摘要:

Ramon M. Barnes Editor Department of Chemistry LGRC Towers University of Massachusetts Am herst MA 01 003-0035 Telephone (413) 545-2294 fax 545-4490 Objective 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- cal excitation source for atomic emission spectroscopy. ICP discharges also are applied commercially as an ion source for mass spectrometry and as an atom and ion cell in atomic fluo- rescence 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 INFOR- MATION NEWSLETTER in 1975. Other popular plasma sources i.e. microwave Induced plasmas direct current plasmas and glow discharges also are induded in the scope of the ICP IN- FORMATION NEWSLETTER. Scope As the only authoritative monthly journal of its type the ICP INFORMATlON NEWSLETTER is read in more than 40 coun- tries by saentists actively applying or planning to use the ICP or other types of plasma spectroscopy. For the novice in the field the K=P INFORMATlON NEWSLETTER provides a oonase 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 lNFORMATION NEWSLETTER. Reg u I ar Features *Original submitted and invited research articles by ICP and *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-Ian- guage ICP papers. *Critical reviews of plasma-related books and software. Conