrated salt solutions (911C2913) and for the determination of Sb in zinc electrolysis liquids (9 1 /C29 12). The latter method employed a particularly novel tandem separation approach in which the Sb was reacted with KI to form Sb13 which was extracted into xylene and subsequently converted into For the determination of trace element impurities in high-purity solids it is preferable if these can be analysed directly rather than after digestion in order to avoid dilution of the sample and reduce risks of contamination. Atomic emission spectrometry using a d.c.arc is particularly suited to these determinations in view of the simultaneous multielement capabilities of the technique. Sensitivity can be improved using such a system by distilling the matrix from a carrier such as carbon (91/341 911470) or AgCl-SrF on which the impurities are retained and preconcentrated. Using this approach Durinov et al. (911370) were able to obtain limits of detection of 0.01-1 ppb (ng g-l) for the determination of 19 trace elements in high-purity boron bromide.Laser ablation ICP-MS is a relatively new technique for trace element analysis of solid samples which is rapidly gaining popularity. Perkins et al. (911C1637) applied the technique to the determination of Ba Fe Mg Mn Pb and Sr in calcium carbonate. Good calibration graphs were obtained either using added In203 as internal standard or using a minor calcium isotope. The measured Mg/Ca and Sr1Ca ratios from the shells of certain organisms can be used as palaeosalinometers and palaeothermometers. How- ever laser ablation ICP-MS analysis of bivalve shells showed irregular distributions of the minor and trace elements casting doubt on the validity of traditional methods which use a bulk shell digestion approach. A more traditional (if somewhat less quantitative) approach to spatially resolved elemental analysis of solid surfaces is SIMS.Hussain et al. (9112356) used SIMS to study the distribution of magnesium stearate lubricant on the sur- faces of sodium chloride tablets. X-ray fluorescence is undoubtedly one of the most widely utilized techniques for direct bulk analysis of solid samples within industry. However the technique is prone to severe matrix eflects arising from particle size and X-ray absorp- tion effects. This often necessitates that samples are fused into a glass bead prior to analysis. If the sample contains sulphides however problems can occur due to volatiliza- tion of sulphur species and/or attack of the platinum crucibles used to perform the fusion. Norrish and Thomp son (911205) developed a method to overcome these problems involving short pre-oxidation treatment using sodium nitrate prior to fusion.X-ray fluorescence methods have also been reported for the determination of bromides -US SbH3. in caesium iodide (91/3027) and of S in sulphur sorbents and coal ash (9 1/3 177). In addition to its traditional role in determining total element concentrations in samples there is growing evidence that in some cases information can also be obtained regarding the chemical form of the element in the sample. LaBrecque and Rosales (90/4157) used Co WKa! intensity ratios to study the calcination products of cobalt carbonate (9014 I 57). Results were consistent with those obtained using XRD. A review of use of XRF within a cement plant (9112683) may also be of interest.Determination of trace element impurities in high-purity gases is an important requirement within the semiconduc- tor industry. Shishov (9112689) has produced a review (1 33 refs.) on spectrochemical analysis of high-purity volatile inorganic hydrides halides alid organometallic substances in which the limitations of several techniques were com- pared. Specific applications described included the determi- nation of arsine in mixtures of phosphine using AAS (9111339) and the determination of P in trichloro- silane using ICP-OES (91/77). Methods for the determina- tion of trace metal impurities in high-purity N2 H2 HCl NH BzH6 SiH ASH and PH3 using ETAAS have also been established (9 112624). Many of the methods presented are suitable for on-line control. Several papers have been published dealing with elemen- tal analysis of fertizizers using AAS (9 1 / 1009 9 1 / 1 290 91/1291 91/3583) ICP-OES (91/2791) and XRF (9113456).Readers may also be interested in an indirect method for the determination of ammonia using AAS (9 1/927) and a comprehensive review on the determination of trace impurities in chalcogens covering a wide variety of analytical techniques (9 11342). 2.3.2. Acids Unlike previous years this review year has seen very little work published on the determination of trace elements in high-purity acids (but see also section 3.2 for semiconductor reagents). One exception is a report on the use of an ultrasonic nebulizer for the analysis of high-purity acids using ICP-OES (9 1 /C 19 12). It can perhaps be inferred that the techniques available are now adequate for most applica- tions of this type.Readers may also be interested in an ETAAS method for the determination of ppb concentra- tions of Hg in concentrated hydrochloric sulphuric and phosphoric acids (9112714). The method described in- volved reduction of mercury compounds using NaBH or Snn and trapping of the resulting mercury vapour by amalgamation with gold on the wall of a graphite cuvette. The effect of low concentrations (< 1% v/v) of mineral acids on ICP-OES emission intensities has been studied by Mermet and co-workers (91/2980). An increase in signal was observed for HC1 with maximum enhancement at an acid concentration of 0.00 1 % v/v HClO however caused a suppression of the signal. No significant effect was observed for HNO,.In view of the fact that most standards used for calibration of ICP-OES instruments are prepared in dilute acid solutions this work has serious implications which all analysts making use of this technique will have to take into consideration. One possible solution to the problem is to make use of internal standardization. Garden et al. (9113208) have shown that mineral acid interferences can largely be compensated for by utilizing this approach. Significant enhancements from low concentrations of min- eral acids in ICP-AFS have also been reported (91/2865) with the effect being more pronounced when propane was used as reducdant. 2.4. Nuclear Materials Atomic spectroscopic methods play an important role in the nuclear industry for quality assurance at different stages304R JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY DECEMBER 199 1 VOL.6 of nuclear fuel fabrication (9 1/944) and for monitoring low- level radioactive waste water treatment (9 l/C550) and leaching of vitrified radioactive waste (9 1/1374). Generally comprehensive approaches are adopted in which atomic spectrometry plays a key role alongside other techniques such as alphahewgamma activity counting ion chromato- graphy and electrochemistry. Certified reference materials for use in nuclear safeguard applications and in geological and environmental research are distributed by the New Brunswick Laboratory (9 UC1947). Inductively coupled plasma OES forms a major part of most schemes for elemental analysis of nuclear materials. However most of these materials exhibit complex spectra originating from heavy elements such as uranium.The elements of interest therefore generally have to be separated from the matrix. A review with 110 references has been published on the use of ICP-OES for analysis of high-purity substances including nuclear materials (9 112690). This review compared the analytical performance of ICP-OES with and without the aid of preconcentration techniques. The most commonly reported approach for removal of uranium or thorium from solutions was extraction using solvents such as tri(2-ethylhexyl) phosphate (TEHP) (91/C546) TOP0 (9 VC547) or tributyl phosphate (TBP) (9 1/C2729). However these methods are generally not fast enough for process control applications and also can generate large volumes of flammable contaminated sol- vent.Most recent work has therefore concentrated on column based extraction systems. Columns which have been described include TBP-modified poly(trifluoroviny1 chlo- ride) (91/435) TEHP coated acrylic resin (91/C546) and 7 1 1 anion-exchange resin (9 1/3 1 30). Uranium could be stripped from the former column using nitric acid and since the TEHP resists acid degradation it was claimed that the columns can be used indefinitely. For elements present at very low concentrations some form of preconcentration was required in addition to matrix separation. Two ap- proaches have been described for the determination of rare earth elements in uranium and nuclear fuels using precon- centration on levextrel-PMBP resin (9113 130) and concen- tration on an alumina column followed by precipitation with oxalic acid (91K2729).Matrix separation using ion exchange has also been described for at-line analysis of plutonium process streams (9 1/C55 1). For determination of Te in spent fuel reprocessing streams anion exchange was preceded by a rough separation by precipitation (90/3952). Simply changing the pH of the solution to make it alkaline was found to precipitate most of the fission products along with heavy metals but did not affect the Te. Cation- exchange separation has also been used with a.c. arc OES for the determination of B in uranium metal (91/2607). In addition to time and convenience considerations extraction techniques also have the disadvantages that some of the trace elements can be extracted the uranium matrix may not be fully extracted and the separation can cause contamination.Wangen et al. (91K541) and van Veen et al. (91K2885) have reported chemometric ap- proaches for compensation of uranium interference in ICP- OES spectra based on least-squares fitting of spectral regions and Kalman filtering respectively. Encouraging results were reported and in the latter case limits of detection were obtained for 12 elements in a 4% uranium solution which were suitable for ASTM C787 specifications without use of chemical separation. As with ICP-OES determination of trace elements in nuclear materials using AAS usually requires matrix separa- tion. For example Heinig et al. (91/2677) found that although Ru could be determined directly in model repro- cessing solutions using FAAS in the range 20-80 pg ml-l for lower concentrations separation of Ru was required.Matrix separation techniques for both FAAS and ETAAS were similar to those adopted for ICP-OES e.g. extraction chromatography with GDX-30 1 beads treated with trialkyl- phosphine oxide (911439) or levextrel-TBP resin (9 1/2373). When combined with ETAAS ppb limits of detection could be achieved. X-ray fluorescence is an attractive technique for process monitoring in view of the inherent stability and robustness of the technique. Saleem et al. (91/3294) described a simple method for the determination of Dy Er Eu Gd and Sm in uranium solutions using XRF with matrix matched stan- dards. Energy dispersive XRF is a particularly attractive technique for monitoring processes since several elements can be measured simultaneously.However owing to the limited dynamic range of this type of detector intense lines originating from the matrix must be eliminated from the measured spectrum. Gal'tsev et al. (91/3401) described a system which makes use of reflection from a pyrolytic graphite assembly to eliminate unwanted lines from the fluorescence spectrum of nuclear power plant spent fuel reprocessing liquids prior to measurement of Mn Pd Rh Ru and Zr using EDXRF. As with other atomic spectros- copic techniques performance of XRF for analysis of nuclear materials can be improved using matrix separation. A method for the determination of Ga in plutonium using anion exchange and XRF has been reported (91/454).Unlike most other atomic spectroscopic techniques for the analysis of nuclear materials the simple ICP-MS spectra produced by nuclear materials means that for many applications this technique can be used with no matrix separation (9 1/C 1649). This advantage coupled with the extremely high sensitivity of the technique (ppt limits of detection) (91/C544) have resulted in its gaining wide- spread application throughout the nuclear industry. Appli- cations reported during the review period have included measurement of transmutation products in materials for fusion reactors (91K1648) and determination of 99'c and 237Np in effluents (9 l/C1647). Unfortunately isobaric and polyatomic ion interferences particularly below mass 80 often necessitates that a combination of ICP-OES and ICP- MS is used in order to obtain complete elemental coverage (9K542).A possible solution to this problem is use of coupled ion chromatography ICP-MS. Alonso et al. (9 1 /C 1632) have used this approach both for elimination of matrix and isobaric interferences and for speciation studies of transuranium elements in solution (9 1K1632). Although most applications reported so far have utilized conventional nebulization for sample introduction other approaches such as laser ablation for direct analysis of solids (9 1 /C545) and electrothermal vaporization (914343 9 1/C545) are gaining popularity for the analysis of nuclear materials. Another sensitive element and isotope detection system for plutonium and other long-lived radioactive nuclei which has been reported is RIMS (9112290).Detection limits of the order of 1 x lo7 atoms were achieved with a four colour multi-step resonance ionization scheme which nearly matched the target of 1 x lo6 atoms required for environ- mental applications. However since detection limits of 1 x lo6 atoms can be readily achieved with commercial ETV-ICP-MS systems (91/C543) it is difficult to see how the cost and complexity of the RIMS approach can be justified especially in view of the rapid multi-element capability and versatility of ICP-MS. The latter approach will almost certainly find more widespread applications throughout the nuclear industry. 2.5. Process Analysis and Automation X-ray fluorescence is particularly well suited to on-line elemental analysis in view of its stability robustness non-JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY DECEMBER 199 1 VOL.6 305R destructive nature and ability to operate in harsh industrial environments. Applications of on-line XRF and XRD analysis techniques to industrial process control have been reviewed by Hietala and Kalnicky (911145). On-line XRF has been used in mineral processing applications for about 20 years and continues to find widespread applications in this field for example for on-stream ore slurry analysis (9 111 44). Applications in other industries have been slower to develop but may be boosted by the availability of a new commercial EDXRF process analyser (9 l/C209 1). The analyser is enclosed in a stainless-steel NEMA 4X cabinet which can operate in a Class 1 Division 1 Group C or D area.Sample excitation is accomplished using a water cooled 50 kV 1 mA rhodium anode X-ray tube with detection using a thermoelectrically cooled Si(Li) detector. The unit can accommodate up to eight flowing streams with eight static cells for calibration. The system may be particularly useful for applications within the petroleum industry e.g. determination of S in hydrocarbon streams Pb in gasoline and additive elements in lubricating oils. Leland et al. (91/143) discussed use of fundamental parameters software for calibration of the latter two on-line applications. X-ray fluorescence has also been used for the determination of SO2 in ambient air and in stacks of a tobacco curing plant (9113555). Sulphur dioxide was col- lected on filters impregnated with 5% Na2C03 and 3% glycerol and S was then determined using EDXRF.The limits of detection for S were about 30 pg using a sealed proportional counter system and about 2 pg using a system with a Si(Li) detector. For monitoring liquid process streams ICP-OES is an attractive option in view of its speed multi-element capability and low detection limits for most elements. However in general sample introduction systems used with laboratory based ICP-OES systems are not suited to continuous operation without maintenance which is a requirement in process control applications. Foster and Carroll (9 1/C2027) described a sample introduction system which was specifically designed for on-line analysis. The ICP can be used in conjunction with on-line preconcentra- tion systems if very low concentrations of elements are to be determined.Knapp and co-workers (9 1/ 102) compared two chemically bonded chelating ion-exchange systems which were found to be suitable for automatic-on-line preconcen- tration of trace elements for water analysis. On-line real-time analysis of process gas streams such as gassification and combustion processes is becoming increasingly important. A high-power high-flow mixed gas helium-argon ICP-OES instrument has been described which is suitable for these applications (9 1/466,9 l/C2029). The particulate laden gases were injected directly into the ICP torch at high temperatures (500 "C) and at the high sample flow rates (up to 5 1 min-l) necessary to prevent loss of large particles (1 0-20 ,urn) between the process sampling point and the plasma.Elements of interest including As Ca Cd Fe Pb S and V were continuously monitored to provide real-time process information. Automated analysis of solid samples by AAS and ICP- OES has been the subject of some attention during the review period. Kempeneer et al. (91/1506) described a system for AAS analysis which consists of a powder sampler an integrated microbalance and a microprocessor controlled transport and handling system for the sample boat. Generally however handling of solids is a more difficult process to automate than that of solutions. Haswell et al. (91/C773) have therefore adopted an alternative approach to automated solid sample analysis in which slurries of the material to be analysed were passed continu- ously through a microwave oven and digested on-line.This novel approach may prove to be useful in eliminating some of the particle size limitations which have restricted application of direct sluny nebulization for sample intro- duction in atomic spectrometry. An expert system for real- time control of an atomic absorption spectrometer may also be of interest (9 11468). 3. ADVANCED MATERIALS This section of the review is concerned with developments made in the characterization of advanced materials using atomic spectrometric techniques. It is evident from the literature that there has been an increase in activity in this field in the past year particularly in respect of the analysis of high-purity inorganic materials. This area has been widened in the current review to include catalysts which are essentially materials with a highly specific functionality derived from an inorganic structure (e.g.noble metal on alumina). In previous ASU reviews in this series informa- tion on the characterization of catalysts had been included in the Chemicals section because of the strong association with that industry's operations. However in view of the growth of the inorganic materials sector it is considered that developments in methodology for the characterization of catalysts is now more usefully presented in association with the ceramics and refractories topic since similar analytical problems are encountered. A summary of analyti- cal methods for the analyses of advanced materials is given in Table 3. 3.1. Polymers and Composites A number of reviews have been published in the period covered by this ASU.The characterization of plastic materials using surface analysis techniques [e.g. SIMS electron spectroscopy for chemical analysis (ESCA) and LMMA] has been surveyed (9112340). The application of atomic spectrometry to the analysis of advanced materials has been discussed within the context of present capabilities and likely future needs particularly in respect of the direct characterization of solids (9 1/837). Specific reviews have been published on the application of transmission electron microscopy in materials science (9113476) and on the use of total reflection XRF in forensic work including the examination of plastics inks and fibres (9 112648). There has been a significant increase in the last review year in the use of laser ablation as a means of sampling polymer based materials for examination by MS.Laser desorption FTMS was utilized for the determination of mixtures of sodium alkyl benzene sulphonate ionic surfac- tants on textiles (9 112258). The identification of indigo dyed fibres was achieved using LMMS to fingerprint the materials (9 112 175). Both atomic and molecular ions produced by the laser beam induced evaporation were used in discrimination of the fibres on the basis of the mass spectra obtained. The classification of polymers using LMMS has been aided by the application of pattern recognition in distinguishing spectral features (9 112 165). The mass spectra of 19 different polymers were obtained in the range 0-300 u at three different laser irradiances and linear discriminant analysis was performed on the principal component data using the Resolve software package.It was shown that the mass spectra were distinct and could be easily differentiated using this pattern recognition ap- proach. Other examples of the use of LMMS in the306R JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY DECEMBER 1 99 1 VOL. 6 TABLE 3 SUMMARY OF ANALYSES OF ADVANCED MATERIALS Technique; atomization; analyte form* Sample treatmenthmments Element Matrix Reference POLYMERS AND COMPOSITES- Al Paint aerosols SEM-XRF or SIMS M - ; S or L Bulk paint samples and aerosol size fractions Determination of distribution of As ions in ion Material dissolved in hot nitric acid; B determined in Sample heated in DMF 1-2 drops of acetic acid analysed to determine element mass distribution implantation masks range 250-1290 ppm added and cooled solution diluted with acetone; detection at 228.8 nm HC1; silicates if any volatilized with H,SO,-HF; solution diluted to 50 ml with water and analysed for Cu at 324.7 nm detection of F at major levels; precision 1-2% at 30% F level 10 g of sample ashed and extracted with 20 ml of Layered structure dispersive element used for As for As As for Cu; detection for Mn at 279.5 nm Sample preparation as for cd detection at 283.3 nm Collaborative trial to evaluate the precision of method recommended method published Microwave assisted digestion of samples claimed to improve recoveries Sample is calcined at 650 "C and ash treated with formic acid to reduce the palladium oxide formed; solution evaporated residue dissolved in aqua regia and diluted with water Depth profiling of migration of S as sulphate through 200 pm thick coating Investigation of bloom and other surface defects using SEM with X-ray spectrometer facility Samples treated with organic solvents and diluted with acetone; interferences investigated Six types of white paint were found to have Ti contents in range 19-33% Sample introduced into instrument in form of stable oil-water emulsion by adding IBMK and Brij-30 Depth profling of flame retardant material for Cl Sb Si and Zn by progressive removal of thin layers of sample using a lathe Graphite furnace pretreatment of solid sample followed by laser ablation into ICP-MS instrument for qualitative survey analysis of PVC polypropylene synthetic rubber and paints Direct qualitative and quantitative analysis of nylon polypropylene polyethylene and polyester using laser ablation sampling Quantitative analysis for Ca Mg Na and Si as oxides in identification of paint used in coatings Determination of pigments additives and coating layers using energy dispersive instrument Quantitative analysis of solid polymers by laser ablation Samples prepared by embedding beads or powders in epoxy and microtoming thin sections; differentiation of polymers by pattern recognition on LMMS spectra Mapping of spatial distribution of ions in a variety of matrices Direct quantification of Al Ca Fe K Na and Si using wavelength dispersive instrument Determination of inorganic components (unspecified) in base material by X-ray microanalysis 9113506 9 1 I234 1 9111 133 91/13 As Polyimide B Carbon fibre- epoxy composites Cd Poly(viny1 chloride) M,F;L M,ETA,L cu Rubber M,F;L 9113116 F Poly(tetduoroethy1ene) XRF;-;S 9111592 M&! Polyimide Mn Rubber Pb Poly(viay1 chloride) Pb Paint SIMS M,F;L M,ETA;L M-;L 9112341 91/31 17 91113 9 11 1039 Pb Paints AE;ICPL 9 llC2026 Pd Acrylonitrile rubber M,F;L 9 113045 S Phenolic coating S EPDM rubber Sn Poly(viny1 chloride) Ti Paint Zn Plastics Various (4) Nylon PIXE-;S 9113384 9 1 I3470 91194 9111 168 91/71 1 9014 1 64 SEM;-;S M F or ETA;L Electron probe or M,F;L M,F;L xw,-;s Various Polymers and paints MS;ICP;S 911104 Various Polymers MS;ICP;S 91lC751 Various (4) Paint Various Paper Various Polymers Various Polymers xw,-;s xw,-;s MS;ICP;S MS$aseqS 9111 182 9 llC17 19 91x1923 91/2165 Various Polymers Various (6) Polyethylene Various Vinyl adhesive tape MS;laser,S xw,-;s XRF;-;S 91/21 79 9112543 9112565JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY DECEMBER 199 1 VOL.6 307R Table 3 SUMMARY OF ANALYSES OF ADVANCED MATERIALS-continued Technique; atomization; analyte form* MS;ICP;S Element Matrix Various Plastics Sample treatmentfcomments Laser ablation sampling using internal standard for semiquantitative analysis accurate within a factor of 2; quantitative data agreed well with XRF and NAA data Reference 91/3205 SEMICONDUCTORS Al Al Al Al Al Al Al As As As As As B B Bi Silicon wafers AA;-;L Impurities remaining on the wafer are collected into the liquid resulting from the reaction of the oxide and HF vapour Use of tetrabutyl ammonium chloride as a sensitizing agent; matrix interference from iron and calcium was eliminated by standard additions Zeeman-effect background correction.(Detection limit 8 ppm) resonant transitions to enhance ion yield for time- of-flight MS Measurement of aluminium content in matrix layers of nm thickness Samples were decomposed in HN0,-HF-H,02 and after evaporation residues were dissolved in HCI; variations in sample preparation for different techniques reported; comparison of methods See ref. 91/929 Direct introduction of gas through base of ICP torch; gas handling rig allowed mixture of argon hydrogen silane and arsine in precise amounts measurement at interfaces and in bulk sputtering rate in each layer to translate intensity-time signal into concentration-depth Two-dimensional profiling of shallow (sub-pm) As doped regions As for Al Microsampling technique used in conjunction with Direct laser ablation of sample by tuning to known Study of thin layered material using arsenic Quantification using relative sensitivity factors and 91/464 Industrial silicon AA;F;L 91/929 Industrial silicon AA;F;L 91/1469 Aluminium gallium arsenide MS;laser;S 91/2289 Aluminium gallium arsenide Silicon SIMS or TEM 91/2367 9 1/295 1 AA or AEETA or ICP or DCPL 91/3011 91/858 Industrial silicon Silane AA;F;L MS1CP;G Gallium phosphide- Titanium disilicidel silicon gallium arsenic phosphide SIMS SIMS 91/2270 91/2301 Silicon Silicon Gallium arsenide SEM 91/2308 9 11295 1 91x1 738 AA or AEETA or ICP or DCP;L MS;r.f.spark$ Semiquantitative analysis with claimed 20% accuracy using relative sensitivity factors. (Range of B levels found from ppm to sub-ppm) As for As Silicon dioxide-titanium Cadmium mercury telluride disilicide-silicon SIMS AA;ETA;L 91/2301 91/924 Layers of material ( 5 mg) were removed by etching with 2.5% bromine in 4 mol dm-3 HBr detection using Zeeman-effect background correction. (Detection limit 0.4 ppm Bi) As for B. (C measured as low as 150 ppb) Response for Ca enhanced by presence of tetrabutyl ammonium chloride; normal calibration could be used Samples were analysed by layer following oxidation and etching; Cd fluorescence detected at 228 nm and method reported to be free of systematic error Calibration was camed out using external standards consisting of thin films of doped gelatine on pure wafers; accuracy confirmed by FAAS As for Bi.(Detection limit 0.14 ppm Cu) Sample ashed in oxygen to remove tellurium the residue dissolved in HN0,-H,SO (1 + 5) and Cu concentrated on Pt rod electrode which was part of HCL assembly. (Detection limit 10 ppb of Cu) implantation before and after annealing Depth profiling of Er concentration resulting from As for A1 Use of high-resolution instrument to avoid spectral Determination camed out using normal calibration interference on Fe curve; see Ca C ca Gallium arsenide Industrial silicon MS;r.f. spark$ AA;F;L 91fC1738 91/30] 1 Cd Cadmium mercury telluride AF;ETA,L 91/ 1104 c o Silicon wafers XRF;-;S 911164 c u c u Cadmium mercury telluride High-purity tellurium AA;ETA;L AE;HCL;S 91/924 91/3056 Er Silicon SIMS AA,-;L MS;ICP;L AA;FL 9 112325 Fe Fe Silicon wafers Electronic grade reagents 91/464 9 lfC1897 Fe Industrial silicon 91fC3011308R JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY DECEMBER 199 1 VOL. 6 Table 3 SUMMARY OF ANALYSES OF ADVANCED MATERIALS-continued Technique; atomization; analyte form* SIMS Element Ga Gd Ge H Hg In K Li Na Na 0 0 P P Tb Te Various Matrix Silicon and silicon dioxide multilayers Metallic thin film on silicon wafer Gallium arsenide Sample treatment/comments Liquid metal ion source based on Ga used to achieve Quadrupole spectrometer used for depth profiling at Study of extent of Ge migration from high-resolution depth profiling sub-pm resolution nickel-germanium-gold ohmic contacts to gallium arsenide Instrument operated in direct bombardment mode and H detected using quadrupole analyser by monitoring SiH As for Cd; tellurium was found to interfere with Hg determination by cold vapour method Direct determination using platform furnace with Zeeman-effect background correction; recoveries in the range 94-108% reported Study of matrix effects in the determination of alkali metals; sample dissolved in 6 mol dm-3 HCl- 14 mol dm-3 HNO (3+ 1) and diluted with H,O.(Detection limit for K was 1.6 ppb) As for K. (Detection limit for Li was 0.2 ppb) As for K. (Detection limit for Na was 1 ppb) As for Al As for B. (0 measured as low as 50 ppb) Study of oxygen diffusion through silicon dioxide Study of phosphorus diffusion; evidence for As for A1 coating on silicon wafer segregation of dopants along dislocations found Reference 9112265 91lCl778 9 1/23 1 3 9 112346 9111 104 911429 911219 91/219 911219 9 11464 91lC1738 9112594 9 112305 9112951 78 04 11 MS;GD,S SIMS Silicon hydride films MSsputtered neutra1s;S Cadmium mercury telluride AF;cold vapour;L Indium-mercury cadmium telluride AA;ETA;S Cadmium mercury telluride AE;F;L Cadmium mercury telluride Cadmium mercury telluride Silicon wafers Gallium arsenide Silicon dioxide coatings AE;F;L AE;F;L MSr.f. spark$ SIMS AA;-;L Silicon TEM or SIMS Silicon AA or AE; ETA or ICP or DCP;L MS;GD;S Metallic thin film on silicon wafer Cadmium mercury telluride Electronic grade quartz As for Gd 91x1 91/1 91/ AF;ETA;L MS;ICP;L As for Cd; Te fluorescence was detected at 214 nm Sample dissolved in mixture of HN0,-H,SO,/HF evaporated to dryness; residue dissolved in HCl-HNO and evaporated again with final dissolution in 2% HNO,; comparison with NAA AAS XRF and AES Total reflection instrument with rotating anode X-ray tube and monochromatic primary radiation used to improve SIN for detection of As Cr Cu K Ni and V Complex extraction of matrix in organic solvents and determination of impurities in aqueous phase; ppb detection limits The Pd Pt and Ru were isolated in turn by extraction with three different organic solvent systems and Ir remained in the aqueous phase Direct sample introduction of pyrophoric gases using specially designed five inlet ICP torch.(Detection limits reported at low ppb levels) bromine water; arsenic eliminated by evaporation and gallium by extraction; impurities Ba Co Cr In Ni Te and Zn dopant determined in resultant aqueous phase Separation of Bi Cd Cu Fe Mg Mn Ni Sr and Zn from matrix by pre-concentration on cellulose Hyphan collector and elution with 2 mol dm-3 HC1.(Detection limits 10-250 ng g-I) Extraction chromatography using HDEHP on PTFE with 0.5 mol dm-3 HNO elution or TBP on PTFE with 0.5 mol dm- HBr to separate radionuclides of impurity elements from those of the matrix methods for determination of As Cr Cu Fe Ge Ni and Sb impurities; accuracy assessed by NAA Quantification of ten dopant elements using caesium primary ion beam Sample decomposed with mixture of HCl and Comparison of acid decomposition and fusion Various (6) Silicon wafers XRF;-;S 91/147 Various (1 7) Trimethyl gallium and trimethyl aluminium AE;-;L AA;ETA;L MS;ICP;G AE;ICP;L 9 1/345 9 1/397 9 1lC760 911919 Various (4) Silicon Various (30) Electronic-grade gases Various (7) Gallium arsenide Various (9) High-purity gallium AE;ICP;L 9 1 /C940 Various Indium NAA 91lC1733 Various (7) Silicon MS;ICP;L SIMS 9 1/C 1736 9 112269 Various (10) Gallium arsenide and indium phosphideJOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY DECEMBER 199 1 VOL. 6 309R Table 3 SUMMARY OF ANALYSES OF ADVANCED MATERIALS-continued Element Various (1 1) Various Various (20) Various (5) various Various Various (6) Technique; atomization; Matrix analyte form* High-purity silicon AE;ICPL Silicon on insulator XRF-;S High-purity cadmium AE1CP;L and zinc High-purity gallium AA;ETA;L Gallium indium and AEiICP- bismuth compounds High-purity gallium ESCA or High-purity gallium M,ETA;L MS;spark;S Various (24) High-purity tellurium Various (1 9) Molybdenum disilicide GLASSES- Al Pharmaceutical glass containers B Borosilicate glasses c o Commercial glass Cr Commercial glass c u Zirconium fluoride Er Optical fibre precursors Ge Glass optical fibre Ni Zirconium fluoride P Glass optical fibre REE ( 14) NIST SRM 6 10 Glass REE NIST SRMs 610 6 12 and 6 14 Glass Various (6) NIST SRMs 6 10 612 614 and 1003a Glass Various Opaque red glass MS or AA,spark or ETA;S AA or AE;ETA or 1CP;L AA;ETA,L x-ray emission;-;S AE;ICP;S AE;ICP;S AA;ETA;L AE1CP;L AE;DCP;S M;ETA;L AE;DCP;S MS;spark;S SIMS AA,ETA,L Electron probe or AE1CP;L Sample treatmentlcomments Pressurized dilution of the sample in dilute HNO,; recoveries for Al Ba Ca Cu Fe K Mg Na Pt Si (as oxide) and Zn were in the range 96-1 10% heavy metals on sample surface chromatography with trioctylamine and tributyl phosphate-PTFE using HCl elution Extraction of Cd Co Cu Fe and Ni as pyrrolidine dithioformates into IBMK in the presence of tartarate Direct technique described with limits of detection at the sub-ppm range; error of 15% reported Trace element residues determined at 10- lo0 ppb level Gallium in the matrix was converted into trichloride and volatilized by gaseous HCl; residual impurities (Al Cd Cu Fe Mg and Pb) were dissolved in 0.25 mol dm-3 HNO and determined at ng g-I level sieved to a grain size of 100 mesh and homogenized in an inert atmosphere in a shaker; powders were mixed to provide a concentration range; AAS results used to provide relative sensitivity factors for SSMS Sample was dissolved in HF-HN0,-H,SO diluted and passed through a Dowex cationexchange column to remove the matrix and analytes were eluted in 2 mol dm- HNO Total reflection X-ray instrument used to detect Acid digestion in autoclave followed by extraction Samples (pure and impure) were powdered and Samples were heated in an autoclave for 1 h at 120 "C; aluminium released into distilled water measured at 5 ppb spectrometry was used to measure B.(Detection limit of 20 ppm reported) introduced to the ICP as a slurry; detection of inorganic colourant Low-energy electron-induced X-ray emission Samples were ground dispersant added and As for Co Analysis of 30% m/v solutions for Cu using Zeeman- effect background correction and platform atomization.(Detection limit of 3.2 ng g-I Cu reported) High-temperature disgregation of the sample was adopted; wavelength of detection was 337.376 nm. (Detection limit of 0 . 0 3 ~ ml-l was reported) Direct insertion of fibre via feed mechanism beneath plasma base; recoveries in the range 107- 1 16% for approximately 250 ppm of Ge As for Cu. (Detection limit of 6.3 ng g-I of Ni reported) As for Ge; recoveries for P at 335-805 ppm level were in the range 100-1 10% Powdered standard was briquetted with equal mass of graphite and analysed using %i as an internal reference Quantitative analysis for REEs using relative sensitivity factors for calibration Materials were powdered and suspended in 3% vlv HF solution; matrix silicon is removed as fluoride and analyte is extracted into aqueous phase for detection of Cu Co Cr Mn Fe and Ni Microanalysis of solid for major and minor elements of lead silicate glasses coloured by copper(1) oxide Reference 9112380 91t2589 9 1 lC2877 9113240 9113261 9113389 9013980 9014007 9014023 91lC1715 9 1lC1806 9 llC2922 9 1x2922 91189 9 1lC2926 911874 91189 911874 9 1/22 1 5 90x4045 911196 9 11932310R JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY DECEMBER 199 1 VOL.6 Table 3 SUMMARY OF ANALYSES OF ADVANCED MATERIALS-continued Technique; atomization; analyte form* XRF;-;S Element Matrix Various Glass fragments Sample treatmenthmments Energy dispersive XRF with lateral resolution of 0.3 mm was used in SEM to identify small glass fragments Samples of ZrF were decomposed by evaporation with H,SO and dissolution in dilute HNO,; BaF and LaF were decomposed by HClO and dissolved in HCl; AlF was fused with sodium carbonate and dissolved in HC1 with H,O Samples were powdered and surface contamination cleaned using HCl; samples dissolved in HF-HCl then HClO and diluted to volume with HC1 Acid leachates were analysed for the presence of alkali metals and alkaline earths in order to study corrosion effects identification of glass fragments (by detection of Ca Fe Sr and Zr) and ICP for ten elements using dissolution Direct quantification of bulk and trace elements with a spatial resolution of better than 10 pm.(Detection at the low ppm level) techniques for determination of contaminants at the sub-ppb level Comparison of energy dispersive XRF for A survey of sample preparation and use of the above Reference 911962 9111251 9111427 lC1741 lC2036 9112323 9 113396 Various (4) Zirconium fluoride glass precursors M,F;L Various (48) Window glass fragments MSICPL Various Stained glasses AA or AE;-;L Various (10) Glass fragments XRF or AE1CP;S or L Various Alkali-borosilicate glasses SIMS Various Metal fluorides and fluoride glasses AA or MS;ETA or 1CP;L CERAMICS AND REFRACTORIES- Al Tungsten oxide B Boron carbide AA ETA L Sample was decomposed with ammonium citrate Sample loaded in the form of a slurry; detection of H,O and ammonia; sensitivity reported as 15 pg the dicaesium metaborate cation to determine isotope ratio Sample dissolved in HNO and Ba measured to sub- ppm levels without interference at 455.03 or at 493.409 nm when europium or terbium oxides were present Use of HCl and HNO treatment to distinguish between phases of differing chemical composition Detection of Br as indium chloride after introducing indium as an indicator metal into hollow cathode discharge Sample powder of sub-pm particle size was dispersed ultrasonically in water and the slurry introduced into the ICP; C was detected at 193,091 nm producing high count rates for light elements such as C same ion was used for bombardment; C emission yield used for quantification Separation of Cd using strong cationexchange resin and elution with 5 mol dm-’ HCI and ultrasonic desorption Use of layered synthetic microstructures for Caesium ions were implanted in the films and the As for Br 9 113004 9119 MS; thermal ionization;S Ba Rare earth oxides AE1CP;L 9 11 1008 Ba Br Superconductor Aluminium oxide 9 112 1 57 9 11347 AEF;L Molecular emission; HC,S Silicon nitride AE;ICP;S 911108 C C Superconductor films Electron micro probe 911122 C Titanium carbide films SIMS 9112267 Titanium dioxide AA;ETA;L 9113 107 Cd Aluminium oxide Molecular M F L XRF;-:S emission;HC,S 9 1 I347 c u c u Superconductor Superconductor 6lms As for Ba Standardization procedure for determination of Sample introduced into the atomizer as a 0.25% m/v Cu:Ba and Cu:Y ratios in oxide films slurry of powder in ethanol-water (9+ 1); measurements at 294.4 nm ion-exchange resin; detection at 356.166 nm using standard additions in the range 6- 1000 ppm Separation of Hf from matrix using Ag 1-X8 Biorad Wavelength dispersive instrument used to detect Hf 9 1121 57 9 113098 Aluminium oxide AA;ETA;L 911845 Ga Hf Zirconium oxide AE;ICPL 9 113 141 Hf Zirconium oxide XRF-;S 9 113296JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY DECEMBER 199 1 VOL.6 31 1R Table 3 SUMMARY OF ANALYSES OF ADVANCED MATERIALS-continued Element Matrix K Tungsten oxide Na Tungsten oxide Nd Ceramic pigments Pb Superconductors Pb High-purity yttrium oxide Sr Rare earth oxides V Zirconia Y Superconductor Y Yttria stabilized zirconia Zr Hafnium oxide REE (1 4) Thulium oxide REE (8) Europium oxide Technique; atomization; analyte form* AA;FL AA;€L AE or XRFFL or S AE;ICPL AA,FHy AEICP;L AEICP;L AERL AEICP;L XRF-;S AE;ICP;L AE;ICP;L REE (1 4) High-purity europium oxide XRF;-;S Various ( 16) Zirconium carbide and nitride AE;ICPL Various (5) Aluminium oxide-chromium AEICP;L oxide powders Various (22) Barium titanate AEICP;L Various (4) Superconductor AA;FL Various Ceramics AE;arc;S Various (1 1) Rare earth oxides AE; d.c.arc;S Various (9) Barium titanate Various Superconductors AA or AE; F or 1CP;L AE;ICPL Various (7) Aluminium nitride AE;ICP;L and zirconia Various (8) Refractory SRMs AE;ICPL Various (7) Zirconium oxide AE;ICP;L Sample treatmentlcomments Sample was dissolved in ammonia cooled HNO caesium chloride and then citric acid and water added; K was determined in the supernatant liquid As for K Samples were either dissolved in HCl diluted and analysed using N,O-C,H flame or pelletized for XRF Speciation of PblV by recovery of insoluble residue; Pb" determined by difference from total Pb content Generation of hydride with sodium tetrahydroborate; RSD of 1 1% for measurement of 2 ppm of Pb As for Ba; Sr measured at 421.552 or at 407.771 nm in the presence of europium oxide Solvent extraction of V using potassium butyl xanthate in pH range 0.009-2.5 As for Ba Powders were decomposed with H,SO under pressure Powdered sample was pressed into a pellet and and diluted with 10% vlv HCl analysed by WDXRF with a tungsten anode tube and lithium fluoride crystal (Zr measured in the range 0.0 1-4%) Effect of organic solvents studied recoveries in the range 82-1 10% reported and RSDs of 1.9-9.3% Optimization of instrumental parameters to minimize interferences in detection of Ce Dy Gd La Nd Pr and Sm Impurities detected by reduction with zinc powder adsorption by P507 levextral resin elution with HCl and precipitation with ammonia; measurement on filtered precipitate limits in the ppb range; comparison with AAS data The powder was dissolved under pressure in 5 ml of H,SO and diluted with water to 100 ml and analysed for Ca Fe Mg Na and Ti Pressure decomposition of sample with HC1 or fusion with sodium carbonate or lithium borate; detection of majors and 20 impurity elements Examination of inter-element interferences in determination of Bi Ca Cu and Sr; effects removed by addition of sodium chloride Preparation and analysis of standard materials for spectral analysis based on ceramic oxides of Al Si Y and Zr containing also Ca Fe Mg Na and Ti as impurities signals in determination of trace elements in rare earth oxides Microwave assisted digestion of sample in HCl followed by extraction with APDC with chloroform and re-extraction into HNO yttrium-barium-copper oxide.(Al Mg and Zr found at levels between 50 and 250 ppm) Study of sample preparation and selection of suitable instrumental parameters for determination of Al Ca Fe Mg P Si and Ti development of methodology for detection of Al Ca Fe Mg Mn S Si and Ti pressure evaporated to dryness with HC10 and diluted with water prior to determination of Al Ca Cr Fe Mg Ti and Y Samples were digested in HNO and H F detection Study of effect of chloride salt carriers on emission Determination of contaminants in Introduction of samples as 1% m/v slumes; Powdered sample was dissolved in HF under Reference 9 11 1480 9 111480 9113284 9113159 911414 9 11 1008 9112539 9112157 9113031 9113174 911392 9 11 1024 9 111226 91180 91183 91197 9 11222 911270 9 11393 9 1 lC483 9 11C549 9 1 I836 911864 9111015312R JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY DECEMBER 199 1 VOL.6 Table 3 SUMMARY OF ANALYSES OF ADVANCED MATERIALS-continued Technique; atomization; analyte form* AE;ICP;L Element Matrix Various (6) Superconductors Sample treatmentlcomments Samples were dissolved in HCl and an internal standard added Nitrides were digested under pressure using acid and zirconia was decomposed by carbonate-borate fusion A method for preparing standards containing Co Cry Cu Fe Mn Ni and Pb as impurities to pure matrices was described for calibration of instrument for analysis of refractories Fe Mn Ni and Pb using diethyldithioformate and CCl with recoveries >90%; detection by Pre-concentration and extraction of Cd Co Cr Cu ETV-ICP-OES Precipitation of Co Cu and Ni by addition of 142- pyridiylazo)-2-napthol and separation from tungsten by complexation with ammonia Measurement of major constituents including Ba Bi Ca Cu Pb Sr and T1 by dissolution in HNO Precision of better than 5% reported for quantification of Cay Fe Na S Si and T1.(Detection limits at 10 ppb level for 30 s integration) Major components Ba Bi Ca Cu Pb Sr and T1 in a variety of materials Quantitative elemental profiling in Bi-Sr-Ca-Cu-0 layers for majors minors and traces Comparision of sulphated decomposition and acid dissolution with carbonate-borate and lithium borate fusion procedures determination of Co Cu and Ni by addition of sodium docecyl sulphate effect decomposition for determination of Mo Ti V and Zr Direct examination of sample deposited on thin Mylar sheet provided ng level detection using PIXE but poorer sensitivity by EDXRF Comparison of fusion extraction and slurry methods; calibration by standard additions; good agreement for Al Ca Fe Mg Na Ti and Y using slurry method Laser ablation sample introduction for both sources in determination of Dy Er Eu and Yb Pressure dissolution of sample in HN0,-HF-fuming H,SO for 8 h followed by AAS or direct analysis of a 1% d v aqueous slurry by ICP-OES Optimization of instrument conditions and selection of wavelengths for detection of La Pb Ti and Zr and many impurities IBMK.(Detection limits in range 1-10 ppm and Elimination of interference from tungsten on Samples were heated in an autoclave with HF to Detection of Dy Eu Sm Tb and Y in 30% vlv RSDs 2.6-5.3%) Sample fused in caustic-peroxide and dissolved in HCl and detection of Ca Fe and Mg at 422.7 248.3 and 285.2 nm respectively Method described for determining the composition of thin films of superconducting materials Fundamental parameter method used to detect Al Ca Fe K Mg Na Si and Ti present as oxides Quantitative analysis for Ba Cu 0 and Y using a matrix correction procedure Use of 20% NaF as carrier enhanced spectral intensities by inhibiting evaporation of tungsten trioxide dissolution in dilute HC1 addition of lanthanum and coprecipitation as hydroxide then redissolution of solid and analysis by ICP-AES Fusion of sample with nitrate and carbonate then Reference 9111 161 AE;ICP;L Various Boron and aluminium nitrides and zirconia 9111 171 Various (8) Refractory borides carbides and nitrides XRF;-;S 9111217 Various (8) Lanthanum oxide AE;ICP;L 9111340 Various Tungsten oxide 9111473 AA;F;L Various (6) Superconductors Various (6) Alumina powder AA or AE;F or 1CP;L MS;GD;S 9 111 60 1 9 1 IC 1 654 Various (7) Superconductors AA or AE;F or 1CP;L SIMS AE;ICP;L 91lC1725 91lC1728 9 1 IC 1754 Various (10) Superconductor Various (1 5 ) Calcia partially stabilized zirconia Various Tungsten oxide AA;F,L 9112370 Various (4) High-purity alumina AE;ICP;L 9 112409 XRF or PIXE Various Superconductors 9112588 Various ( 10) Zirconium dioxide AE;ICP;L or S 9 llC28 1 3 Various (4) Yttrium oxide Various Silicon carbide AE;ICP or FANES$ AA or AE;ETA or 1CP;L or S 91lC2867 91lC2892 AE;ICP;L 9 1 lC29 1 9 Various (29) Ceramics Various ( 5 ) Gadolinium oxide AE;ICP;L 13010 13093 I3 134 13360 Various Silicon nitride AA,F;L Various Superconductors Various (8) Alumina-silica refractory Various (4) Superconductor Various (28) High-purity tungsten trioxide AE;ICP;- XRF-iS Electron probe AE;d.c.arc;S 9113364 9 113498 Various ( I 1) Silicon nitride AE1CP;L 9014025JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY DECEMBER 199 1 VOL. 6 313R Table 3 SUMMARY OF ANALYSES OF ADVANCED MATERIALS-continued Element Matrix CATALYSTS- c1 Reforming catalysts c o Boron modified cobalt- alumina catalysts Pt Reforming catalysts Pt Aluminium oxide Pt Molecular sieve catalyst Rh Catalysts Various Catalysts and alumina support Various (1 6) Zeolite fluid cracking catalysts Various (4) Heterogeneous catalysts + REE Technique; atomization; analyte form* Sample treatment/comments XRF-;S EXAFS XRF-;S AA;ETA;L M F L AE;ICP;L M F L AE;ICP;L AA;FL Energy dispersive instrument with rhodium target modified with an aluminium foil filter; calibration using external catalyst standard amounts of colbalt oxide and cobalt surface phase on catalyst Matrix correction for absorption used in quantification of Pt The sample was boiled with aqua regia washed and diluted with HCl then precipitated with tin(I1) chloride washed digested in aqua regia and diluted Pressurized digestion in aqua regia-HF and addition of copper sulphate solution; detection at 265.9 nm Solvent extraction of Rh with potassium hexyl xanthate into xylene; interference of nickel avoided by preextraction with butyl xanthate The A1 matrix was masked with potassium oxalate and Cd Cu and Pb were separated by adsorption on sulphydryl cotton and re-eluted with HC1 Acid digestion using ‘Spectrasol’ reagents which deactivate HF without using boric acid Microwave digestion of samples under pressure using HN03-H3P04 for detection of Co Fe Mo and Ni Cross correlation analysis used to detect relative Reference 9 113295 9 112966 91156 911453 9112381 91185 9 11 1093 9 1 lC2093 91/2471 *Hy indicates hydride generation and S L G and S1 signify solid liquid gaseous or slurry sample introduction respectively.Other abbreviations are listed elsewhere. investigation of polymer systems included a study of the reactive selectivity of oligomers in polyglycol samples to alkali metal ions (91/2179) and the application of an FTMS instrument for full mass range scanning on a single laser shot (91/2169). Laser ablation has also been used as a means of introducing polymeric materials to an ICP-MS instrument (91/C751 91/C1629 91K1923). A detailed report on the application of laser ablation ICP-MS to the analysis of a range of filled and unfilled plastics has now been published (9113205). It was reported that semi- quantitative analysis of polypropylene nylon poly(viny1 chloride) polyethylene and polyester could be achieved with an accuracy of a factor of two or better by ratioing to carbon as an internal standard.Quantitative analysis achieved employing calibration standards yielded good agreement with results obtained using other techniques such as WDXRF and NAA. The influence of instrumental parameters on the analytical performance which can be achieved by laser ablation ICP-MS has also been studied by the same workers (91/C820). It was found that the position of the beam focus had a considerable influence on both the magnitude of analyte intensities and the precision obtained. It was considered that operating the Nd:YAG laser at a focus about 10 mm above the surface of the polymer sample yielded best precision and results consistently below 1 Ooh RSD could be achieved for elements in the mid-ppm concentration range.Laser ablation has also been used in conjunction with ICP-AES for the analysis ofpolymers and paints (9 1 / 104). A graphite furnace was incorporated in the ablation chamber which allowed the electrothermal pre-treatment of samples prior to evaporation using the laser. Emission signals were detected using a multi-element emission spectrometer. The system was used for qualitative scanning or survey analysis but quantification was hindered by a lack of calibration standards. Paints were also examined directly using XRF (9111 182 91/C1719 9113506) and electron probe micro- analysis (9 1/1168). Results of a collaborative trial evaluat- ing the precision of an official method for the determination of total and soluble Pb content of dry paint films have been published (9 1/1039).British Standard chemical tests for the analysis of raw and vulcanized rubber by FAAS published in the last year may also be of interest (9 1/3 1 16 9 1/3 1 17). Traditional methods of sample preparation for the analy- sis of plastics such as ashing or wet oxidation are relatively slow and can be subject to losses particularly for the determination of volatile elements in a matrix such as poly- (vinyl chloride) (PVC). One alternative is to make use of the organic nature of the polymer by using a dissolution approach (see J. Anal. At. Spectrom. 1990 5 347R). This involved treatment of the PVC sample with dimethyl formamide and adding a few drops of acetic acid and then diluting with acetone prior to analysis by FAAS.This pre- treatment has now been used for the determination of Cd and Pb in PVC using ETAAS (91113) and Sn in PVC by both FAAS and ETAAS (91/94). In a related approach Zn was determined in plastics by FAAS following treatment of the sample with IBMK and Brij-30 an emulsifier. The resultant oil-water emulsion formed was found to be sufficiently stable to be introduced directly into the flame. The method was suitable for the determination of Zn in the range 0.1 to 1 ppm. Glow discharges have as yet not been applied to the analysis of polymeric materials owing to difficulties in sustaining the plasma with non-conducting samples. The use of r.f. supported discharges obviates the need for a conducting sample allowing the direct analysis of insula- tors (911C2799 91/C2800,91/C2850). It is to be hoped that such developments will continue allowing the depth profil- ing capability of the GD to be used in the examination of314R JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY DECEMBER 199 1 VOL.6 polymers. The related technique of sputtered neutral MS offers a similar potential (9 l/C278 1). A few abstracts were received concerning the application of SIMS to the study of polymeric systems. The distribution of Mg and As ions in polyimide were determined experimentally using SIMS (91/2341). The surface of a polycarbonate material was treated using a carbon tetrafluoride-oxygen plasma dis- charge and the surface of the sample examined by SIMS and XPS (9112324). It was found that with very low amounts of oxygen in the gas feed extensive fluorination of the surface occurred and perfluorinated islands were formed.How- ever under conditions of high oxygen supply very low amounts of fluorine only were observed on the surface of the polycarbonate and etching took place. The use of a DCP discharge cleaning method to eliminate background from perfluorinated polyalkylethers in SIMS analysis may also be of interest (91/2302). 3.2. Semiconductor Materials Interest in the development of new or improved methods for the analysis of semiconductor materials remains high with over 100 abstracts received for the period under review. Of these the great majority (>60) were concerned with the characterization of silicon-based materials. Several review articles which discussed the available spectro- analytical techniques and their relative merits in applica- tions from the electronics industry may be of general interest (91/281,91/282,91/1075,91/2272).A survey ofthe use of the AA AE SSMS NAA and laser techniques for the analysis of high-purity germanium has also been published (9 112407). Undoubtedly SIMS remains an indispensable tool for the characterization of semiconductor materials. A general overview of the potential of SIMS for the analysis of very large scale integrated silicon devices is highly recommended (91/2366). One of the major problems in the application of SIMS remains that of correlation of ion response with concentration (i. e. quantification). Progress towards iden- tifying a suitable semiconductor standard for quantification has been assessed (9014 1 36).A three-stage implantation of 2sSi followed by loB implantation at 50 keV was reported to produce a material with a smooth B depth distribution. Low dose energetic ion implantation has also been pro- posed as a method for depth scale calibration in SIMS (9 1/2280). However it was considered that implantation conditions including species and energy had to be optim- ized for the particular problem. Calibration is particularly problematic as the complexity of multi-layer systems grows. An analytical method for the quantitative depth profiling of titanium-silicon multi-layer samples has been published (91/2301). In this approach a processing algorithm con- verted the dopant (B or As) intensity time profile into concentration by applying sensitivity factor and sputtering rate corrections for each layer.The use of the depth projling capability of SIMS has been reported in a range of applications. The nature of hydrogen- ated silicon films on chromium gallium arsenide and titanium substrates have been examined using SIMS with oxygen bombardment (9 1/228 1). The interf'ace between the film and the substrate was examined by changing the angle of the primary ion beam. Boron-doped hydrogenated silicon was examined by SIMS (9 112333) and sputtered neutral MS (9 1/2346). Several publications were devoted to SIMS depth profiling of silicon-germanium layers (91/2279 91/2295 91/2348) the latter of these being hydrogenated. The application of a new type of sputtered neutral MS to the depth profiling of germanium-silicon multi-layers was also described (9 1/2271).It was claimed that this new system labelled SNART offered high sputter- ing rates with minimal matrix effects post-ionization and as a consequence accurate quantification. The character- istics of silicon-silicon oxide layers were determined by using a gallium ion liquid metal ion source as the primary beam to trace the yield of implanted gallium (91/2265). Gallium was found to be a good marker for thin oxide layers at a silicon-silicon interface and the technique gave improved spatial resolution. The accumulation of Fe at the silicon-silicon dioxide interface has also been studied by SIMS (9 1/2299). Other applications reported included the use of SIMS to assess distribution of Cu and Ga in silicon using oxygen bombardment (9112276) and a study of Er implanted in silicon before and after rapid thermal anneal- ing (91/2325).There was considerable interest in the application of electron microscopy to the characterization of silicon-based materials. The advantage of techniques such as SEM is that it is possible to obtain two-dimensional information (lateral and depth profile) at high resolution (9112308). Thus dopant As concentrations were delineated in shallow regions of a silicon sample using an HF etching procedure followed by cross-sectional SEM examination. A relative positional accuracy of 15-20 nm was claimed. In a similar study one- and two-dimensional dopant profiles were obtained for p-n junctions in etched silicon specimens using both scanning and transmission electron microscopy (91/2309).The SEM method was applied to diodes with junctions 2 pm deep and the TEM approach devoted to fully processed bipolar transistors with junctions 130 nm deep. The profiles obtained were found to be in good agreement with SIMS data. Indeed TEM can be used to study surface alterations on silicon wafers induced as a result of SIMS analysis (9 112306). Oxygen bombardment of the surface at 4.5 keV of a silicon sample was found using TEM to produce an amorphous layer 20 nm deep. An accumulation of As at the altered layer was found following SIMS profiling of an As doped sample. This approach is also useful in the study of residual damage in silicon wafers following dopant ion implantation (9 112307). The effect of boron difluoride implantation was studied using TEM and Raman spectroscopy.It was found that the distribution of B and F and the residual morphological damage had a significant effect on the electrical properties of the im- planted layer. Other applications of TEM reported included a study of the dopant profiles of B and P implants in silicon (9 1/2305) silicon oxynitride implanted layers (9 1 /23 lo) As and B doping of titanium silicide (91/2311) and Co implantation in silicon (9 1 /23 12). There were relatively few reports concerning the applicu- tion of GD-MS to the analysis of silicon-based semiconduc- tors and very little indication of conference presentations of previous years finding their way into the primary literature. A GD instrument using a quadrupole mass spectrometer was shown to be able to detect Gd in a metallic thin film on a silicon wafer (91K1778 91K2109). The use of cryo-cooling of the ion source was claimed to minimize interferences allowing the use of a lower resolu- tion detector.A few papers were published concerning the use of XRF for the direct analysis of impurities in silicon wafers (91/147 91/164 91/2589). A review of the prin- ciples and applications of XRF using the total reflection geometry is recommended to those with an interest in this field (9 1 /2400). Inductively coupled plasma mass spectrometry continues to find application in the determination of impurities in silicon (91K1736) and in electronic grade quartz (91/111). There have been some interesting developments in the direct analysis of electronic-grade reagents by ICP-MS.A number of precursor gases used in semiconductor pro- duction are pyrophoric and in the case of silane are also toxic (91/958). Thus a gas handling rig was constructed which allowed the accurate mixing of argon 1% silane andJOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY DECEMBER 199 1 VOL. 6 315R gas standards for the determination of As (25 ppm v/v arsine in argon) and I (25 ppm v/v methyl iodide in argon) and this was connected directly to the central injector of the ICP torch. Standardization was achieved via dilution of the arsine and methyl iodide standard gas mixtures on line. Quantification was also achieved by ratioing analyte inten- sities to that for the silicon matrix which was used as an internal standard. Detection limits for As and I in silane were given as 0.55 and 0.65 ppb respectively.A high- temperature aerospace alloy was used to fabricate the MS sampling cone to reduce deposition of the refractory matrix. The cone glowed a dull red colour during operation and it was found that signal integrity could be maintained for longer periods using this modification. The use of a low- pressure MIP torch was also found to eliminate orifice deposition in this type of analysis (911C1628). In another approach to the same problem a five-inlet ICP torch was designed for the analysis of pyrophoric semiconductor gases (911C760). Detection limits for over 30 elements were reported at ppb levels. The detection of Fe by ICP-MS is well known to be limited by the spectral background from argon oxide.The use of ETV for sample introduction to the ICP-MS has been shown to remove this interference (911C1617 911C1897). The detection limit for Fe in the analysis of high-purity semiconductor-grade acids was reported to be of the order of 10-20 ppt using this technique. It was implied that further improvement in the detection limit could be made by using a magnetic sector instrument instead of a quadrupole mass filter but no details were given in the abstract. Applications of ICP-AES to the determination of trace elements in high-purity silicon (91/2380) and in molyb- denum disilicide (9 112380) have been described. However there was little work of any great novelty reported in the year under review using ICP-OES. These comments also apply to developments in AAS where relatively few applications merit comment.Graphite furnace applications involving the determination of platinum group metal dopants in silicon (91/397) impurities on the surface of silicon wafers (911464) and trace impurities in molyb- denum disilicide (9014023) have been reported. A review of the principles of laser AAS and its application to the determination of concentration profiles of Bi Pb and Ru in thick multilayer electrical structures may be of interest (9 1/95 1). The characterization of gallium arsenide-based semicon- ductors using AA and AE techniques was the subject of a recent review (9 113303). However there were relatively few abstracts received relating to these techniques for the analysis of gallium based semiconductors in the year under review and only some of these are worth highlighting. The determination of impurities and dopant concentrations in zinc-doped gallium arsenide by ICP-OES has been reported (91119).The sample was treated sequentially by cleaning and decomposition with hydrochloric acid and bromine water and elimination of matrix elements by evaporation of arsenic and extraction of gallium. A range of analytes including Ba Co Cr In; Ni Te and Zn were determined in the aqueous phase resulting from the sample preparation stage. Detection limits were reported to be in the ng g-l range. Trimethyl gallium is an important precursor in semiconductor manufacture but is difficult to analyse because of its pyrophoric nature. A separation process was proposed based on the conversion of gallium into a chloride form by treatment with 6 mol dm-3 hydrochloric acid (91/345).The reaction was carried out in a Fluoroplast reaction vessel in an inert gas atmosphere. Impurities were separated from the matrix by extraction of HGaCl with oxygenated solvents. A reducing agent such as hydrazine or ascorbic acid was added to prevent coextraction of Fern and Zn. After separation of the Ga the remaining aqueous phase was heated to dryness and the vessel washed with hydrochloric acid. The resulting solution was then analysed by AE for the determination of Al Ba Ca Cd Co Cr Cu Fe K Mg Mn Na Ni Si Ti V and Zn. Detection limits in the ng g-' range were reported. The detection of trace element impurities in high-purity gallium has also been carried out using separation-extraction procedures.A num- ber of analytes including Cd Co Cu Fe and Ni were extracted as pyrrolidinedithioformates into IBMK in the presence of tartarate (91/3240). These elements were then detected in the extract by ETAAS. The advantage of the method was considered to be low experimental blanks made possible by the one-step matrix removal and pre- concentration procedure. In a different approach Ga was volatilized as the trichloride following treatment with gaseous hydrogen chloride (90/3980). Residual impurities were dissolved in 0.25 mol dm-3 nitric acid and were detected using ETAAS. Recoveries obtained by this method were in the range 92-105% for Al Cd Cu Fe Mg and Pb. Detection limits were given in the 1.5- 1 1 ng g-l range. The advantage of this method was reported to be a reduction in the risk of contamination.Mass spectrometric techniques continue to be employed for the analysis of high-purity gallium and related materials. For example RIMS has been used in depth pro$Zing of doped gallium arsenide and aluminium gallium arsenide layered structures (9 11C625). Quantification was made possible by normalizing dopant signals to that of the matrix assuming similar sputter rates. Laser ablation RIMS using a time of flight mass spectrometer has been utilized for the detection of As Ca and Ga in an aluminium gallium arsenide sample (9 1/2289). Improved sensitivity of several orders of magnitude was achieved by tuning the ablation laser to match the resonant atomic transitions for As and Ga using the same dye laser. Spark source MS is an extremely sensitive technique for the analysis of gallium- based semiconductors.The distribution of trace element impurities in high-purity gallium was studied by SSMS (91/3389). It was found that trace elements could be detected in the range 10-100 ppb using this technique. A radiofrequency spark source MS system was applied to the determination of semi-insulating gallium arsenide and its precursors (911C1738); samples were sparked under ultra- high vacuum using a pulsed voltage generator. The resultant ions were focused onto an ion sensitive Q-plate by means of electrostatic and magnetic sectors. Mass spectra were interpreted using a computerized optical microdensito- meter. It was reported that microphotometric measurement of dopants and residual impurities allowed reliable semi- quantitative analysis with an accuracy of 20%.In undoped gallium arsenide only B and 0 were detected as residual impurities. Surface analysis techniques such as secondary ion mass spectrometry (SIMS) continue to be applied to the charac- terization of gallium-based semiconductor materials. Car- bon- l 3 doped aluminium gallium-aluminium gallium ar- senide superlattices were subjected to impurity induced disordering by silicon and zinc and the resultant materials were examined by SIMS (9 112349). The modulation depth of the SIMS "Al and 13C signals was used as a probe of sublattice interdiffusion. Both silicon and zinc were found to enhance carbon diffusion in the matrix. The description of a focused ion beam which is claimed to combine the capabilities of ion microscopy ion lithography SIMS and ion milling in a single instrument is likely to be of general interest to workers in the semiconductor field (9112303).The system was applied to a SIMS scan across a gallium arsenide-aluminium gallium arsenide heterojunction. Gal- lium and indium phosphide materials have also been examined by SIMS. Examples reported included the analy- sis of gallium arsenide-gallium arsenide phosphide layered316R JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY DECEMBER 199 1 VOL. 6 structures (91/2270) and a study of ion yield in the measurement of ten dopant elements in gallium arsenide and indium phosphide materials (9 1/2269). Studies involv- ing plasma secondary neutral MS indicated that the elemental sensitivity factors found in the examination of gallium arsenide gallium phosphide and indium phosphide materials were dependent on mass differences of the components (91K2851).It was reported that the relative sensitivities could be less than one order of magnitude for masses of less than 100. New methods for the analysis of cadmium mercury telluride and precursors continue to be proposed and these are summarized conveniently in Table 3. The role of analytical techniques in the study of matrix components and impurities in cadmium mercury telluride was discussed in a review (91/3390). Amongst the techniques considered were AAS XRF SSMS LMMS and SIMS. The last has been used in depth profiling of impurities in layer grown cadmium mercury telluride (9112275). Layer by layer analysis of the main components in cadmium mercury telluride has been carried out using an oxidation and etching process followed by AF detection (91/1104).The high sensitivity of AF for the determination of Cd Hg and Te coupled with the use of ETA allowed a depth resolution of 10 nm to be achieved. An AA method was also described for the layer by layer determination of impurities in cadmium mercury telluride (9 1/924). Layers were removed using 2.5% bromine in 4 mol dm-3 hydrobromic acid. A Zeeman-effect background corrected ETA method was proposed for the detection of Bi and Cu in 5 mg layers. Detection limits in the sub-ppm range were reported. A Zeeman-eflect background correction system was used to good effect in the direct determination of In in solid indium cadmium mercury telluride by ETAAS (9 1/429).A zircon- ium coated platform was used which was reported to eliminate interferences from halides. Indium recovery was in the range 94-108% and the RSD was less than 6% for the method. A comparison of the relative merits of ETAAS SSMS and GDMS for the analysis of high-purity tellurium may also be of interest (9014007). 3.3. Glasses Ceramics and Refractories 3.3.1. Glasses A review by workers from NIST on the characterization of high-purity metal fluorides and fluoride glasses has been published (91/3396). Emphasis was given to aspects of sample preparation for these materials and methodology associated with ICP-MS and ETAAS detection of elemental impurities at the sub-ppb level. A graphite furnace AA instrument with Zeeman-effect background correction was used for the detection of Cu and Ni ppb levels in zirconium fluoride (91/89).The sample was introduced to the instru- ment as a 30% m/v solution of zirconium fluoride. Palladium nitrate and nitric acid were used as chemical modifiers in conjunction with platform atomization which helped protect the tube from erosion. The technique was validated by recovery experiments and by the use of the standard additions procedure. Detection limits for Cu and Zn were reported to be 6.3 and 3.2 ng g-l respectively and RSD values were typically less than 10%. A slurry extraction method was developed for the analysis of glass materials by ETAAS (9 1/ 196). Samples were powdered and suspended in water containing 3% hydrofluoric acid.The slurries were prepared in autosampler cups and were agitated by passing argon gas through the solution which served to mix the slurry and remove the matrix as silicon tetrafluoride. Analyte metals such as Co Cr Cu Fe Mn and Ni were extracted into the aqueous phase of the slurry. A range of NIST glass standards were analysed using the method and the results compared with a conventional digestion procedure. Inductively coupled plasma emission spectrometry has also been used in conjunction with slurry sampling metho- dology for the analysis of glasses (9K2922). The glass samples were ground and introduced to the plasma in the form of an aqueous slurry stabilized by the addition of a dispersant. Factors such as the particle size the amount of suspended solids present and the influence of different dispersing agents were studied.One of the advantages of ICP-OES compared with AAS for this type of analysis is that data can be rapidly gathered on a multi-element basis. Thus it is possible to use this information to discriminate the source of glasses by elemental fingerprinting (91K2036). In this study 81 samples of automobile side glass windows were analysed by ICP-OES using a sample dissolution procedure. It was found that the levels of at least ten elements detected by ICP-OES allowed identification of the source of the glass. It is possible to use ICP-MS for elemental fingerprinting of glasses (see J. Anal. At. Spec- trom. 1990 5 350R). Details of a conference presentation on this subject have now been published (91/247).The concentration of some 48 elements were determined by ICP-MS following acid dissolution of typically 4% or less. Tests performed to assess the selectivity of the method towards glass type indicated a success rate in discriminating the source of origin of 85% of American window glass samples and 90% of Australian glass samples. Dissolution of glass samples can be extremely time consuming and methods are required which can analyse solid samples directly. Laser ablation ICP-MS appears to offer promise combining the rapidity of sampling with high sensitivity particularly for rare earth elements. However even in this case it would appear that some benefit may be obtained from performing sample preparation analysis (9 1 /C2823). It was found that borosilicate glass was easier to sample by laser ablation if the specimen surfaces were etched or frosted instead of being smooth.An alternative method of solid sampling suitable for the analysis of glass fibres has now been published (911874 see also J. Anal. At. Spectrom. 1990 5 350R). The glass fibre was continuously fed into a DCP (modified to include a thin sample feed tube inside the standard sample introduction tube) and directly atomized. The resultant AE signals were detected optically using an Cchelle spectrometer. It was found that glass fibres with a high silica content such as optical fibres with high melting- points could be analysed with acceptable accuracy by integrating the optical signal generated. This was not possible with low melting-point glasses such as soda lime as the fibres tended to sag or bend with heat.In such cases the sample was introduced in a pulsed manner with a residence time of less than 10 s in the DCP. Signals were then measured as peak heights on a chart recorder and averaged. Results obtained using the continuous method showed reasonable agreement with known values of Ca Ge and P in fibres. However it was concluded that the pulsed technique was innaccurate based on results from the analysis of soda lime glass television screen glass and lead glass. X-ray spectrometric techniques have also been used for the examination of glasses. Energy dispersive XRF has been suggested as a potential method of distinguishing between glass types (91/C2036) but it has also been reported that the technique can suffer from size effects which affect X-ray intensities (9 1/962).A new technique known as low-energy electron induced XRF has been applied to the determina- tion of B in borosilicate glasses (91K1806). Low energy X- ray emission was induced by secondary electrons produced in a glow discharge. The emission was detected using an X- ray vacuum spectrometer utilizing a lead stearate crystal analyser. The detection limit for B in glass was reported to be 20 ppm. There were also reports of the application ofJOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY DECEMBER 199 1 VOL. 6 317R EXAFS to the examination of glasses. These included a study of the role of Fe and U in the corrosion of sodium borosilicate glasses (9 1/3376) an investigation of diffusion properties of oxide glasses and glass surfaces (9 113377) and a study of the structural environment of Mn and Sr in the dry and hydrous silicate glasses (9113459).An example of the use of a radiofrequency powered glow discharge for the analysis of NIST SRM multicomponent glass by AES may also be of interest (91/878). 3.3.2. Ceramics and refactories The advent of high-temperature superconduclors several years ago stimulted a demand for analytical methodology for the characterization of these materials. Most of the techniques for inorganic analysis have now been applied to the task but reports on sample preparation methodology continue to appear. These are summarized in the appropri- ate section of Table 3. The analysis of thin films of superconducting material is becoming increasingly impor- tant and as a consequence methods for examining solids directly are being explored.X-ray techniques offer the advantage of non-destructive analysis which is important in the study of unique structures. Thus EDXRF has been used to determine the composition of thin films of superconduc- tor material (9111532) and has been compared with PIXE for a similar application (9 112588). Various film substrates were used including thin Mylar sheet and thicker magne- sium oxide alumina and strontium titanate backings. It was found that EDXRF provided superior detection limits to PIXE for Ba Cu and Y (in the mid-ng range) on thin backing and that the use of thicker backing materials degraded these considerably. A method for the preparation of standards for the determination of Y:Cu and Ba:Cu ratios in a superconducting yttrium-barium-copper oxide film by XRF has also been reported (9113098).Scanning- beam X-ray diffractometry was used in the determination of phase composition of superconductor films (9 1/3057). It was recommended that the technique was used for the examination of films more than 1 nm thick. In a novel approach AAS was used to monitor and control the deposition rate of semiconductor on substrates (911111). Since the light beam from the HCL could be passed through the vapour stream this enabled the region of sampling to be very close to the surface of the substrate thus permitting estimation of the composition of the film being deposited. This information was used to control the composition of the film as it was developed. Thin layers of superconducting material have been de- posited by laser ablation prior to analysis by MS (9 112288) or SIMS (9 11C1728 9 112283).In the latter case PIXE and Rutherford backscattering were also used to characterize the samples. A review of the application of Rutherford backscattering to the examination of superconducting oxide thin films has been published (9113493). A time-ojflight atom probe which yields high sensitivity chemical atom detection with atomic resolution imaging capability has been described (9112365). The instrument consisting of a field ion microscope and a time-of-flight mass spectrometer with a positron sensitive detector was applied to the study of surface segregation in a yttrium barium copper oxide superconductor.The analysis of rare earth oxides continues to receive attention although it should be pointed out that the majority of the abstracts received contained information at least a decade away from current awareness. Most publica- tions revisited sample preparation methodology or re- discovered the inherent spectral interference problems associated with ICP-OES for the analysis of such samples. This information is available for reference in Table 3. The use of a high-resolution spectrometer system to minimize spectral intei$erences in REE matrices may be considered useful reading in this context (91/865). A slurry introduc- tion procedure for the determination of trace elements in zirconia by ICP-OES was compared in terms of analytical performance with conventional procedures involving fu- sion with ammonium sulphate followed by dissolution or extraction of the resulting residue (9 1/C28 13).The slurry procedure consisted of ultrasonic dispersion of the zirconia powder in water acidified with hydrochloric acid. It was found that good agreement was obtained between the slurry and conventional procedures for the determination of Al Ca Fe Mg Na Ti and Y. Laser ablation provides an alternative method of introducing solid samples into the ICP (9 11866). A laboratory constructed carbon dioxide laser (spot size 0.24 mm) was used to ablate samples directly and a 1 m focal length spectrometer was used to measure REE signals from the ICP. Results indicated that this. approach was efficient for the determination of REEs. The direct analysis of REEs in yttrium oxide using laser ablation inside a graphite furnace has been described (911C2867).A ruby laser was used to ablate solid materials into a non-thermal plasma discharge sustained at low pressure inside the furnace. Detection limits and precision obtained for the more volatile elements were in the same range as for laser ablation ICP-AES. However the results obtained for the analysis of Dy and Er were not so favourable owing to the high energy required for the production of free atoms of these elements. The development of non-oxide ceramics continues and a great deal of effort has been devoted to establishing suitable methodology for quantitative analysis of these materials. Unfortunately the properties which make non-oxide cera- mics attractive (e.g.high temperature stability resistance to chemical attack) cause problems in sample preparation. Consequently much of the literature is devoted to the development of sample preparation procedures for opening out these structures prior to analysis by ICP-AES. Several abstracts were received concerning the use of slurry intro- duction procedures for ICP-AES. Broekaert and co-workers (9 1/C492,9 1/C2892) compared dissolution and slurry ICP- AES procedures for the analysis of silicon carbide. The dissolution procedure involving heating and sample for 8 h with a mixture of nitric hydrofluoric and sulphuric acids was also evaluated in conjunction with ETAAS. The slurry procedure required only that the sample powder was suspended in water and treated ultrasonically for 15 min.It was reported that provided the particle size of the sample was less than 10 pm accurate determination of trace impurities in the ppm range could be achieved using the slurry method. This finding was confirmed in a separate study comparing pressurized wet digestion of silicon car- bide with slurry analysis both by ICP-AES (911C2735). However it was observed that even when using a high power (2-4 kW) plasma accuracy was not always guaran- teed. Tracer experiments indicated that the largest particles were separated by nebulization and that transport efficiency was the limiting factor on accuracy for the determination. The C content of silicon nitride (particle size t 5 pm) was determined using a slurry ICP-AES method (911108). An extended torch was used to minimize the C blank and this was further reduced by the use of high-purity argon and suspension of the sample in fresh high-purity doubly distilled water.Calibration and addition methods were carried out using acetic acid as a reference C standard. A limit of detection of 0.018% C was reported. Finally impurities in silicon carbide were determined directly using solid sampling ETV-ICP-AES (91K228 1). A variety of thermochemical additives such as barium nitrate barium carbonate lead borate or sodium borate and volatilization aids such as potassium fluoride silver chloride and cobalt fluoride were evaluated both separately and in combina-318R JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY DECEMBER 199 1 VOL. 6 tion for their efficacy in removing the sample from the electrically heated graphite crucible and introducing it into the ICP.The combination of barium nitrate and cobalt fluoride was found to be the most suitable and the methodology was used to determine Al Cr Mn Mo Ni V and W in silicon carbide powder. Sample preparation methods for the analysis of alumi- nium and silicon oxide based ceramics are listed in Table 3. The length of time required for these methods and their relative complexity has stimulated research to find simpler and more rapid means of characterizing these materials. The application of slurry sampling is increasing in popular- ity as an alternative to digestion procedures (9112232 91/2968 see also J. Anal. At. Spectrom. 1990 5 356R). Slurry-based methods have been proposed for the determi- nation of Ga in alumina by ETAAS (911845) and Pd and Pt in alumina by ETAAS (911C2152).However the high temperature of the ICP provides more effective atomiza- tion of refractory materials. Brenner and Long (911C771 9 1/864) utilized slurry sampling in conjunction with mixed- gas plasmas for the analysis of a number of refractory RMs including aluminium rich fire brick (NIST SRM 269) silica brick (BCS CRM 3 15) and silicate brick containing alumina (NIST SRMs 198 and 199). Slumes of 1% m/v composition were introduced to the ICP using a Babington type high solids nebulizer and analysed in plasmas containing 5% oxygen in argon 10% nitrogen in argon and pure argon. It was found that the argon-oxygen plasma exhibited the highest analytical sensitivity for Fe and Si.Other studies of aerosols produced by slurry nebulization of alumina pow- der indicated that evaporation is incomplete for particles with diameters exceeding a critical value (911C1767). Transport efficiency may also depend on particle morpho- logy (911C2803). Different shapes of particles were found on sampling above the plasma using a cascade impactor both in the case of alumina and silicon carbide. The fraction of each type of particle collected was dependent on plasma conditions indicating the need for optimization to make the best use of slurry sampling. Efforts continued towards developing direct solid sampl- ing methods for the analysis of oxide ceramics. Laser ablation ICP-MS has been increasingly cited as a promising method for the characterization of such materials (911C1772 911C1922 911C2809 see also J.Anal. At. Spectrom. 1990 5 356R). Sadly much of the work described in conference reports fails to appear subsequently in the primary literature. Nevertheless a number of groups appear to be agreed on the benefits of the method in this application. Examples of the applications of laser ablation ICP-MS cited this year include the analysis of ferrite ceramics using UV laser (91/C1920) trace analysis of alumina silicon nitride and zirconia (9 11C508) and unspe- cified ceramics and superconducting materials (9 1 1 0 10). An attempt to improve quantification of laser ablation ICP- MS using non-matrix matched standards for the analysis of ceramics based on the element enthalpy of atomization was unsuccessful (911C1925). This was attributed to the fact that the analytes were present in the form of oxides and carbides rather than the metal itself.Glow discharge mass spectrometry has also been proposed as a method for the ultra-trace level analysis of ceramics (9 11C782 9 11C173 1). The quantitative determination of Ca Fe Na S Si and Ti in alumina was demonstrated using a high-resolution GDMS instrument (9 1 /C 1 654). Precision of the order of 5% relative was achieved and calibration linearity was demonstrated over at least two orders of magnitude. Detection limits in the ppb range based on an integration time of 30 s were claimed. One of the difficulties in the application of d.c. powered GD sources is that non- conducting materials such as ceramics have to be mixed with a conducting host matrix in order to achieve a stable discharge.However the advent of r.f. powered GD sources should overcome this limitation. At least two different systems have now been constructed and applied to the analysis of ceramics but few details are available on analytical performance as yet (9 11C2006 9 l1C2855). Catalysts are essentially materials that are designed with in-built functionality. Their activity usually increases with surface area and consequently highly porous struc- tures such as those constructed from aluminas and zeolites provide ideal substrates for this activity. Consequently the chemistry of these systems is rather similar to that of ceramics and refractories and the structure of the review has been modified to include the abstracts relevant to catalysts in this section.The composition of catalyst materials is often confidential and methodologies tend to be reported in the open literature only in generic terms. Nevertheless a summary of the analytical methods specific to catalysts is given in Table 3. There was little innovation in this area in the year under review. Flame AAS methods have long been used in the petroleum industry for the analysis of catalysts. The determination of Co Fe Mo and Ni in heterogeneous catalysts by FAAS has been reported (9 11247 1). Microwave assisted digestion of the samples in closed vessels in a mixture of nitric and phosphoric acids was claimed to give total recovery of analyte elements without complete destruction of the sample. In another application of FAAS trace levels of Cd Cu and Pb in catalysts and alumina support were pre-concentrated from the matrix on sulphydryl cotton.The elements were washed off the cotton with hydrochloric acid and analysed directly. Plasma emission methods have been reported for the analysis of fluid cracking catalysts based on acidic decom- position (911C1734 91/C2093) rhodium catalysts (91185) and alkali media (9 1K2839). Automotive catalysts have been characterized by ICP-MS using microwave assisted dissolution for sample preparation (9 lK2073). X-ray fluorescence has been applied to the determination of chloride in reforming catalysts (9113295) and to the measurement of platinum in used reforming catalysts (91156). Finally the use of EXAFS for investigation of the cobalt phase on boron-modified cobalt alumina catalysts may be of some interest (9112966).A cross-correlation method of data analysis of the spectra was used to determine the relative amounts of cobalt oxide and cobalt surface phase present on the catalysts.JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY DECEMBER 199 1 VOL. 6 319R LOCATION OF REFERENCES The full list of references cited in this Update have been published as follows 9013592-9014 179 J. Anal. At. Spectrom. 1990 5(8) 36 1R-378R. 9111-911825 J. Anal. At. Spectrom. 1991 q l ) 41R-68R. 911826-911C1687 J. Anal. At. Spectrom. 1991 q3) 109R-136R. 91/C1688-91/2702 J. Anal. At. Spectrom. 1991 q4) 153R-185R. 9112703-911C2928 J. Anal. At. Spectrom. 1991 q5) 221R-227R. 9112929-9113584 J. Anal. At. Spectrom.1991 6(7) 257R-280R. Abbreviated forms of the literature references quoted (excluding those to Conference Proceedings) are given on the following pages for the convenience of the readers. The full references names and addresses of the authors and details of the Conference presentations can be found in the appropriate issues of JAAS cited above. Abbreviated List of References Cited in Update 9013952. Anal. Sci. 1990 6 97. 9013957. Spectrochim. Acta Part B 1990 45 119. 9013965. Spectrochim. Acta Part B 1990 45 271. 9013973. Spectrochim. Acta Part B 1990,45,427.90/3976. Spectrochim. Acta Part B 1990,45 615. 9013980. Anal. Chim. Acta 1989 226 193. 9013991. Zh. Prikl. Spektrosk. 1989,51 903.9013995. Anal. Chem. 1990 62 1155. 9013998. Fresenius Z. Anal. Chem. 1989 335 648.9014001. Fresenius Z. Anal. Chem. 1989 335 698. 9014006. Fresenius Z. Anal. Chem. 1989 335 893. 90l4007. Fresenius Z. Anal. Chem. 1989 335 900. 9014008. Fresenius Z. Anal. Chem. 1989 335 910. 90l4010. Fresenius Z. Anal. Chem. 1989 335 971. 90/4012. Fresenius 2. Anal. Chem. 1989 335 1005. 9014015. Fresenius J. Anal. Chem. 1990,336 120.9014023. Bunseki Kagaku 1990 39 19. 9014025. Bunseki Kagaku 1990 39 49. 9014027. Bunseki Kagaku 1990 39 171. 9014136. Second Ion Mass Spectrom. Proc. Int. ConJ 6th 1987 433 9014146. J. Anal. At. Spectrom. 1990 5 195. 9014157. J. Anal. At. Spectrom. 1990 5 269. 9014162. Analyst 1990,115,865. WI4164. Anal. Proc. 1990,27,186. 9014167. Bunseki Kagaku 1990 39 T17. 9014173. At. Spectrosc. 1989,10 144.9117. J. Anal. At. Spectrom. 1990 5 325.9119. Analyst 1990 115,911. 91/12. Analyst 1990 115 943. 91/13. Analyst 1990 115 955. 91/16 Appl. Spectrosc. 1989,43 1 132.91119. Appl. Spectrosc. I989,43 1187. 91/21. Appl. Spectrosc. 1989 43 1257. 91145. At. Spectrosc. 1990 11( l) 1. 91/50. Spectroscopy (Eugene Oregon) 1989 4 36. 91/56. Analysis 1990 18(l) 24. 91/77. Anal. Sci. 1990 6 803. 91180. Anal. Sci. 1990,6 3 15. 91/83 Bunseki Kagaku 1990,39 39.91184. 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ISSN:0267-9477    

DOI:10.1039/JA991060283R

出版商:RSC    

年代:1991

数据来源: RSC

摘要:

JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY DECEMBER 1991 VOL. 6 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. 322R a.c. AA AAS AE AES AF AFS AOAC APDC ASV CCP CMP CRM cw d.c. DCP DMF DNA EDL EDTA EDXRF EIE EPMA ETA ETAAS ETV EXAFS FAAS FAB FAES FAFS FI Fr FTMS GC GD GDL GDMS Ge(Li) HCL h.f. HG HPGe HPLC IAEA IBMK ICP ICP-MS IR alternating current atomic absorption atomic absorption spectrometry atomic emission atomic emission spectrometry atomic fluorescence atomic fluorescence spectrometry Association of Official Analytical Chemists ammonium pyrrolidinedithiocarbamate (ammonium pyrrolidin-1-yl dithioformate) anodic-stripping voltammetry capacitively coupled plasma capacitively coupled microwave plasma certified reference material continuous wave direct current d.c.plasma Nfl-dimethy lformamide deoxyribonucleic acid electrodeless discharge lamp ethylenediaminetetraacetic acid energy dispersive X-ray fluorescence easily ionizable element electron probe microanalysis electrothermal atomization electrothermal atomic absorption electrothermal vaporization extended X-ray absorption fine structure flame AAS fast atom bombardment flame AES flame AFS flow injection Fourier transform Fourier transform mass spectrometry gas chromatography glow discharge glow discharge lamp glow discharge mass spectrometry lithium-drifted germanium hollow cathode lamp high frequency hydirde generation high-purity germanium high-performance liquid chromatography International Atomic Energy Agency isobutyl methyl ketone (4-methylpentan-2- inductively coupled plasma inductively coupled plasma mass spectrome- try infrared spectrometry spectroscopy one) IUPAC LC LEI LMMS LTE MECA MIP MS NAA NaDDC NIES NIST NTA OES PIGE PIXE PMT PPb PPm PTFE QC r.f.REE(s) RIMS RM RSD S/B SEC SEM SFC Si(Li) SIMAAC SIMS S/N SR SRM SSMS STPF TCA TIMS TLC TOP0 TXRF u.h.f. uv VDU vuv WDXRF XRF International Union of Pure and Applied liquid chromatography laser-enhanced ionization laser microprobe mass spectrometry local thermal equilibrium molecular emission cavity analysis microwave-induced plasma mass spectrometry neutron activation analysis sodium diethyldithiocarbamate National Institute for Environmental National Institute of Standards and nitrilotriacetic acid optical emission spectrometry particle-induced gamma-ray emission particle-induced X-ray emission photomultiplier tube parts per billion parts per million pol ytetrafluoroethy lene quality control radio frequency rare earth element(s) resonance ionization mass spectrometry reference material relative standard deviation signal to background ratio size-exclusion chromatography scanning electron microscopy supercritical fluid chromatography lithium-drifted silicon simultaneous multi-element analysis with a continuum source secondary ion mass spectrometry signal to noise ratio synchrotron radiation Standard Reference Material spark source mass spectrometry stabilized temperature platform furnace trichloroacetic acid thermal ionization mass spectrometry thin-layer chromatography trioctylphosphine oxide total reflection X-ray fluorescence ultra-high-frequency ultraviolet visual display unit vacuum ultraviolet wavelength dispersive X-ray fluorescence X-ray fluorescence Chemistry Studies Technology .

ISSN:0267-9477    

DOI:10.1039/JA991060322R

出版商:RSC    

年代:1991

数据来源: RSC

摘要:

32313 JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY DECEMBER 199 1 VOL. 6 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. 9113585. 9113586. 9113587. 9113588. 9 113589. 9 1 I3 590. 9 11359 1. 9113592. 9113593. 9113594. Allain P. Berre S. Premel-Cabic A. Ma- Y. Delaporte T. Concentrations of rare earth elements in plasma and urine of healthy subjects determined by inductively coupled plasma mass spectrometry Clin. Chem. 1990,36,2011. (Lab. Pharmacol. Centre Hosp. Univ. Rue Larrey 49033 Angers Cedex France). Fpruta N. Optimization of the mass scanning rate for the determination of lead isotope ratios using an inductively coupled plasma mass spectrometer J. Anal. At. Spectrom. 1991 6 199.(Div. Environ. Chem. Natl. Inst. Environ. Stud. 16-2 Onogawa Tsukuba Ibaraki 305 Japan). Kim C.-k. Seki R. Morita S. Yamasaki S.4 Tsamura A Takaku Y. Igarashi Y. Yamamoto M. 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Opt. 1991,30 387. (Royal Inst. Technol. Phys. Dept. I S-100 44 Stockholm Sweden). Snowdon P. Skippon S. M. Ewart P Improved precision of single-shot temperature measurements by broadband CARS by use of a modeless laser Appl. Opt. 1991,30 1008. (Shell Res. Thornton Res. Centre P.O. Box 1 Chester CH1 3SH UK). Eichler J. P. F. Wolff W. Wolf H. E. Coelho F. S. de Barros S Borges A. M. Ackermann G. Processing of holographic AgBr films studied by X-ray fluores- cence analysis Appl. Opt. 1991,30 1201. (Technische Fachhochschule Berlin Physiklabor D- 1000 Berlin 65 Germany). Papers 91/C3619-91/C3765 were presented at the 1991 Pittsburgh Conference and Exposition on Analytical Chemistry and Applied Spectroscopy McCormick Place-on-the-Lake Chicago IL USA March 3rd-8th 199 1.91lC3619. Dahlquist R. L. Eldridge R. Tasker D. Fry R. C. New high electron number density (end) ICP (11) analytical figures of merit (Applied Research Labs./ Fisons Instruments 249 1 1 Ave. Stanford Valencia CA 91355 USA). 9 1 /C3620. Dahlquist R. L. Eldridge R. Tasker D. Kenessey B. New high electron number density (end) ICP (I) configurations and design optimization (Applied Re- search LabsJFisons Instruments 249 1 1 Ave. Stanford Valencia CA 91355 USA). 9 l/C362 1. Floyd R. C. Determination of trace level contaminants in power plant steam cycle samples by inductively coupled plasma atomic emission spectrometry (ICP- AES) with ultrasonic nebulization (USN) (Fisons Instruments 15300 Rotunda Dr.Suite 30 1 Dearborn MI 48 120 USA). 91/C3622. Koga M. Okumoto T. Okamoto Y. Ogan K. High- power nitrogen microwave-induced plasma mass spec- trometer for trace element analysis (Hitachi Naka Works 882 Ichige Katsuta Ibaraki 3 12 Japan). 91lC3623. Samuel O. Gautherin J. C. Le Marchand A. Lang Y. Brenner I. B. Polyscan ICP spectrometers-scann- ing polychromators for problem solving in multi- element analysis (Jobin Yvon (ISA) 16-18 Rue du Canal Longjumeau Cedex 9 1 163 France). 91/C3624. Fredeen K. J. Denoyer E. R. Hager J. W. Methods development strategies for laser sampling ICP mass spectrometry (Perkin-Elmer 76 1 Main Ave. Norwalk 9 1/C3625. Oho K. New electrothermal sample vaporizing method for ICP emission spectroscopy (Shimadzu 1 Nishinokyo-Kuwabaracho Nakagyo-ku Kyoto 604 Japan).91/C3626. Delles F. Frary B. Automation of the USEPA’s contract laboratory program requirements for the determination of elements in waste waters by graphite furnace atomic absorption spectrometry (GFAAS) (Varian Optical Spectroscopy Instruments 20 1 Hansen Court Wood Dale IL 60 19 1 USA). 91/C3627. Knowles M. Shrader D. New design graphite furna- ce-platform assembly used to determine a reference range for human urinary manganese (Varian Optical Spectroscopy Instruments 20 1 Hansen Court Suite 108 Wood Dale IL 60191 USA). 91/C3628. Wang J.-s. Evans E. H. Caruso J. A. Addition of molecular gases to Ar gas flows for the reduction of polyatomic ion interferences on arsenic and selenium in inductively coupled plasma mass spectrometry (Dept.Chem. ML 172 Univ. Cincinnati OH 4522 1 USA). 91/C3629. Stockwell P. B. Ebdon L. C. Corns W. Vapour generation techniques to measure arsenic by atomic fluorescence (P. S. Analytical B4 Chaucer Business Park Kemsing Sevenoaks Kent TN15 6QY UK). 91/C3630. Li Z. McIntosh. S. Carnrick. G. Slavin. W.. Determi- CT 06859-02 19 USA). nation of tin using hydride hS’including flow injec- tion analysis (FIA) and trapping in a graphite furnace (Perkin-Elmer 761 Main Ave. Norwalk CT /C3631. Bozic J. Ethier R. L. Balleny J. M. Rapid determi- nation of traces of selenium and tellurium in copper electrolytes (INCO Ltd. Central Process Technol. Copper Cliff Ontario POM 1N0 Canada). /C3632. Offley S.G. Seare N. J. Tyson J. F. Kibble H. A. B. Determination of hydride-forming elements in metals by flow injection atomic absorption spectrometry with 06859-0237 USA).JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY DECEMBER 199 1. VOL. 6 325R on-line matrix isolation (Dept. Chem. Univ. Technol. Loughborough Leicestershire LE11 3TU UK). 91IC3633. Alvarado J. Carnahan J. W. Determination of As Sb and Se with electrothermal vaporization into a helium microwave-induced plasma (Dept. Chem. Northern Illinois Univ. DeKalb IL 601 15 USA). 91K3634. Prell L. J. Lindner J. D. Letourneau V. A. Dobb D. E. Hinners T. A. Simultaneous ICP-AES determina- tion of As Sb and Se by hydride-generation sample introduction (Lockheed Eng. Sci. Co. 1050 E. Flam- ingo Rd. Las Vegas NV 891 19 USA).91K3635. Shrader D. Moffett J. 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Non- metal selective liquid chromatography detection a moving band liquid chromatography-helium microwave induced plasma interface (Dept. Chem. Northern Illinois Univ. DeKalb IL 601 15 USA). 911C3640. Bullock A. Charalambous P. Milton D. Trace elemental analysis of conducting solid samples using the VG Gloquad (VG MicroTrace Ion Path Rd. Three Winsford Cheshire CW7 3BX UK). 9llC3641. Koirtyohann S. R. History of atomic absorption spectroscopy from an academic perspective (Dept. Chem. Univ. Missouri Columbia MO 65203 USA). 9 1/C3642. Slavin W. Waters symposium on atomic absorption spectroscopy (Perkin-Elmer 76 1 Main Ave.Norwalk 91lC3643. Ward A. F. Hahn J. C. Bostick A. W. Development of a generic control system using atomic spectroscopy for real-time process monitoring (Ward Scientific 2 Ray Ave. Burlington MA 0 1803 USA). 9 l/C3644. Anderau C. Quality control concept for ICP emission and mass spectrometry (Perkin-Elmer 76 1 Main Ave. Norwalk CT 06859-0219 USA). 91K3645. Fister J. C. 111 Oleski J. W. Vaporizing aerosol droplets a key to understanding spatial emission profiles and matrix effects in inductively coupled plasmas? (Dept. Chem. Univ. North Carolina Ven- able and Kenan Labs. CB No. 3290 Chapel Hill NC 911C3646. Tyler G. Finotello F. Nham T. Automation of the USEPA's contract laboratory program requirements for the determination of 15 elements in a variety of environmental samples by inductively coupled plasma optical emission spectrometry (ICP-OES) (Varian Op- tical Spectroscopy Instruments 20 1 Hansen Court Suite 108 Wood Dale IL 60 19 1 USA).91/C3647. Liang D. C. Graphite furnace-from an atomizer for AAS to a plasma emission source for AES (Aurora Instruments 303 1 Main St. Vancouver British Co- lumbia V5T 3G6 Canada). 911C3648. Barber T. E. Walters P. E. Wensing M. W. CT 06859-0237 USA). 27599-3290 USA). Winefordner J. D. Reference locked diode laser atomic absorption spectroscopy (Dept. Chem. Univ. Florida Gainesville FL 326 1 1 USA). 91/C3649. Su E. G. Irwin R. L. Liang 2.-w. Michel R. G. Background correction by wavelength modulation in laser-excited atomic fluorescence spectrometry (Dept. Chem. Univ. Connecticut U-60 Storrs CT 06268 USA).9 1x3650. Liang Z.-w. Irwin R. L. Michel R. G. Signal-to-noise ratio of transient signals in laser-excited atomic fluores- cence spectrometry in an electrothermal atomizer (Dept. Chem. Univ. Connecticut U-60 Storrs CT 9 l/C365 1. Tyson J. F. Bysouth S. R. Gluodenis T. J. Larue R. M. Adeeyinwo C. E. Seare N. J. On-line closed loop dilution procedure for flame atomic absorption spec- trometry (Dept. Chem. U iv. Massachusetts Am- herst MA 01003 USA). f 91/C3652. Gill R. J. Grey R. G. Liddell P. R. Peile R. C. Wallis N. J. Analysis of -samples containing high concentrations of dissolved solids using flame AAS (GBC Scientific Equipment Pty 22 Brooklyn Ave. Dandenong Victoria 3 175 Australia). 9 1/C3653. Miller-Ihli N. J. Novel approach for multi-element graphite furnace analyses of solids (US Dept.Agric. ARS Nutr. Compos. Lab. Beltsville MD 20705 USA). 91/C3654. Batie W. Sciutto T. Kahn H. L. Multi-element ppb analysis by rapid sequential furnace atomic absorption (Analyte Corp. 910 Chevy Way Medford OR 97501 USA). 911C3655. Beach. C.. Moffett. J.. ADDlication of a new furnace 06269-3060 USA). platfoA 'design for the analysis of environmental samples (Varian Optical Spectroscopy Instruments 201 Hansen Court Suite 108 Wood Dale IL 60191 USA). /C3656. Giiell 0. A. Holcombe J. A. Rademeyer C. J. Monte Carlo optimization of graphite furnace design (Dept. Chem. Univ. Texas Austin TX 78712 USA). /C3657. Gokhale P. Shah A. Lutz M. X-Ray fluorescence analysis of fluid cracking catalysts (Akzo Chemicals 13000 Bay Park Rd Pasadena TX 77507 USA)./C3658. Adamson B. W. Bonvin D. Juchli K. Anzelmo J. A. Boyer B. W. Improvements in light element and liquids analysis using wavelength dispersive X-ray spectrometry (Applied Research Labs. CH 1024 Ecu- blens Switzerland). 91K3659. Grindle A. E. Foster R. W. Sotera J. J. Autoanalysis of wide concentration range environmental samples by ICAP using an intelligent automatic dilution system (Thermo Jarrell Ash 8E Forge Parkway Franklin MA 02038 USA). 91/C3660. Dulude G. R. Sotera J. J. Dauzvardis M. J. Interfacing an ion chromatograph with a multi-element AA (Thermo Jarrell Ash 8E Forge Parkway Franklin MA 02038 USA). /C3661. Schlemmer G. Schrader W. Baasner J. Portala F. On-line preconcentration with the flow injection tech- nique-benefits and limitations (BodensqFwerk Per- kin-Elmer P.O.Box 10 11 64 D-7770 Uberlingen Germany). /C3662. Genna J. L. Ruschak M. L. McAninch W. D. Craig W. C. Automated ICP method for the on-line analysis of aluminium alloys (Aluminium Company of America Alcoa Labs. Alcoa Center PA 15069 USA). 91/C3663. Long S. E. Riviello J. Practical aspects of coupling IC to ICP-MS for sample matrix modification (Techno- logy Applications USEPA 26 West Martin Luther King Dr. Cincinnati OH 45219 USA). 91K3664. Sheppard B. S. Heitkemper D. T. Wolnik K. A. Caruso J. A. Liquid chromatographic detection by helium-argon inductively coupled plasma mass spec- trometry (Natl. Forensic Center USFDA 1141 Cen- tral Parkway Cincinnati OH 45202 USA).326R 9 1x3665. 9 llC3666.91K3667. 91/C3668. 91K3669. 9 1K3670. 9 1x367 1. 9 lK3672. 9 1K3673. 91K3674. 9 1x3675. 9 1/C3676. 91/C3677. 9 1/C3678. 91K3679. JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY DECEMBER 199 1 VOL. 6 Kumar U. T. Evans E. H. Dorsey J. G. Caruso J. A. Speciation of organotin compounds by high-perform- ance liquid chromatography and detection by induc- tively coupled plasma mass spectrometry (Univ. Cin- cinnati Dept. Chem. ML 172 Cincinnati OH 4522 1 USA). Vela N. P. Story C. Evans E. H. Caruso J. A. Shen W.-l. Determination of organotin compounds by cou- pling supercritical fluid chromatography (SFC) and inductively coupled plasma mass spectrometric (ICP- MS) detection (Dept. Chem. Univ. Cincinnati Cin- cinnati OH 45221 USA). Averitt D. W. Trace metals in concentrated phospha- tic fertilizers and animal feeds by ICP-MS (IMC Fertilizer New Wales Operations QC Lab.P.O. Box 1035 Mulberry FL 33860 USA). Reffner J. A Grazing angle FTIR microscopy (Spec- tra-Tech Stamford CT 06906 USA). Seace K. man K. Iwata H. Improved analytical performance with new pyrolytic platforms used in simultaneous GFAA multielement determinations (Hitachi Instruments 44 Old Ridgebury Rd. Danbury CT 06810 USA). Hunault P. Le Marchand A Nod M. Brenner I. B. Recent developments in GD-ES instrumentation and methodology for bulk and surface analysis (Jobin Yvon (ISA) 16-18 Rue du Canal Longjumeau Cedex 9 1 163 France). Wllkopf U. Paul M. Applications of ICP-MS with sample introduction by electrothermal vaporization (Bodenseewerk Perkin-Elmer Postfach 10 1 164 D- 7770 ijberlingen Germany). Grillo A.C. Balas C. Collins B. Robotics and microwave digestion for totally automated sample preparation (Questron Corp. P.O. Box 2387 Prince- ton NJ 08619 USA). McLean M. A. Vestal M. L. Abramson F. A. Development and performance of an element and isotope selective detector for normal-bore HPLC using a microwave-induced plasma reaction interface and mass spectrometry (Vestec Corp. 9299 Kirby Dr. Houston TX 77054 USA). Tye C. T. McCurdy E. Marshall L. Design philoso- phy for a new environmental ICP-MS (VG Elemental Ion Path Rd. Three Winsford Cheshire CW7 3BX UK). Clark J. Greb U. Ronan G. Wheeler D. Improved sensitivity in GDMS an evaluation of glow discharge cell design and operating parameter (VG MicroTrace Ion Path Rd. Three Winsford Cheshire CW7 3BX UK).Majidi V Robertson J. D. Investigation of palladium and selenium interaction with the graphite surface by Rutherford backscattering (Dept. Chem. Univ. Ken- tucky Lexington KY 40506 USA). Peters S. E. O. Jowett M. E. Cooley W. B. Analysis of super alloys by inductively coupled plasma (ICP) with a conductive solids nebulizer (CSN) (Fisons Instruments 1 5300 Rotunda Drive Suite 30 1 Dear- born MI 48120 USA). Anzano J. M. Anwar J. Smith B. W. Winefordner J. D. Laser-excited atomic fluorescence in graphite fur- nace in solid samples determination of thallium in bovine liver (Dept. Chem. Anal. Div. Leigh Hall 109 Univ. Florida Gainesville FL 326 1 1-2046 USA). Pomeroy R. S. Baker M. E. Kolczynski J. D. Denton M. B. Indirect determination of phosphate silicate and arsenate by HPLC-AES (Dept.Chem. Univ. Arizona Tucson AZ 85721 USA). 9 1/C3680. 9 1/C368 1. 9 1K3682. 9 1/C3683. 91K3684. 911C3685. 9 1K3686. 91K3687. 91K3688. 91/C3689. 9 1/C3690. 9 1/C369 1. 9 1K3692. 9 l/C3693. 9 1/C3694. 9 1/C3695 Grandsard P. Megargle R. Markelov M. Automated standard preparation system (Cleveland State Univ. Chem. Dept. Cleveland OH 441 15 USA). Aramata M. Kawate Y. Asada S. Trace analysis of U and Th in electronic materials by flash atomized ICP- MS (Shin-Etsu Chemical Co. Isobe Annaka Gunma 379-0 1 Japan). Merchant S. G. Reliability of a new technique of preparing samples for energy dispersive analysis of X- rays (EDAX) for multi-elemental analysis (Dept. Chem. Sardar Pate1 Univ. Vallabh Vidyanagar 388 120 Gujarat State India).Mahan C. A. Holcombe J. A. Immobilized algae for preconcentration of part per trillion levels of metals in complex matrices (Dept. Chem. and Biochem. Univ. Texas at Austin Austin TX 78712 USA). Fernando M. C. E. Determination of lead in evapo- rated milk (Ener-tec Phils. Philippine Atomic Energy Comm. 1162 Casanas St. Sampaloc Manila The Philippines). h a t N. A Sneddon J. Use of flow injection analysis inductively coupled plasma atomic emission spectrometry and electrothermal atomization atomic spectrometry for the direct determination of copper iron selenium and zinc in blood (Dept. Chem. Univ. Lowell Lowell MA 01854 USA). Huang A.-h. Tao L.-h. Zhu J.-h. Wang X.-p. Determination of arsenic-binding compounds in rats livers by column chromatography-flameless atomic absorption spectroscopy (Environ.Med. Res. Lab. Hunan Med. Univ. Changsha Hunan 4 10078 China). Denton M. B Future of charge transfer detector arrays in atomic spectroscopy (Dept. Chem. Univ. Arizona Tucson AZ 85721 USA). Mermet J. M. Laser ablation and the future of solid- sample atomic spectrometry (Lab. Sci. Anal. Univ. Lyon I 69622 Villeurbanne Cedex France.). Harrison W. W. Klingler J. A. Mei Y. Ratliff P. H. Glow discharge a born-again source for atomic spec- troscopy (Dept. Chem. Univ. Florida Gainesville FL 326 1 1 USA). Horlick G. Shao Y.-b. Feng X.-b. ICP-MS and GD- MS complementary or competitive? (Dept. Chem. Univ. Alberta Edmonton Alberta T6G 2G2 Canada). Barnes R. M. Martines L. J. Automated flow- through microwave digestion for on-line sample prepa- ration and inductively coupled plasma spectrometry (Univ.Massachusetts Dept. Chem. Lederle GRC Towers Amherst MA 01003-0035 USA). Hasty E. T. Littau S. E. Engelhart W. G. Optimiza- tion of microwave sample preparation using parameter feedback control (CEM Corp. P.O. Box 200 Mat- thews NC 28 106 LJSA). Walsh A. Development of AAS methods of elemental analysis-some personal reminiscences (Honorary Fellow Div. Mater. Sci. and Technol. CSIRO Coded Bag 33 Clayton Victoria 3 168 Australia). Olesik J. W. New insights into processes controlling analytical signals in inductively coupled plasmas (Dept. Chem. Univ. North Carolina Venable and Kenan Labs. CB No. 3290 Chapel Hill NC Story W. C. Evans E. H. Heitkemper D. T. Caruso J. A. Speciation studies of selenium and arsenic by reversed-phase high-performance liquid chromato- graphy employing hydride generation and inductively coupled plasma mass spectrometric detection (Dept.Chem. Univ. Cincinnati ML 172 Cincinnati OH 27599-3290 USA). 4522 1-01 72 USA).JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY DECEMBER 199 1 VOL. 6 327R 91/C3696. 9 1 ~ 3 6 9 7 . 9 1/C3698. 9 1 /C3699. 9 1 /C3700. 9 1 /C370 1. 9 1 /C3702. 91/C3703 91/C3704 Schindler J. S. Tisdale R. C. Application of X-ray fluorescence techniques to environmental measure- ments (ASOMA instruments 122 12-H Technology Blvd. Austin TX 78727 USA). Batie W. Bernhard A. E. Fast automated multi- element elemental analysis of sludges and effluents using a new sequential atomic absorption spectrometer (Analyte Corp. 910 Chevy Way Medford OR 97504 USA).Irwin R. L. Wei G.-t. Butcher D. J. Takahashi J. Walton A. P. Michel R. G. Laser-excited atomic fluorescence spectrometry with Zeeman background correction for the determination of trace elements in real samples. (Dept. Chem. Univ. Connecticut Storrs CT 06268 USA). Sneddon J. Li K.-p. Hwang 2.-w. Teng. Y.-y. Quantitative interaction of a laser beam with solid metals (Dept. Chem. Univ. Lowell Lowell MA 0 1854 USA). Gonon L. Mennet J. M. Mathe D. Optimization of an acid mixture for microwave-assisted digestion of steels (Lab. Anal. Sci. Bat. 308 Univ. Lyon I 69622 Villeurbanne Cedex France). Gaunt J. A Analytical performance of an automatic sample preparation system for atomic absorption spec- trometry (Dept. Civil Construction Eng. 123 Town Engineering Bldg Iowa State Univ.Ames IA 5001 1 USA). de Mauleon N. Berthoumieux G. Fedry M. Mathe D. Microwave digestion method for determination of mineral elements in health food by atomic absorption spectrometry (flame). Comparative studies between conventional and rapid methods microwave digestion and NIR analysis for determination of total nitrogen (Lab. Dietetique et Sante SA BP 106 31250 Revel France). Brenner I. B. Gautherin J. C. Le Marchand A. Lavenir E. Samuel O. Lagrave X. Automated rapid analysis of complex materials by ICP-AES-applica- tion of elemental tracers for the analysis of high solid and viscous materials (Jobin Yvon (ISA) 16-18 Rue du Canal Loniziumeau. Cedex 9 1 163. France). tively heated target (Dept. Chem. Howard L. Hunter Chem. Lab.Clemson Univ. Clemson SC 91/C37 1 1. McCaffrey J. T. Barnett W. B. Hager D. G. Recent improvements in QA/QC control using automated atomic absorption instruments (Perkin-Elmer 76 1 Main Ave. Norwalk CT 06859-0219 USA). 911C3712. Bysouth S. R. Tyson J. F. Debra4 E. Gluodenis T. J. Larue R. M. Extending the capabilities of flame atomic absorption spectrometry with on-line sample treatment (Dept. Chem. Univ. Massachusetts Am- herst MA 01003 USA). 91lC3713. Carnrick G. Schickli J. Slavin W. Increasing graph- ite furnace atomic absorption productivity (Perkin- Elmer 761 Main Ave. Norwalk CT 06859-0219 USA). 9 1K37 14. Riby P. G. Harnly J. M. Styris D. L. Determination of boron by hollow anode furnace atomization non- thermal excitation spectrometry (USDA NCL BHNRC Bldg. 16 1 BARC-East Belstville MD 20705 USA).91K3715. Schlemmer G. Schrader W. Shuttler I. Huth R. Avoiding carryover in graphite furnace determinations of refractory elements (Bodenseewerk Perkin-Elmer P.O. Box 101 164 D-7770 herlingen Germany). 9 1 /C37 16. Hutton R. C. Gregson D. Vogel W. Steiner J. D. Eastgate A. Alternate sampling strategies for ICP-MS (VG Elemental Ion Path Rd. Three Winsford Chesh- ire CW7 3BX UK). 91/C3717. Bengtson A. Eklund A. Quality control of coated metal products by glow discharge emission spectros- copy (Swedish Inst. for Metals Res. Drottning Kristi- nas vag 48 S-114 28 Stockholm Sweden). 9 1x37 1 8. Krupa R. J. Owen E. E. Thorne E. H. IV Design of a new scanning monochromator for ICP-AES (Baird Corp 125 Middlesex Turnpike Bedford MA 01730 USA).91K3719. Quimby B. D. Dryden P. C. Sullivan J. J. Sulphur simulated distillation using GC-AED (Hewlett-Pack- ard P.O. Box 900 Avondale PA 193 1 1 USA). 29634- 1905 USA). - 91X3720. Starn T. K. Broekaert J. Hieftje G. M. Atmospheric Nwogu V. I. Zhu G.-x. Browner R. F. Studies on sampling glow discharge as an ionization and excitation electrothermal . - . . . vaporization . . (ETV) . sample introduc- . . source for optical emission spectrometry and mass tion for inductively coupled plasma atomic emission spectrometry (ICP-AES) (Sch. Chem. and Biochem. Georgia Inst. Technol. Atlanta GA 30332 USA). 9 1/C3705. Nygaard D. D Bulman F. D. Wang X. R. Analysis of complex samples using ICP-OES with ultrasonic nebu- lization (Baird Corp. Anal.Instrum. Div. 125 Middlesex Turnpike Bedford MA 0 1730 USA). 91/C3706. Salit M. L. Travis J. C Wythoff B. J. Strategies for extracting chemical information from an ICP-FTS system (Natl. Inst. Stand. Technol. Inorg. Anal. Res. Div. Chem. Bldg. Room B-222 Gaithersburg MD 20899 USA). 91/C3707. Cassagne P Fry R. C. Towards an expert system for ICP-AES-defining a minimum set of prominent lines satisfying 50 selected applications (Applied Research Labs. En Vallaire Ecublens 1024 Switzerland). 91/C3708. Bi C.-l. Vela N. P Evans E. H. Cmso J. A. Inductively coupled plasma atomic emission spectro- metry for high-resolution gas chromatographic detec- tion of organolead compounds (Dept. Chem. Univ. Cincinnati Cincinnati OH 4522 1-0 172 USA). 9K3709. Barnes R. M. Jacksier T.Jahl M. J. Sealed inductively coupled plasma discharge for gas analysis (Univ. Massachusetts Dept. Chem. Lederle Grad. Res. Center Towers Amherst MA 01003-0035 USA). 91/C3710. Strange C. M. Marcus R. K. Particle beam sample introduction to a glow discharge device with a resis- spectrometry,- (Dept. Chem. Indiana Univ. Blooming- ton IN 47405 USA). 9 1 /C372 1. Brushwyler K. R. Hieftje G. M. Multichannel atomic emission spectrometry with a Grimm-type glow dis- charge source (Dept. Chem. Indiana Univ. Blooming- ton IN 47405 USA). 9 1x3722. Miyama T. Ohmori Y. Yuasa S. Analysis of gaseous elements by optical emission spectrometry (Shimadzu Corp. 1 Nishinokyo-Kuwabaracho Nakagyo-ku Ky- oto 604 Japan). 91/C3723. Lazik C. Marcus R. K. Analytical characterization of a radiofrequency powered glow discharge atomic emis- sion source (Dept.Chem. Howard L. Hunter Chem. Labs. Clemson Univ. Clemson SC 29634- 1905 USA). 91K3724. Cable P. R. Marcus R. K. Radiofrequency glow discharge device with an external sample mount geo- metry for mass spectrometric analysis (Dept. Chem. Howard L. Hunter Chem. Labs. Clemson Univ. Clemson SC 29634- 1905 USA). 91K3725. Webster G. K. Carnahan J. W. Atomic emission detection for supercritical fluid chromatography using a moderate power helium microwave-induced plasma (Dept. Chem. Northern Illinois Univ. DeKalb IL 601 15 USA). 91/C3726. Belmore R. J. Jarrell R. F. Hodges C. E. Utilizing graphics capabilities of a computer-controlled spark328R 91/C3727. 91K3728. 9 1/C3729. 91/C3730. 9 1 /C3 73 1. 91IC3732.91/C3733. 9 1/C3734. 9 1/C3735. 91/C3736. 91/C3737. 9 1/C3738. 91/C3739. 9 1/C3740. 9 1/C374 1. JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY DECEMBER 199 1 VOL. 6 spectrometer for better metals analysis (Thermo Jarre11 Ash 8E Forge Parkway Franklin MA 02038 USA). Araki S. Sato S. Okano M. Ogura M. Analysis of electroplated terne steel sheet by glow discharge emis- sion spectrometry (NKK Corp. Fukuyama Works 1 Kokan-cho Fukuyama 72 1 Japan). Castillano T. L. Determination of regulatory method detection limits by GC-MS IC GFAA and ICP for refinery waste water (Chevron USA 324 West El Segundo Blvd El Segundo CA 90245 USA). Faires L. M. Patton C. J. Environmental applica- tions of chelation concentration-inductively coupled plasma mass spectrometry (US Geol. Surv.Natl. Water Quality Lab. 5293 Ward Rd Arvada CO 80002 USA). Bullock A Charalambous P. Milton D. Precision and accuracy measurements using a VG Gloquad (VG MicroTrace Ion Path Rd. Three Winsford Cheshire CW7 3BX UK). Clark J. Ronan G. Greb U. Bullock A. Trace analysis of insulating and semi-insulating materials by GDMS (VG MicroTrace Ion Path Rd. Three Wins- ford Cheshire CW7 3BX UK). Smith T. Advanced alloy grade classification technique for metals arc spectrometers (Arun Technology Unit 16 Station Rd. Southwater West Sussex RH13 7UD UK). Driscoll J Wood C. Ekmijian E. Powell T. Tech- niques for field screening of lead in paint by X-ray fluorescence (HNU Systems 160 Charlemont St. Newton Highlands MA 02 16 1-9987 USA). Shimura M. Akiyoshi T. Tsukada K. Measurement of paint film thickness on steel by XRF spectrometry (Chem.Anal. Branch Keihin Works NKK Corp. Minamiwataridacho 1 - 1 Kawasakiku Kawasaki 2 10 Japan). Puchyr R. F Raja R. New method for chromium determination in chrome-phosphate treatment of ah- minium surface (American Natl. Can Company 433 N. Northwest Highway Barrington IL 60010 USA). Knowles M. Delles F. Hoobin D. L. Champion B. R. Howell M. J Automation of an atomic absorption spectrometer for on-stream analysis of total iron in zinc sulphate solutions (Varian Optical Spec- troscopy Instruments 201 Hansen Court Suite 108 Wood Dale IL 601 9 1 USA). Massart D. L. Smeyers-Verbeke J. Van Keerberghen P. Penninckx W. Wan& X.-n. Rius X. de Kleijn J. P. Spanjen L. G. C. W. Expert systems for method development and validation in atomic absorption (Vrije Univ.Brussel Laarbeeklaan 103 B-1090 Brus- sels Belgium). Roehl R. Alforque M. M. Riviello J. Joyce R. J. Organic and inorganic arsenic speciation and quantita- tion using ion chromatography and ICP-MS detection (California Public Health Found. California Dept. Health Serv. Hazardous Mater. Lab. 21 5 1 Berkeley Way Berkeley CA 94704 USA). Manabe R. M. Siriraks A. Riviello J. Chelation sample preconcentration for the analysis of water- miscible organic solvents by inductively coupled argon plasma emission spectroscopy (Thermo Jarrell Ash 175 Jefferson Dr. Menlo Park CA 94025 USA). Tyler G. Nham T. T. Brodie K. Determination of trace elements in organic samples in ICP-ES with the use of oxygen (Varian Optical Spectroscopy Instru- ments 201 Hansen Court Suite 108 Wood Dale IL 60191 USA).Lana= J. A. Direct ultratrace analysis of brines via inductively coupled plasma optical emission spectros- copy (Anal. and Eng. Sci. At. Spectrosc. Lab. Dow 91/C3742. Siriraks A. Riviello J. Harrold M. Manabe R. Elimination of iron and aluminium as spectral interfer- ences in sample matrices by chelation sample pre- treatment inductively argon plasma emission spectros- copy (Dionex Corp. 1228 Titan Way Sunnyvale CA 94086 USA). 91/C3743. Eastgabe A. R. Vogel W. ICP sample desolvation stability (Fisons-ARL En Vallaire 1024 Ecublens Switzerland). 91/C3744. Patrick F. E. Gibson J. E. Kandetzki P. E. Charac- terizing phosphate rock using ICP (IMC Fertilizer Inc. P.O. Box 867 Bartow FL 33830 USA).91/C3745. Matthes S. A. Rapid determination of Au Pt and Pd in ore concentrates by a standard additions method utilizing a high resolution scanning sequential ICP (US Dept. Interior Bur. Mines Albany Res. Center 1450 Queen Ave. SW Albany OR 97321 USA). 91/C3746. Tyler G. Finotello F. Wilson P. Nham T. Dynamic off-peak background correction (OBC) for low level analysis in geological samples by inductively coupled plasma optical emission spectrometry (ICP-OES) (Varian Optical Spectroscopy Instruments 20 1 Hansen Court Suite 108 Wood Dale IL 60191 USA). 9 K3747. Foster R. W. Grindle A. E. Schleicher R. G. Sotera J. J. Spectrographic-like analysis of environmental samples using a programmable ICP (Thermo Jarrell Ash 8E Forge Parkway Franklin MA 02038 USA). 9 1/C3748.Borer M. W. Hieftje G. M. Extraction-microwave plasma source for atomic emission spectrometry (Indi- ana Univ. Dept. Chem. Bloomington IN 47405 USA). 911C3749. Olson L. K. Vela N. P. Carey J. M. Caruso J. A. Determination of halogenated compounds using super- critical fluid chromatography-plasma spectroscopy (Dept. Chem. Univ. Cincinnati Cincinnati OH 45221 USA). 91/C3750. Jones K. J. Carnahan J. W. Mechanistic studies of non-metal excitation in the helium microwave-induced plasma (Dept. Chem. Northern Illinois Univ. De- Kalb 1L 601 1 5 USA). 91/C3751. Ruiz A. I. Zhang H.-q. Zhu G.-x. Browner R. F. Vaporization processes in particle beam interface-low pressure MIP sample introduction (Sch. Chem. and Biochem. Georgia Inst. Technol. Atlanta GA 91/C3752. Zhu G.-x.Zhang H.-q. Browner R. F. Low-power microwave-induced plasma with aqueous sample intro- duction (Sch. Chem. and Biochem. Georgia Inst. Technol. Atlanta GA 30332-0400 USA). 9 1/C3753. Msimanga N. D. Browner R. F. Effects of solvent and liquid flow on a proposed model for pneumatic nebuliz- ' ers (Sch. Chem. Georgia Inst. Technol. Atlanta GA 30332 USA). 9 1/C3754. Chan S.-k. Investigation on ultrasonic nebulization of high solid samples into an inductively coupled plasma (CETAC Technologies 302 South 36th St. Suite 101B Omaha NE 68 13 1 USA). 91/C3755. Tan M. A. Zhu G.-x. Browner R. F. Characteriza- tion and optimization of ultrasonic nebulizers and their desolvation systems for inductively coupled plasma atomic emission spectrometry (Sch. Chem. and Bio- chem. Georgia Inst.Technol. Atlanta GA 91/C3756. Bernhard A. E. Batie W. Kahn H. L. Direct depth profile analysis of coatings with fast-sequential AA equipment (Analyte Corp. 910 Chevy Way Medford OR 9750 1 USA). 9 1/C3757. Chan S.-k. Kwan W. N. Analysis of crude oils using an inductively coupled plasma with ultrasonic nebuli- zation (CETAC Technologies 302 South 36th St. 30332-0400 USA). 30332-0400 USA). USA Freeport TX 77541 USA). Suite 101B Omaha NE 68131 USA).JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY DECEMBER 1 99 1 VOL. 6 329R 911C3758. 9 1lC3759. 9 11C3760. 9 1 lC376 1. 911C3762. 9 1lC3763. 9 1lC3764. 911C3765. 9 113766. 9 113767. 9113768. 9113769. 9 113770. 9 11377 1. 9113772. Xu N Majidi V. Ehmann W. D Markesbery W. R. Determination of aluminium in brain tissue (Dept.Chem. Univ. Kentucky Lexington KY 40506 USA). Klemp M Puig L Trivedi K Sacks R High-speed vacuum-outlet capillary GC with element-selective plasma detection (Dept. Chem. Univ. Michigan Ann Arbor MI 48 109 USA). Broadhead My Fredeen K. J Analysis of geological samples by laser sampling ICP mass spectrometry (Chem. and Mineral. Sew. 445 West 2700 South Salt Lake City UT 641 15 USA). Sullivan J. J. Quimby B. D. Free M. 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Chem. and Appl. Chem. Univ. Salford Salford M5 4WT UK). Harriott My Tborbum Bums D. Chimpalee N Applications of a slotted tube atom trap and flame atomic absorption spectrometry determination of anti- mony in copper-based alloys after hydride generation Anal. Proc. 1991,243,193. (Dept. Anal. Chem. Queen’s Univ. Belfast Belfast BT9 5AG UK). Harriott M. Thorburn Bums D. Donaghy C. Deter- mination of total tin in acid digests of seaweed and sediments using hydride generation and quartz-tube electrothermal atomization Anal. Proc. 199 1,28 194. (Dept. Anal. Chem. Queen’s Univ. Belfast Belfast BT9 5AG UK). Jakubowski N. Contributions in the field of atmo- spheric plasma source mass spectrometry J.Anal. At. 27599-3290 USA). 9 113773. 9 113774. 9 113775. 9 113776. 9113777. 9113778. 9113779. 9 113780. 9113781. 9113782. 9 113783. Spectrom. 1991 6 249. (Inst. Spektrochem. und angew. Spektrosk. Postfach 10 13 52 D-W4600 Dort- mund Germany). Travis J. C. Turk G. C. Watters R. L Jr Yu L.-j. Blue J. 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Glow-discharge spectroscopy Hyomen Gijutsu 1990 41 502.(Kawasaki Steel Chiba 260 Japan). Maeda S. Surface analysis Hyomen Gijutsu 1990,41 1322. (R and D Lab. 11 Nippon Steel Sagamihara 229 Japan) . Uchiyama K. Tanimura H. Ishimoto K. Sasaki M. Tamaki Y. Ochiai M. Kobayashi Y. Kada~rm E. Terasita S. Michiura J Metal concentrations in gallstones measured by inductively coupled plasma338R 9 1 /4007. 91/4008. 9 1/4009. 9 1/40 10. 91/4011. 9 1/40 12. 9 1 /40 1 3. 9 1/4014. 9 1/40 15. 9 1/4016. 9 1 /40 1 7. 9 1/40 18. 91/4019. 91/4020. JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY DECEMBER 199 1 VOL. 6 spectrometer Zgaku no Ayumi 1990 154 135. (Dept. Gastroenterol. Surg. Wakayama Med. Coll. Wakay- ama 640 Japan). Perez Gallego J. J. Iglesias J. M. Vergara A. Del Barrio S. Alvarez A Inductively coupled plasma atomic emission spectrometry in the quantitative ana- lysis of industrial argdlsceous minerals sepiolite Znd.Min. (Madrid) 1989 31(290) 27. (Spain). Lal M. Choudhury R. K. Studies of trace elements in biological systems by energy dispersive X-ray fluores- cence (EDXRF) and proton induced X-ray emission (PIXE) methods Indian J. Phys. B 1991 65 30. (Nucl. Phys. Div. Bhabha At. Res. Cent. Bombay 400 085 India). Ramanan V. Reddy G. S. Rao C. R. M. Ganesh S. Determination of gold in geological materials by cold extraction and atomic absorption method Indian Miner. 1989 43 154. (Chem. Div. Geol. Surv. India Madras 600032 India). Martinez-Tarazona M. R. Palaaos J. M. Tascon J. M. D. SEM-EDX characterization of inorganic con- stituents of brown coals Ins?.Phys. ConJ Ser. 1990 98 327. (Inst. Nac. Carbon Derivados CSIC Oviedo 33080 Spain). Valcarcel M. Gallego M. Montero R. Indirect continuous automatic determination of pharmaceuti- cals by atomic absorption spectroscopy J. Pharm Biomed. Anal. 1990,8,655. (Dept. Anal. Chem. Univ. Cordoba Cordoba 14004 Spain). Ivanenko V. V. Kovalenko V. V. Kustov V. N. Grigor’ev A. I. Metelev A. Yu. Nuclear methods of elemental analysis of ocean bottom sediments J. Radioanal. Nucl. Chem. 1991 147 321. (Inst. Chem. Vladivostok USSR). Pillay A. E. Peisach M. Zeolite analysis PIXIE XRF or neutron activation J. Radioanal. Nucl. Chem. 1991 153 75. (Dept. Chem. Univ. Witwatersrand 2050 South Africa). Amemiya T. Itoh K. Spzaki S. Watanabe Y. Contents of nickel and cobalt in cosmetics Kenkyu Nenpo-Tokyo-toritsu Eisei Kenkyusho 1990 (41) 75.(Tokyo Metrop. Res. Lab. Public Health Tokyo Japan). Arzamastsev A. P. Bykov A. V. Lependina 0. L. Listov S. A Nikolaev V. I. Petrov N. V. Rusakov V. S. Filippova E. V. Chuppin A. V. Shul’gin V. I. Methods for identifying iron in drugs Khim.-Farm Zh. 1990 24 73. (Pharm. Fac. I. M. Sechenov First Moscow Med. Inst. Moscow USSR). Chmilenko F. A Baklanov A. N. Chuiko V. T. Determination of trace heavy-metal impurities in natural brines with ultrasonic sample preparation Khim. Tekhnol. Vody 1990 12 1039. (Dnepropetr. Gos. Univ. Dnepropetrovsk USSR). Koch K. H. Oblq K. Flock J. Rationalization of multi-elemental analysis by application of X-ray fluo- rescence analysis Labor-Praxis 1990 14 1022. (Ho- esch Stahl A.-G.D-4600 Dortmund 1 Germany). Lickl E. Atomic absorption spectroscopy and food analysis Lebensm.- Biotechnol. 1990,7 166. (HBLVA Chem. Ind. 1170 Vienna Austria). Arikawa Y. Iwasaki M. Determination of selenium in biological samples by hydride generation atomic absorption spectrometry after combustion in high- pressure oxygen Nippon Kagaku Kaishi 199 1 (2) 120. (Fac. Home Econ. Japan Women’s Univ. Tokyo 112 Japan). Sugimoto F. Maeda Y. Azami T. Environmental analysis. L. Graphite furnace atomic absorption spec- trometry of trace amounts of cadmium in environmen- tal water by zinc-diethyldithiocarbamate coprecipita- 91/4021. 9 1/4022. 91/4023. 9 1/4024. 9 1 /4025. 9 1/4026. 91/4027. 91/4028. 9 1/4029. 9 1/4030. 91/4031. 9 1/4032. 9 11403 3. 9 1/4034. 9 114035. tion method Nippon Kaisui Gakkuishi 1990 44 124.(Dept. Appl. Chem. Himeji Inst. Technol. Himeji 67 1-22 Japan). Kawamara T. Maeyama S. Oshima M. Ishii Y. Miyahara T. Solid-surface analysis beam line with a grating-crystal monochromator at the Photon Factory Nucl. Znstrum. Methods Phys. Res. Sect. A 1989 275 462. (NTT Appl. Electronics Lab. Tokyo 180 Japan). Rahman S. Khalid N. A h e d R. Qureshi I. H. Determination of lead and cadmium in pulses and cereals by atomic absorption Pak. J. Sci. Ind. Res. 1990 33 85. (Nucl. Chem. Div. Pakistan Inst. Nucl. Sci. Technol. Islamabad Pakistan). Kohno M. Tamara K. Azuma J. Total analysis of major constituents in soils by X-ray fluorescence spectrometry using calibration lines prepared with soil reference materials (NDG- 1 - 8) Pedorojisuto 1990 34 37.(Agric. Coll. Kobe Univ. Kobe Japan). Valdes E. V. Leeson S. Research note use of X-ray fluorescence spectrosopy to analyse calcium and phos- phorus in poultry feeds Poult. Sci. 1990 69 1803. (Dept. Anim. Poult. Sci. Univ. Guelph Guelph Ontario N 1 G 2W 1 Canada). Khodonov M. T. Sal’nikov V. D. Lysyakova V. I. Karpov Yu. A Mathematical certification of atomic emission analysis with an induction plasma Probl. Sovrem. Anal. Khim. 1989,6 26. (USSR). Drobyshev A. I. Layer-by-layer analysis by atomic emission spectroscopy Probl. Sovrem. Anal. Khim. 1989,6 39. (USSR). Panichev N. A Lowering the limits of detection of atomic absorption analysis by concentrating the ele- ments to be determined in an electrothermal atomizer Probl. Sovrem. Anal. Khim.1989 6 72. (USSR). Simon L. Radionuclide X-ray fluorescence analysis in coal mining-present status Radioisotopy 1990 31 193. (Ustav Geol. Geotech. CSAV Prague Czecho- slovakia). Tye C. T. Henry R. Abell I. D. Gregson D. Analysis of elements without dissolving the solids laser ablation ICP-MS rapidly identifies major minor and trace elements with ppb detection limits Res. Dev. 1989,31 76. (VG Instruments Inc. Danvers MA 01923 USA). Kobayashi R. Imaizumi K. Determination of cad- mium cobalt copper nickel and lead in urine by inductively coupled argon plasma emission spectro- metry after solvent extraction Sangyo Igaku 1990,32 272. (Occup. Health Serv. Cent. Jpn. Ind. Saf. Health Assoc. Tokyo 108 Japan). Homma S. Shimojo N. Yamaguchi S. Nondestruc- tive X-ray fluorescence spectroscopic imaging of trace elements on methylmercury and selenium adminis- tered guinea pigs Sangyo Zgaku 1990,32,276.(Univ. Tsukuba Tsukuba 305 Japan). Doerffel K. Niedtner R. Hejtmanek M. Ksandr Z. Tagle I. Possible improvement of detection sensitivity in flame AAS Sb. Vys. Sk. Chem.-Technol. Praze Anal. Chem. 1989 H23 89. (Sekt. Chem. Tech. Hochsch. ‘Carl Schorlemmer’ Leuna-Merseburg 0-4200 Merse- burg Germany). Bastin G. F. Heijligers H. J. M. Quantitative electron probe microanalysis of ultralight elements (boron-oxygen) Scanning 1990 12,225. (Cent. Tech. Ceram. Univ. Technol. 5600 MB Eindhoven The Netherlands). Casuccio G. S. Gmelich F. A. Hamburg G. Huggins F. E. Nissen D. A. Vleeskens J. M. Coal mineral analysis a check on interlaboratory agreement Scann- ing Microsc.1990 4 227. (R.J. Lee Group Monroe- ville PA USA). Ephraim J. H. Mathuthu A. S. Marinsky J. A.,JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY DECEMBER 199 1 VOL. 6 339R 9 114036. 9 114037. 9114038. 9 114039. 9 1 /4040. 9 1 I404 1. 9 114042. 9114043. Complex forming properties of natural organic acids. Part 2. Complexes with iron and calcium SKB Tech. Rep. 1990 90 21. (Dept. Water Environ. SOC. Linkoeping Univ. Linkoeping Sweden). Laird D. A. Dowdy R. H. Munter R. C Suspension nebulization analysis of clays by inductively coupled plasma atomic emission spectroscopy Soil Sci. SOC. Am. J. 1991 55 274. (Soil Water Manage. Res. Unit ARS USA). Taniguchi K Ninomiya T. Total reflection X-ray fluorescence spectrometry Tetsu to Hagane 1990 76 1228.(Fac. Eng. Osaka Electro-Commun. Univ. Ney- agawa 572 Japan). Nakazaki M. Shimishi K Determination of tin in blood Toyama-ken Eisei Kenkyusho Nenpo 1989 13 230. (Toyama Inst. Health Toyama 939-03 Japan). Kubo My Determination of nickel in ferronickel by atomic absorption spectrometry Toyama Kogyo Koto Senmon Gakko Kiyo 1990,24,3 1. (Toyama Natl. Coll. Tech. Toyama Japan). Lamen J Milman N Leth P Asnes S. Elements in normal and cirrhotic human liver. Potassium iron copper zinc and bromine in cellular and connective tissue fractions measured by X-ray fluorescence spec- trometry Trace Elem. Med. 1990,7 1 18. (Dept. Phys. R. Vet. Agric. Univ. Copenhagen Denmark). Lisetskaya G. S Bilenko N. S. Zaets V. V. Atomic absorption determination of cobalt in hypochlorite solutions Ukr.Khim. Zh. 1990 56 951. (GosNII- Khlorproekta Kiev USSR). Schroen W Eismann G Danzer K Thermochemi- cal reaction in trace element determination in alumina by atomic emission spectroscopy Wiss. Z. -Friedrich- Schiller- Univ. Jena Naturwiss. Reihe 1990 39 276. (Sekt. Chem. Friedrich-Schiller-Univ. Jena Ger- many). Zhu L. Yang Y.-z Liu T Quantitative electron probe microanalysis for multi-element microparticle specimens Wuhan Dame Xuebao Ziran Kexueban 1989 (3) 75. (Cent. Anal. Meas. Wuhan Univ. Wuhan China). 9 114044. 9 1 14045. 9 1 f 4046. 9114047. 9 114048. 9 114049. 9 1 f4050. Berthold T. Jagodzinski H. Analysis of the distribu- tion of impurities in crystals by anomalous X-ray scattering 2. Kristallogr. 1990 193 85. (Inst. Kristal- logr. Mineral. Univ. Muenchen D-8000 Munich 2 Germany).Hara S. Hayashi N. Hirano S. Zhong X. N. Yasuda S. Determination of germanium in some plants and animals 2. Naturforsch. C Biosci. 1990 45 1250. (Fac. Integr. Arts Sci. Hiroshima Univ. Hiroshima 730 Japan). Mende H. E. Spitzbart H. Sieke V. Vogel C. Concentrations of sodium potassium magnesium and calcium in vaginal fluid Zentralbl. Gynaekol. 1990 112 1175. (Win. Gynaekol. Geburtshilfe Med. Akad. DDR-5020 Erfurt Germany). Korneev V. A. Ivanov V. K. Pchelintsev A. M. Odinochkina T. F. Agrafenin A. V. Quantitative emission spectral analysis without standards in crimi- nal forensic and forensic-medical practice Zh. Prikl. Spektrosk. 1990 52 535. (Sci.-Res. Inst. Forensic Med. Moscow USSR). WP J. Zhang M Ma Y. Jiao Q.-g. Hou H. Determination of plasma zinc levels after administra- tion of controlled-release tablets of zinc sulphate and observations of its side-effects on digestive tract Zhongguo Yiyao Gongye Zazhi 1990 21 393.(Dept. Dosage Forms Shanghai Inst. Pharm. Ind. Shanghai 200433 China). Tamm R. Roedel G. Furnace for electrothermal atomization of samples in atomic absorption spectros- copy Eur. Pat. Appl. EP 381 948 (Cl. GOlN21/74) 16 Aug 1990 DE Appl. 8 901 529 10 Feb 1989; 12 pp. (Bodenseewerk Perkin-Elmer D-7770 ijberlingen Germany). Ortner H. Hlavac R. Wilhartitz P. Sychra V. Doled J. Puschel P. Atomizer made of a high- melting metal for flameless atomic absorption spectros- copy Eur. Pat. Appl. EP 377 253 (Cl GOlN21/74) 11 Jul 1990 CS Appl. 89175 04 Jan 1989; 5 pp. (Metallwerk Plansee A-6600 Reutte Austria).

ISSN:0267-9477    

DOI:10.1039/JA991060323R

出版商:RSC    

年代:1991

数据来源: RSC

摘要:

JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY DECEMBER 199 1 VOG. 6 587 Conference Report IUPAC International Congress on Analytical Sciences (ICAS ’91)-Joint and Satellite ‘Kitami’ Conference-New Approaches in Trace Element Analysis by Atomic Spectroscopy September 2nd-4thY 1991 Kitami Japan The joint and satellite ‘Kitami’ confer- ence on ‘New approaches in trace element analysis by atomic spectro- scopy’ was held in the northern Japanese city of Kitami attracting about 100 delegates mainly from Ja- pan. It was organized jointly with the 199 1 IUPAC International Congress on Analytical Sciences. The confer- ence was intended to focus on the progress of solid sampling with atomic spectroscopic methods and the prepa- ration and analysis of reference ma- terials. The scientific sessions consisted of invited and contributed oral papers with discussion time for themes of particular importance.The invited speakers from Japan Europe and North America presented lectures on a variety of analytical techniques and it soon became clear that the content of the conference was much wider than originally suggested. The programme for the first day was broken into five short consecutive ses- sions each with a new chairman. The first lecture in session 1 (instrumenta- tion and methodology) was given by K. Kitagawa who described some novel techniques for direct simulta- neous determination of trace elements in solids. These included a multi- element atomic absorption spectro- meter which used up to ten hollow cathode lamps a high frequency Ar or He discharge around a graphite cup electrode containing the sample and a separative column atomizer which was an electrically-heated glassy car- bon tube packed with graphite par- ticles.The second lecture of the ses- sion given by H. Okochi discussed the application of the platform technique for direct analysis of metallic sample solutions by electrothermal atomic absorption spectrometry (ETAAS) a technique that was developed in order to avoid the use of separation procedures which could lead to con- tamination. An overview to the state-of-the-art in reaching accurate results with ETAAS and solid sampling was given by U. Kurfurst in the second session (Theory and ETAAS). Appropriate methods of calibration and statistical treatment of the data were considered. K.Yasuda described the measurement of atomic vapour temperature in a graphite furnace using two-line atomic absorption and the effect of a Pd chemical modifier on these tempera- tures K. Hirokawa described some of the problems in the direct determina- tion of metal samples by ETAAS and the effect of chemicals modifiers on element signal behaviour. In session three (Furnace and Sput- tering/Plasma Atomic Emission Spec- trometry) R. E. Sturgeon described the novel technique for ultra-trace analy- sis of furnace atomization plasma emission spectrometry in which a graphite furnace is intimately linked with an atmospheric r.f. inert gas plasma in a single unit. P. Win de- scribed the control of reactive sputter- ing processes by plasma emission spec- troscopy for the deposition of thin films in the production of semiconduc- tors.Changes in the intensity of the emission were used to monitor changes in sputtered deposition which could be automatically corrected by changing reactive gas flows. Session 4 [Laser Ablation Induc- tively Coupled Plasma] (LA-ICP) was the longest of the conference reflecting the interest in this technique. C. W. McLeod described some results of a study into the feasibility of using laser ablation LA-ICP-AES for the analysis of oils. Advantages of the method include avoiding the use of organic solvents and elimination of viscosity related matrix effects. N. Furuta reported on some fundamental studies of LA-ICP-AES and suggested that the elemental emission signal was not strongly dependent on the length of tubing connecting the ablation cell and the ICP and the weakest point of LA was poor precision due to sample inhomogeneity and laser-sample in- teraction.K. Dittrich described a laser-furnace atomization non-ther- ma1 emission spectrometry (FANES) system combined with an Cchelle spec- trometer for trace multi-element deter- minations in solids. The use of a laser overcomes the 3000 K temperature limitation of conventional FANES. J. G. Williams described the potential of solid sample introduction ICP mass spectrometry (MS). The application of slurry nebulization and laser ablation to the analysis of geological materials was assessed and it was concluded that accurate and precise results could be obtained but only under very con- trolled analytical conditions. C.J. Park showed that Fe Br and Se iso- tope ratios could be determined with microwave-induced plasma mass spec- trometry (MIP-MS). It was found that the alignment of the plasma with the sampling orifice had to be optimized for each element studied. In session 5 (Biological Sample Ap- plication) N. J. Miller-Ihli highlighted the possibilities of determining trace metals in biological materials by slurry ETAAS. Ultrasonic agitation was used to ensure adequate mixing of slurries suspended in a mixture of 5% nitric acid and 0.04% Triton X- 100. G. V. Iyengar surveyed the sampling and processing of biomater- ials for elemental assays and indi- cated many of the key factors in- volved in this very important area reference material validation. In the final paper of the day I.Atsuya re- ported on the direct determination of Co and Ni in powdered biological samples by ETAAS with a pre-ash- ing-solid sampling technique which reduced the mass of the sample to 20% of the original. The second day began with session 6 (Enhancement of Sensitivity) and Y. Thomassen describing the use of radioactive chemical modifiers in an attempt to monitor Sn losses during the analysis of biological materials. K. Matsumoto showed that the sensi- tivity of ETAAS for Sn and several other volatile elements could be en- hanced by the use of Pd as Pd(N03)2 and albumin and that a mixture of the two was particularly effective. In session 7 (X-ray Fluorescence and Food Applications) S. Ikeda showed that metallic elements with ppb con- centrations could be determined in 10 pl of liquid spread on the surface of a silicon wafer by total reflectance X-ray fluorescence but that only ppm levels could be detected from powdered samples spread on the wafer.K. Taki- yama described .three wet ashing and one extraction method for food sub- stance pre-treatment in order to re-588 JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY DECEMBER 199 1 VOL. 6 move the organic component prior to analysis by AAS. In session 8 (Blood and Serum Ap- plications and Reference Materials) A. Hulanicki indicated some of the problems of calibration involved in the determination of trace metals such as Pb Cd Co Mn A1 and Cr in serum by ETAAS. Y. Hirano reported on the determination of trace metals in bio- logical samples by platform ETAAS and showed that interferences from organic substances and electrolytes could be overcome by use of a Pd chemical modifier.S. Suzuki described the highly accurate and precise deter- mination of 30-54 elements in several NIES and NIST reference materials using instrumental neutron activation analysis. To start session 9 (Environmental Sample Application and Metal Atom- izers) K. Ohta reported on the direct determination of Mn in slurried pow- ders of biological materials by ETAAS with a molybdenum tube atomizer and thiourea as a chemical modifier. About 4% hydrogen was added to the argon purge gas to prevent degradation of the atomizer by oxygen. J. Fleckenstein reported on the successful use of a nickel atomizer for the determination of Hg in solid environmental samples. With this method it was possible to assess whether preparation methods were causing loss of Hg from the sample.T. Nakahara began session 10 (New Techniques in ICP and ICP-MS) with a description of a continuous flow gas- phase sample introduction system for the direct and indirect determination of iodine by atmospheric pressure He MIP-AES. Results obtained by this method for the analysis of sea-waters were in good agreement with pre- viously reported values. K. Jin continued the session with a report on the determination of inorganic and methylated Ge species in natural and waste waters at sub-picogram levels using a combined hydride-generation cold-trap ICP-MS method. Minimal sample pre-treatment was required and (10 ml of sample. M. Kubota described some of his studies on ana- lytical characteristics of a tungsten furnace electrothermal vaporization ICP-MS system.Parameters such as analyte signal the effect of introducing hydrogen and memory effects were all discussed. Detection limits for rare earth elements were reported in the range 0.1-0.6 pg ml-l. In the final paper of this session M. Yanagisawa reported on the direct analysis of ceramic powders by slurry nebuliza- tion ICP-MS and ICP-AES. In ceramic processing raw ceramic powders are milled however wear materials from the mill can cause contamination which has to be monitored. Slurry nebulization offered the potential for rapid evaluation without dissolution of the ceramic powders. Results from slurry nebulization were in good agree- ment with those obtained from samples prepared with a bomb digestion.In the final session of the meeting (New Sample Treatment) Y. Dokiya reported on a comparison of water samples taken from Mount Fuji and the Himalayas. Generally higher values of sulphate and nitrate were obtained from Himalayan samples whereas the ratio of Br to C1 (which is an indicator of fossil fuel pollution) was higher in some samples taken from Mount Fuji. Finally J. Holcombe gave a paper on the novel use of immobilized algae and yeast metallothionein for the precon- centration of metal ions in aqueous solutions. Examples were given to il- lustrate the specificity and extraction efficiencies of the technique. The effec- tive preconcentration of the algae sys- tem was said to be 100 1. In addition to the conference lec- tures public lectures were given by Dr. Y. Iyengar and Professor H. Hara- guchi to which many of the citizens of Kitami attended. Several excellent re- ceptions were held during the confer- ence and also an excursion to the beautiful Akan National Park. This gave the non-Japanese delegates a chance to enjoy both the wonderful hospitality of the hosts and the local landscapes. I am sure that I will not be alone in expressing my gratitude to Professor I. Atsuya and members of the organizing committee advisory board and scientific committee for their efforts to ensure smooth running of the scientific and social programmes. John G. Williams NERC ICP-MS Unit Royal Holloway and Bedford New College Egham Surrey UK

ISSN:0267-9477    

DOI:10.1039/JA9910600587

出版商:RSC    

年代:1991

数据来源: RSC

摘要:

588 JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY DECEMBER 199 1 VOL. 6 Conferences and Meetings Third Durham International Confer- ence on Plasma Source Mass Spectro- metry September 13- 18 1992 University of Durham Durham UK This conference sponsored by VG Elemental Cheshire and organized in conjunction with the University of Durham aims to provide a platform for the stimulation and interchange of ideas and experiences in plasma source mass spectrometry and asso- ciated topics. During the 1992 sym- posium particular emphasis will be placed on inductively coupled plasma source mass spectrometry (ICP-MS) and glow discharge mass spectrometry (GDMS) techniques. Call for Papers The conference will consist of invited and open lectures discussion sessions and poster presentations. Papers are invited on all aspects of plasma source mass spectrometry with particular emphasis on ICP-MS and GDMS techniques.Authors wishing to participate in this event should contact Dr. J. G. Holland Department of Geological Sciences The University Science Lab- oratories South Road Durham DH1 3LE UK. For further information please also note the following addresses. Editorial contact Helen Samuel Strategic p.r. Newton House 38 Combe Park Wes- ton Bath BA1 3NR UK. Telephone 0225 480667. For conference informa- tion Grenville Holland Department of Geological Sciences The Univer- sity Science Laboratories South Road Durham DHl 3LE UK. Tele- phone 091 374 2526. Euroanalysis VIII European Confer- ence on Analytical Chemistry September 5-1 1 1993 University of Edinburgh Edinburgh UK The Working Party on Analytical Chemistry of the Federation of Euro- pean Chemical Societies and the Ana- lytical Division of The Royal Society of Chemistry announce the eighth tri- ennial European Conference on Ana- lytical Chemistry Euronalysis VIII to be held at the University of Edin- burgh.The Scientific Sessions will be held at the Appleton Tower George Square. Edinburgh is the beautiful and his- toric capital city of Scotland. It is easily reached by road and rail and has an international airport. Participants may be interested to know that the Conference imme- diately follows the world renownedJOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY DECEMBER 199 1 VOL. 6 Edinburgh Festival which will be held from August 15-September 4 1993 (the last performance of the Edinburgh Military Tattoo will be on Saturday August 28).For Euroanalysis VIII the following officers have been appointed Honorary Chairman-E. J. Newman; Conference Presidium-D. T. Burns Belfast (Chairman) J. F. K. Huber Vienna L. Niinistro Espoo and P. G. Zambonin Bari; and Secretary-Miss P. E. Hutchinson London. ScientiJic Programme Euronalysis VIII will cover develop- ments in instrumentation and meth- odology in all areas of analytical chemistry with emphasis on indus- trial biomedical and environmental analysis. The programme will be de- signed to appeal to practising analyti- cal chemists in industry and to those in academia who are teaching and carry- ing out research. The programme will consist of in- vited keynote lectures and contri- buted oral and poster papers.In order to ensure high quality all contributed papers will be refereed. The official language of the Confer- ence will be English; no translation service will be provided. An extensive Exhibition of Books and Journals is planned and will be held in the Appleton Tower close to where the lectures and posters will be presented. Social Programme A comprehensive programme is being planned for participants and accom- panying persons. It will include half- and full-day excursions and various evening events including a whisky tasting and a Buffet Reception at the Royal Museum of Scotland. Accom modat ion Accommodation has been arranged in the Pollock Halls of Residence of the University of Edinburgh. Single room accommodation only will be available.Participants are asked to make their own arrangements if they wish to stay in hotels. A list of local hotels can be obtained from the Conference Orga- nizer; early booking is advised. Call for Papers All those intending to participate in the Conference are welcome to submit papers to be included in the scientific programme. The Scientific Committee will consider papers according to their relevance to the Conference pro- gramme and their scientific content. A listing of possible topics is presented below but other areas of analytical chemistry will also be considered. In order to facilitate the planning of the scientific programme authors are asked to contact the Conference Orga- nizer as soon as possible. Instructions for authors will be given in the second circular; the final date for the receipt of abstracts is November 30th 1992.Some of the topics expected to be covered are Industrial Analysis-validation of analytical measurements process con- trol analysis materials analysis (in- cluding surface analysis) and energy related analysis. 589 Pharmaceutical and Biomedical Analysis-pharmaceutical methods and drug metabolism forensic science bioselective methods and trace ele- ments in medicine. Environmental A nalysis-at mos- phere soils and sediments food and drink and water. Instrumental Techniques-separa- tion science molecular spectrometry atomic spectrometry electroanalytical techniques expert systems and chemo- metrics coupled techniques sensors laser-ba3ed techniques and flow analy- sis. Publications All invited lectures will be published in a collected volume as the Proceed- ings of the Conference. Authors of contributed papes will be invited to submit manuscripts for publication. Abstracts of all papers will be available to registered scientific participants. For further information the Confer- ence Organizer and address for all correspondence are Miss P. E. Hutch- inson Analytical Division The Royal Society of Chemistry Burlington House Piccadilly London W 1 V OBN UK. Telephone 07 1 437 8656; Fax 07 1 734 1227; Telex 26800 1. The Tourist Office in Edinburgh will be happy to assist with the arranging of pre- or post-Conference tours. The address and telephone number are Edinburgh Tourist and Information Centre 3 Princes Street Edinburgh EH2 2QP UK. Telephone 031 557 1700/2707; Fax 031 557 51 18.

ISSN:0267-9477    

DOI:10.1039/JA9910600588

出版商:RSC    

年代:1991

数据来源: RSC

摘要:

JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY DECEMBER 199 1 VOL. 6 589 Future Issues will Include- The following are some of the papers Laser Excited Atomic Fluorescence ium Niobium and Vanadium in Low- to be published in future issues of Spectrometry-M. A. Bolshov s. N. alloyed Steels by Spark Ablation JAAS. Rudnev and B. Hutsch Coupled to Inductively Coupled Plasma Atomic Emission Spectro- Determination of Cadmium Traces by Determination of Aluminium Titan- metry-Aurora Gomez Coedo M. T.590 JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY DECEMBER 199 1 VOL. 6 Dorado Lopez J. L. Jimenez Seco and Analytical Signal by the Limit Dilu- ductively Coupled Plasma Atomic I. Gutierrez Cob0 tion Method-F. Bosch Reig F. Bosch Emission Spectrometric Detection- Mossi V. Peris Martinez and A.Pas- Takunori Kato Takashi Uehiro Akio Preconcentration and Inductively tor Garcia Yasuhara and Masatoshi Morita CouDled Plasma Atomic Emission Spe&rometric Determination of Metal Ions With On-line Chelating Ion Ex- change-V. Porta C. Sarzanini 0. Abllino E. Mentasti and E. Carlini Evaulation of a Low-powered Argon Microwave Plasma Torch Discharge Determination of Rare Earth Elements by Liquid Chromatographic Separa- tion Using Inductively Coupled Plasma Mass Spectrometry-Diane S. Braverman Application of Radioactive Tracers for Analysis of Trace Metals in Volatile Organic Solvents Using Inductively Coupled Plasma Atomic Emission Spectrometry and Inductively Coup- led Plasma Mass Spectrometry-Steve J. Hill James Hartley and Les Ebdon as an Atomizer for the Determination Investigation of Vaporization Pro- of Mercury by Atomic Fluorescence cesses in Electrothermal Atomic Ab- Spectrometry-Yixiang Duan Xi- sorption Spectrometry-Muhammad Atomic Spectrometry angxing Kong Hanqi Zhang Jun Liu M. Chaudhry David Littlejohn and Evaluation of the Influence of Interfer- Determination of Methylmercury Spe- Environmetal Analysis-Malcolm S.ents in Flame Atomic Absorption cies by Capillary Column Gas Chro- Cresser Janet Armstrong John Dean Spectrometry and Correction of the matography With Axially Viewed In- Peter Watkins and Mark Cave and Qinhan Jin John E. Whitley Update Atomic Spectrometry Updates Scientific Meeting 1992 New Approaches to Sample Preparation and Introduction A one day meeting to be held at Newcastle University Newcastle UK March 26 1992 The speakers will include Dr.Julian Tyson Flow Injection Dr. Bemhard Welz In-line preconcentration Using Flow Injection for Atomic Absorption Dr. Helen Crews On-line Microwave DigestionlCoupling HPLC to ICP-MS Dr. John Williams ETV Sample Introduction for Determination of Isotope Ratios by ICP-MS Dr. Ken Jackson Slurry Nebulization Dr. Simon Chenery Direct Analysis by Laser Ablation Coupled to ICPs Dr. Mike Ramsey Statistical Interrelations Between Sampling and Analysis For further details contact Dr. John R. Dean Department of Chemical and Life Sciences Ellison Building Newcastle-upon-Tyne NE1 8ST UK. Telephone 091 232 6002 ext. 35 17. The registrations fees will be €35 for members of The Royal Society of Chemistry €45 for non-members and f20 for students and OAPs. Some student bursaries will be available for this meeting please contact Dr. Mike Ramsey Imperial College Prince Consort Road London SW7 2BP UK for further details.

ISSN:0267-9477    

DOI:10.1039/JA991060589b

出版商:RSC    

年代:1991

数据来源: RSC

摘要:

JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY DECEMBER 199 1 VOL. 6 59 1 Matrix Interferences From Methacrylic Acid Solutions in Inductively Coupled Plasma Mass Spectrometry J. Marshall and J. Franks ICl Wilton Materials Research Centre P.O. Box 90 Wilton Middlesbrough Cleveland TS6 8JE UK It was found that substantial interference effects were present which dramatically reduced sensitivity in the determination by inductively coupled plasma mass spectrometry of trace elements in methacrylic acid solution. Mass bias effects were observed which led to either enhancement or suppression of analyte signals depending on the conditions used and the concentration of methacrylic acid present in solution (1-10% m/v). An instrumental procedure based on optimizing plasma conditions and spectrometer ion optics settings was found to reduce significantly the magnitude of the interference effect.However the use of aqueous calibration standards still gave rise to errors (changes in slope of 1-1 8% in the presence of 5% m/v methacrylic acid) which could not be corrected for by the use of internal standards when using compromise multi-element analysis conditions. The use of the standard additions method under conditions optimized for the matrix is proposed to avoid such calibration problems. Keywords Inductively coupled plasma mass spectrometry; methacrylic acid; organic solvent; matrix interfer- ence; internal standard Inductively coupled plasma mass spectrometry (ICP-MS) is an extremely sensitive technique for the determination of trace elements in liquid samples.' However few publica- tions have appeared relating to the analysis of organic solvents by ICP-MS.Hutton2 investigated the effect of ICP- MS instrument operating conditions on the determination of trace elements in white spirit and fuel oils. It was reported that a substantial increase in power setting of about 500 W (cJ standard conditions for aqueous solu- tions) was required to maximize analyte sensitivity. The spray chamber of the ICP source unit was cooled in order to control solvent loading of the plasma and a low flow rate of oxygen was used to eliminate the build-up of particulate carbon on the sampling orifice. It was observed that polyatomic peaks due to carbon-related species were pre- sent in the spectrum (e.g. I2CO2+ at m/z 44). Hausler3 reported a procedure for the determination of trace elements in petroleum samples by ICP-MS.The samples were diluted with xylene and then aspirated into the plasma using an incident power of 1500 W. Oxygen was added as a diluent gas at a level of about 2% using a mass flow controller in the argon nebulizer gas line via a T-piece inserted after the spray chamber again to eliminate carbon build-up on the sampling cone. Significant background spectral peaks below m/z 60 were observed and these were attributed to carbon-derived polyatomic species. A number of organic solvents such as acids and alcohols are water miscible. Longerich4 has investigated the effect of such solvents on ICP-MS signals. It was found that in a study of nitric acid acetic acid and ethanol as matrix components in aqueous solution enhancement or suppres- sion of analyte signals could be obtained depending on the operating conditions selected.It was recommended that increased plasma power (1500 W) should be used for the aspiration of mixed aqueous-organic solvents. It was found possible to introduce 12Oh v/v ethanol solution continuously over long periods without clogging of the sampling cone by carbon. Optimization of the nebulizer gas flow rate was required for each individual matrix to achieve maximum sensitivity. Evans and EbdonS have investigated the effect of adding 10% v/v propan-2-01 to aqueous solutions on the level of polyatomic ion interferences in ICP-MS. Again high power levels (1 800 W) were used to sustain the plasma and the spray chamber temperature was kept at 5 "C by a recirculat- ing cooler system.Evidence was presented which suggested that the competitive formation of argon-derived poly- atomic species with carbon on addition of propan-2-01 resulted in a reduction in the levels of other potentially intefering species such as A d + . It is clear from the foregoing that the presence of an organic solvent can have a significant effect on the charac- teristics of the ICP as an ion source for mass spectrometry. Methacrylic acid is used as an intermediate in the develop- ment of resins and paints as a solvent in the electronics industry and in the production of acrylic copolymers. Contamination of methacrylic acid by transition metals can give rise to unwanted side effects during processing and consequently methods of analysis which can detect such analytes at concentrations in the parts per billion range in this matrix are required.In the present work a study has been made of the analytical performance of ICP-MS for a range of analytes in the presence of various concentrations of methacrylic acid. Experimental Instrumentation A Sciex Elan 250 ICP mass spectrometer (Perkin-Elmer Beaconsfield UK) was used for all measurements in this work. It is possible to vary the operational parameters of this instrument in order to optimize the ion response for a given analyte. The parameters that have the most signifi- cant effect are those associated with the plasma discharge itself which affects dissociation and ionization character- istics and with the ion lenses of the quadrupole mass / A Quadrupole filter \ Eb Exit lens Sampler cone Fig.1 Schematic diagram of the Sciex Elan 250 ion optics configuration592 JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY DECEMBER 199 1 VOL. 6 spectrometer which affect beam focusing properties and hence detection. A schematic diagram of the ion lens configuration of the Sciex Elan 250 instrument is shown in Fig. 1. Details of the optimization of each of these parameters is given where appropriate in the relevant sections of the text. Sample Preparation Methacrylic acid is a water-miscible liquid at room temper- ature. Samples were simply diluted in the appropriate ratio (usually 1 + 19 by mass) with distilled de-ionized water. Elemental calibration standards were matrix matched for methacrylic acid content in the range 0-100 ng ml-I.However part of the study involved the interpretation of bias resulting from deviation from the known aqueous standard response and so aqueous standard solutions without the addition of methacrylic acid were also prepared in the same concentration range. Results and Discussion Sensitivity Initially the analysis of dilute methacrylic acid was at- tempted by using the standard ICP and spectrometer conditions employed for measurements on aqueous solu- tions as presented in Table 1. As ICP-MS affords high sensitivity for most elements it was convenient to dilute the sample with distilled water prior to analysis and to use calibration standard solutions made up in 5% m/v metha- crylic acid. This dilution factor was selected to give an appropriate analyte concentration range without sacrificing sensitivity unnecessarily.However it was found that a substantial reduction in analyte ion intensity was observed in the presence of 5% m/v methacrylic acid. While this reduction could be compensated for by the use of matrix- matched calibration standards or by standard additions it clearly indicated an interference effect on the determina- tion which adversely affected sensitivity and consequently precision. Experiments were therefore devised to identify the source of the interference effect with a view to improving analytical performance. It is normal practice in ICP-MS to add a known amount of an internal standard element (e.g. rhodium or indium or an element known to be absent in the sample) to calibration standard solutions and samples. Any change in signal intensity for the internal standard element (e.g.resulting from variations in sample transport) is indicative of a change in analytical performance during measurement runs. Such changes are hence automatically accounted for by ratioing the intensity derived for the analyte to that for the internal standard. The success of this approach relies on the assumption that transport and other interference effects influence the intensities of the internal standard and analyte ion to the same extent. Some studies were therefore made on the effect of methacrylic acid in this regard. Rhodium was used as the internal standard element for all measurements. The influence of 0- 10% m/v methacrylic acid on the signal for 50 ng ml-l of rhodium is shown in Fig.2. The ion intensity for rhodium shows a strong dependence on methacrylic acid concentration. A severe J . 3 0 2 4 6 8 10 Methacrylic acid concentration (%I Fig. 2 Effect of methacrylic acid concentration on the signal for the internal standard (Rh). Optimum conditions for aqueous solution measurement were employed as given in Table 1 . The rhodium concentration used was 50 ng ml-* Table 1 ICP-MS operating conditions Perkin-Elmer Sciex Elan 250 ICP-MS Matrox Electronics Systems CCB-7 computer with 10 Mb hard disk Lear Siegler 7 105 intelligent terminal Mass range (mlz) Mass resolution (m/z) Dwell time/ms Measurement time/ms Measurement mode Internal standard Ion optics settings for aqueous solutions- Barrel lens (Eb) Plate lens (E,) Einzel lens (E,) Photon stop (E,) Forward power/kW Coolant gadl min-l Auxiliary gadl min-l Nebulizer gadl min-l Solution uptake rate/ml rnin-l Sampling depthlmm ICP source conditions (optimum for aqueous solutions)- 4-238 0.6 20 200 Peak hopping Rh (mlz 103) Setting Voltage (96 fsd)* range/V 21 0 to +10 18 0 to -60 80 0 to -20 43 0 to -20 0.95 12.0 1.4 1.2 1.3 20 *fsd=Full scale deflection.JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY DECEMBER 199 1 VOL.6 6.5 5.5 - gJ 4.5 J 3.5 2.5 ~ ~ 50 100 150 200 250 mlz Fig. 3 Analyte intensity as a function of the mascharge ratio and the methacrylic acid concentration 0 O ; D 1; 0 2 ; 0,5; and A 10%. Optimum conditions for aqueous solution measurement were employed as given in Table 1. Analyte concentrations were always 100 ng ml-' depression in the signal is observed at acid concentrations of 5% m/v and above which is at the dilution level used to perform the anlysis.Clearly there is a significant matrix effect present which causes a reduction in the ion intensity for rhodium. In order to establish whether the interference was element specific the effect of methacrylic acid on nine analytes chosen to cover the entire mass range of the spectrometer was investigated. The results are presented as a plot of ion intensities for 100 ng ml-l of each analyte versus mass in Fig. 3. The response curves for aqueous and methacrylic acid solutions show the same trends with respect to mass indicating that the interference to a first approximation affects most analytes to the same extent.Generally the signals for each of the analytes is enhanced in the presence of 1-2% m/v methacrylic acid and depressed in the presence of 5-10% m/v acid relative to the corresponding ion intensities for the aqueous standard solution. The drop in intensity at either end of the mass range is typical of the normal response curve for the Elan 250 system. Use of Rhodium as an Internal Standard An estimation of the relative change in ion intensities can be obtained from the ratios of the signal for the analyte to that of the internal standard (rhodium) as shown in Fig. 4. The percentage change in the ratio should ideally be close to zero if perfect compensation for the interference effect was achieved. As can be seen from Fig. 4 this is generally true within a small error for solutions containing up to 1% m/v methacrylic acid.However at higher acid strengths it is evident that there is substantial bias still present with both positive and negative changes being recorded most noticeably for analytes at either end of the mass range. These results indicate that in addition to general interfer- ence with all analyte signals there is also a mass bias effect. It is worth noting that for some elements the effect is worse in the presence of 5Oh m/v methacrylic acid than for 10% m/v acid solution. It is possible that this observation is an artefact of the internal-standard approach inasmuch as the analyte intensity varies differently in the presence of the matrix. 593 0 50 100 150 200 250 mlz Fig. 4 Percentage change in ana1yte:rhodium intensity ratio as a function of mawcharge ratio and the methacrylic acid concentra- tion 0 O ; D 1; @ 2; 0 5; and A 10%.Optimum conditions for aqueous solution measurement were employed as given in Table 1 0.12 ' 0.5 1-1 0 " ' " ' 1.4 1 0- 1.6 1-1 1.4 c I 0.6 0.4 0.2 O L ' ' ' ' ' 1.5 I 1 1 .o r rr 0.5 -1 0.4 2 0.3 L? 0.2 0.1 0.8 r 0.6 rr 2 0.4 0.2 0 2 4 6 8 1 0 0 2 4 6 8 1 0 Methacrylic acid concentration (YO) Fig. 5 Ratio of analyte to internal standard (Rh) intensity for individual elements as a function of the methacrylic acid concen- tration 0 25; D 50; a 75; and 0 100% Ratios for eight elements are shown individually for a range of analyte and methacrylic acid concentrations in Fig. 5. Each line in Fig. 5 represents a different analyte594 JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY DECEMBER 199 1 VOL.6 concentration. The ratio should be constant in the absence of interference and this would give a series of horizontal lines in the plots. It is clear that this is closest to being achieved in the mid-mass range (copper to indium). There is a definite progression in the series with the maximum interference being observed for 10% m/v methacrylic acid concentration at the low mass end (e.g. beryllium and scandium) and for 5% m/v acid concentration for high analyte masses (e.g. lead and uranium). Calibration graphs for six elements expressed as intensity ratio versus concentration are presented in Fig. 6. Signi- ficant deviations from linearity were observed for different acid matrix concentration levels.For beryllium the calibra- tion graph in 5% m/v acid was linear but of lower slope than that of the calibration graph for aqueous solution indicating a depression in the analyte signal. However the calibration graph for the solutions containing 1 Ooh m/v acid shows an enhanced slope with noticeable upward curva- ture. A similar situation was observed for the calibration graphs for scandium although this situation was compli- cated by the interference of C02H+ arising from the matrix. Scandium would therefore be unsuitable as an internal reference element in this type of application. For copper and indium the calibration graphs were relatively linear with enhanced slopes relative to aqueous solution responses. The magnitude of the enhancement was rather less than for the other elements but increased with increasing acid concentration.However for heavier elements such as lead and ura- nium the largest enhancement was observed for the solution containing 5% m/v methacrylic acid. The intensity ratio values in 10% m/v acid were also enhanced but the 0.12 l---l 0.10 0.08 0.06 - - - 0 20 40 60 80 100 Be concentration (ppb) 0.5 1-1 0 20 40 60 80 100 Cu concentration (ppb) 0.5 1 I Pb concentration (ppb) Sc concentration (ppb) la4 - 1.2 1 .o 0.8 0.6 0.4 0.2 0 20 40 60 80 100 In concentration (ppb) lmO l---l 0.8 - 0.6 - 0 20 40 60 80 100 U concentration (ppb) Fig. 6 Calibration graphs for individual elements for various methacrylic acid concentration levels 0 0; 0 2; my 5; and 0 1 0% graphs showed significant curvature.The effects are clearly related to the difference in the influence of the matrix on the ion intensities of the internal standard and the analyte element. The matrix effect appears to be less for elements that have masses close to that of the internal standard indicating a mass bias interference. Precision The precision of the measurement is also affected by the presence of the methacrylic acid matrix. The analyte relative standard deviations obtained for ten measurements were plotted as a function of mass and are presented in Fig. 7. Good precision is achieved for solutions containing up to 2Oh m/v methacrylic acid but for the higher acid concentra- tions the performance is unacceptable ranging from 5 to 27% relative. The deterioration in precision is related in part to the loss in sensitivity caused by the interferent.This is most obvious for the light mass elements which exhibit lowest sensitivity and poorest precision. Hence while it is possible to use matrix-matched standards for calibration purposes in the analysis of samples containing relatively high concentrations of acid this approach results in operation under conditions of poor precision and inade- quate sensitivity if the normal parameters for aqueous solution measurement are used. Optimization of ICP Parameters The introduction of samples with a significant level (> 1%) of matrix concomitants can alter the temperature character- istics of the ICP discharge. Significant losses in analyte signal intensity can arise because of a resulting perturbation in the population of atom-ion excited states.Alternatively differences in the physical properties of samples can give rise to changes in transport efficiency leading to a variation in the amount of analyte reaching the ICP and hence the MS detector. It was considered important therefore to determine the influence of the ICP parameters on the analyte signals obtained from solutions containing metha- crylic acid. The ICP parameters that have the most 30 I t \ I I I I t 0 50 100 150 200 . mlz io Fig. 7 Analyte precision as a function of the mass:charge ratio and the methacrylic acid concentration 0 O ; e 1 ; . 2; 0,5; and A 1 Ooh. Optimum conditions for aqueous solution measurement were employed as given in Table 1. Analyte concentrations were all 50 ng ml-lJOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY DECEMBER 199 1 VOL.6 595 6.0 5.5 5.0 4.5 4.0 3.5 3.0 2.5 2.0 - 0 -I (a) I I I I I I I 0.8 0.85 0.9 0.95 1.0 1.05 1.1 1.15 1.2 Nebulizer gas flow/l min-’ 5 - 4 - 0.7 0.9 1.1 1.3 R.f. powerIkW - A - = - 4 Auxiliary gas flow/l min-’ 1 t I 1.1 1.3 1.5 R.f. powerIkW Fig. 8 Effect of the various plasma operating conditions on the analyte intensity in the presence of 5% m/v methacrylic acid (a) nebulizer gas flow; (b) auxiliary gas flow; (c) r.f. power; and (d) as in (c) but for aqueous standard solution. Analyte concentrations were all 50 ng ml-I. Elements 0 Rh; 0 La; m In 0 U; + Sr; 0 Pb; A Sc; and A Cu significant influence on analytical performance are gener- ally considered to be the applied radiofrequency power the nebulizer gas flow rate and the auxiliary (or intermediate) gas flow rate.These parameters were optimized for a solution containing 50 ng ml-l of eight analyte elements in 5% m/v methacrylic acid. The results are shown in Fig. 8. The optimum conditions established for nebulizer and auxiliary gas flow rates were similar to those obtained for aqueous solutions. Nevertheless it was found that conditions could be achieved under which the analyte intensity in the presence of methacrylic acid was substantially increased. This was mainly owing to the optimization of the applied radiofre- quency power. It was established that in order to achieve the optimum intensity the ICP power setting had to be increased to a value of 1.35 kW. However as can be seen from Fig. 8 the optimum value for aqueous standard solutions was about 0.9 kW.It is evident from a comparison of graphs shown for aqueous and methacrylic acid media that to operate under either of these conditions would give rise to an apparent signal depression relative to the other. Hence in order to achieve the objective of analysing methacrylic acid samples using aqueous calibration stan- dards it would be necessary to adopt a compromise power setting at the point on the curve where the response is changing most rapidly. Optimization of Ion Optics Mass bias effects in the interface region of the instrument result in an alteration of the trajectory of analyte ions through the quadrupole mass filter and this is particularly severe for light elements which can be more easily deflected by concomitant species.It may be possible to correct for this type of interference by optimization of the mass spectrometer ion optics voltage settings to take account of the influence of the matrix. This was carried out by optimizing the ion optics for the direct analysis of solutions containing 5% m/v methacrylic acid using the ICP para- meters established previously. The voltages that could be adjusted on the Sciex Elan 250 instrument were those of the Einzel lens (EJ the plate lens (Ep) the photon stop (E,) and the barrel lens (E,,) as shown in Fig. 1. The settings were adjusted on the instrument by selecting a percentage of the voltage range available and these values were in turn related to actual voltages. The E2 lens is set by the manufacturer for maximum sensitivity and it was not altered in this work.The intensity of the ion response for 50 ng ml-’ of eight analytes was studied with respect to ion lens voltage settings. The optimum ion lens voltages used for aqueous solution work were used as a starting point and a univariate optimization of each of the four lens settings was then carried out in the order einzel plate photon stop and barrel lenses while aspirating the 5Oh m/v methacrylic596 JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY DECEMBER 1991 VOL. 6 4.5 1 -19 -17 -15 -13 -11 -9 -7 El IV 0 1 6.0 r ( C) 5.5 - 5.0 - 4.5 - 4.0 - 3.5 - 3.0 - -14 -12 -10 -8 -6 -4 -2 0 Es /v 2.5 ' 1 I 1 I -20 -15 -10 -5 0 EPN V.V 5.5 5.0 4.5 4.0 3*51 3.0 2.5 ' I 1 I 1 2 3 4 5 6 Eb N Fig. 9 Analyte intensity as a function of the ion optics settings. Solutions contained 50 ng m1-I of each analyte in the presence of 5Oh m/v methacrylic acid.See Fig. 1 for details of the ion lens configuration. (a) Einzel lens; (b) plate lens; (c) photon stop; and (d) barrel lens. Elements 0 Rh; 0 La; M In; 0 U; + Sr; 0 P b A Sc; A Cu; and * Be acid solution. The results are presented in Fig. 9. The same experiment was carried out by using aqueous standard solutions but in this instance under ICP conditions established for aqueous work and the data are presented for comparison in Fig. 10. It was found that the Einzel lens had relatively little effect on the analyte intensities observed in terms of absolute signal level. The plate lens setting was found to have a much stronger influence on analyte intensities but signals were relatively constant for all the elements in a narrow voltage range.There appeared to be a shift in the position of the curves to less negative values for the methacrylic acid matrix. However the ion response trend with respect to mass appeared to be similar in both aqueous and methacrylic acid media inasmuch as the sensitivity optima shifted towards less negative voltage values as the mass of the element increased. The photon stop lens setting had a clear optimum in terms of analyte ion intensities for the majority of elements in both matrices. However low and high mass elements showed significantly different intensity profiles with respect to photon stop lens voltage setting. For methacIylic acid solution beryllium exhibited an optimum response at - 5 V while lead and uranium afforded maximum sensitivity at approximately - 10 V indicating a strong mass dependence.This pattern was repeated in the example of the barrel lens where most elements exhibited an acceptable level of response at about + 3 V whereas the maxima for beryllium and uranium were found at + 1.5 and + 6 V respectively. There may have been some contribution to a shift in optimum ion optics voltage settings in going from an aqueous to a methacrylic acid matrix as a result of the fact that the optimum ICP power setting was significantly different in each instance since this may have had an influence on ion energy distribution. However in general the shape of the ion optics response graphs and the mass dependent trends observed for the methacrylic acid matrix were similar to those obtained for aqueous solution and to those reported previously for the Elan 250 in~trument.~?~ Overall the optimization of ion optics settings specifically for the methacrylic acid matrix while giving rise to some improvement did not result in large differences in sensitiv- ity in comparison with that achieved when using parameters optimized for measurements on aqueous solutions. It is concluded therefore that in the determination of trace elements in dilute methacrylic acid solutions the selection of ICP source operating conditions has a much greater influence on the magnitude of interference effects from the matrix.However the fact that different behaviour is observed for elements of different mass could indicate that the use of only one internal standard is insufficient for general purpose multi-element analysis.Analyte intensities were re-measured as a function of methacrylic acid concentration under the optimum condi- tions established above for 5% m/v acid solutions. The results are presented in Fig. 1 1. It is evident that sensitivity has been substantially improved for all elements in 5% m/v acid in comparison with measurements made under the optimum conditions for aqueous measurement. However it is also clear that a reduction in analyte sensitivity occurs for more dilute solutions in the equivalent comparison under these conditions. Nevertheless the advantage ofJOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY DECEMBER 199 1 VOL. 6 5.5 5.0 4.5 4.0 597 - - - - 6.0 (a) 4.0 3.5 3.0 5.5 t 1 I - - - 2.5 -20 -18 -16 -14 -12 -10 -8 ? El fv J 2 - 't 0 -16 -14 -12 -10 -8 -6 -4 -2 I I E N 6.0 I 3.51 // x 0 y I 2.5 -20 -15 -10 -5 0 EP N 5.5 - 5.0 - 4.5 - 4.0 - 3.5 - 3.0 t '* '* \ L.D 0 1 2 3 4 5 6 Eb N Fig.10 Analyte intensity as a function of the ion optics settings. Solutions contained 50 ng ml-' of each analyte in aqueous standard solution. See Fig. 1 for details of the ion lens configuration. (a) Einzel lens; (6) plate lens; (c) photon stop; and (d) barrel lens. Elements @ Rh; 0 La m In; 0 U; e Sr; 0 Pb; A Sc; A Cu; and * Be optimizing the system is that higher sensitivity and hence better signal-to-noise ratio can be obtained at a given matrix dilution level. 6.0 I 5.5 - - 0 ) 3 5.0 - 4.5 - 4.0 - 3.5 ' I 1 I 0 1 2 5 10 Methacrylic acid concentration (%) Fig.11 Analyte intensity as a function of the methacrylic acid concentration. Conditions optimized for 50 ng ml-l of each analyte in 5% d v methacrylic acid. Elements @ Rh; 0 La; m In; 0 U; e Sr; 0 Pb; A Sc; and A Cu Use of Alternative Elements as Internal Standards A brief study was conducted to determine if the use of elements other than rhodium as the internal standard would better compensate for changes in analyte signal sensitivity arising from the effect of the methacrylic acid matrix. Cobalt was used as internal standard for elements in the low mass region (beryllium scandium and copper) rhodium for mid-mass range elements (strontium indium and lanthanum) and bismuth for the high mass region (lead and uranium). The ratio of the analyte ion intensity to that of the internal standard was measured as a function of ICP incident power setting in the range 950-1200 W.It was thought that a compromise power setting in this range might yield similar analyte sensitivities in both aqueous and methacrylic acid media thereby allowing the use of aqueous calibration standards. The results are presented in Fig. 12. The use of cobalt as an internal standard for the determination of beryllium proved effective as the inten- sity ratios obtained in the methacrylic acid medium closely followed that for the aqueous standard solution [see Fig. 12 (a)]. For the determination of copper while the ratio values were not identical indicating an enhanced response in the methacrylic acid medium the two curves showed the same general trend with respect to power setting.The difference between the two graphs was at a minimum at 1100 W. However for scandium the results obtained in the presence of 5% ( d v ) methacrylic acid were influenced by power setting to a much greater extent than those for the aqueous solution. This is attributable to spectral interference on the598 JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY DECEMBER 199 1 VOL. 6 0.8 0 0.6 0 0 0 c .- U 0.4 4- .- cn al 4- - 0.2 0 * c 950 1000 1050 1100 1150 1200 Incident power/kW 0.6 0.5 iz 0 c 0 .- c 0.4 r cn al c .- U - 0.3 0.7 - r 0 0.6 - .- t a -. 2 4 0.5 - C al c - 0.4 - 0.31 ' I I I 1 I 950 1000 1050 1100 1150 1200 Incident power/kW I - I I 1 950 1000 1050 1100 1150 1200 0.2' ' Incident power/kW Fig.12 Intensity ratios as a function of power for aqueous standard solutions (as) and in the presence of 5% m/v methacrylic acid. Standard solutions used in (a) 0 5% Be; 0 aq Be; M 5% Sc; 0 aq Sc; e 5% Cu; and 0 aq Cu with Co as the internal standard. Standard solutions used in (b) 0 5% Sr; 0 aq Sr; . 5% In; 0 aq In; e 5% La; and 0 aq LA with Rh as the internal standard. Standard solutions used in (c) 0 5% Pb; 0 aq Pb; M 5% U; and 0 aq U with Bi as the internal standard Table 2 Difference in slope of calibration graphs obtained for aqueous standard solutions and those containing 5% m/v methacrylic acid Internal Change Analyte Isotope 1st IP*/ 2nd IP/ standard in slope (%) element mass eV eV element Be sc c u Sr In La Pb U 9 45 63 88 115 139 208 238 9.32 6.54 7.72 5.69 5.79 5.6 1 7.4 1 6.08 18.2 12.8 20.3 11.0 18.9 18.8 11.4 12.57 c o c o c o Rh Rh Rh Bi Bi +11.0 + 1.1 + 17.0 - 6.4 + 5.6 -0.7 -15.8 - 18.4 Internal standard- 59 7.86 17.0 - - co Rh 103 7.46 18.1 - Bi 209 7.29 16.7 - - *IP = ion potential.+Suggested value. scandium mass due to breakdown products of the metha- Fig. 12(b). For strontium the ratioed responses were crylic acid (e.g. CO,H+). Again with use of a power setting similar for aqueous and methacrylic acid solutions only at of about 1 100 W the ratios were closest for aqueous and the higher power settings and were closest at 1100 W. For methacrylic acid matrices. indium the intensity ratio to rhodium in methacrylic acid Similar data for elements in the mid-mass range ob- solution was also very substantially different from the tained with rhodium as internal standard are presented in aqueous response at low power but the two graphsJOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY DECEMBER 199 1 VOL.6 599 3.0 (a) 3.0 ( b ) 1 Analyte concentration/ng ml-' Ana I yte concent rat ion/ng m I-' Analyte concentration/ng ml-' Fig. 13 Calibration graphs obtained at a compromise power setting of 1 150 W for aqueous standard solutions (as) and in the presence of 5% m/v methacrylic acid. Standard solutions used in (a) 0 5W Be; 0 aq Be; D 5% Sc; 0 aq Sc; + 5% Cu; and 0 aq Cu with Co as the internal standard. Standard solutions used in (b) a 5% Sr; 0 aq Sr; D 5% In; 0 aq In; + 5% La; and 0 aq La with Rh as the internal standard. Standard solutions used in (c) 0 5% Pb; 0 aq Pb; D 5% U; and 0 aq U with Bi as the internal standard.The percentage difference in the slopes of the calibration graphs for aqueous and methacrylic acid solutions is given in Table 2 converged at higher power settings at about 1 150-1 200 W. The graph for lanthanum in 5% m/v methacrylic acid solution also showed significant fluctuation at low power unlike that for the aqueous standard but this deviation was minimized at about 1100 W. The intensity ratios obtained for lead and uranium with use of bismuth as the internal standard are shown in Fig. 12(c). The ratios for lead in the two matrices were largely unaffected by the ICP incident power setting and were parallel except for some convergence of the methacrylic acid response at low power. The intensity ratios for uranium were widely different at all power settings except at lOOOW where the responses for the aqueous and methacrylic acid solutions crossed.Calibration graphs were established for each of the analytes in both aqueous and 5% m/v methacrylic acid media by using the appropriate internal standard as indicated above. The results are presented in Fig. 13. A compromise power setting of 1150 W was used for the measurements. The change in the slope of the calibration graphs obtained for aqueous and methacrylic acid matrices was calculated. These data are presented in Table 2. While some of the calibration graphs (e.g. for lanthanum) are very similar for the two matrices others (e.g. those for copper and uranium) have differences in slopes of greater than 15% in the two media.There did not appear to be any correlation in the effectiveness of the internal standard based on either proximity of mass or in terms of ionization potential. Conclusions It is evident from the results obtained in the present study that analytical performance can be improved for measure- ments carried out in the presence of methacrylic acid by a systematic optimization of ICP-MS instrumental para- meters. Substantial improvements in sensitivity were demonstrated for the direct determination of all elements in methacrylic acid by using this approach. It would seem however that it is not generally practicable to employ an aqueous calibration strategy for multi-element analysis using compromise instrument conditions for determina- tions in 5% m/v methacrylic acid. It is possible that for single element operations optimization of instrumental parameters in conjunction with the use of an appropriate internal standard may provide satisfactory results. The method of matrix matching of samples and standards could be used in conjunction with the optimization approach but it has been found in practice that solvent contamination is a problem for the determination of some elements at low concentrations. Consequently the method of standard additions is preferred for this type of analysis. This work was made possible by the loan of the Sciex Elan600 JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY DECEMBER 199 1 VOL. 6 250 ICP-MS instrument from Perkin-Elmer (UK). The authors are grateful to P. Mitchell and P. Sumner of Perkin- Elmer who agreed to the provision of this equipment and to ICI for permission to submit this paper for publication. References 1 Van Heuzen A. A. in Applications of Inductively Coupled Plasma Mass Spectrometry eds. Date A. R. and Gray A. L. Blackie Glasgow UK 1989 ch. 7 p. 169. Hutton R. C. J. Anal. At. Spectrom. 1986 1 259. 2 3 4 5 6 7 Hausler D. Spectrochim. Acta Part B 1987 42 63. Longerich H. P. J. Anal. At. Spectrom. 1989 4 665. Evans E. H. and Ebdon L. J. Anal. At. Spectrom. 1990 5 425. Schmit J.-P. and Chtaib M. Can. J. Spectrosc. 1987,32 56. Schmit J.-P. and Chauvette A. J. Anal. At. Spectrom. 1989 4 755. Paper 1 /02185K Received May 9th 1991 Accepted June 28th 1991

ISSN:0267-9477    

DOI:10.1039/JA9910600591

出版商:RSC    

年代:1991

数据来源: RSC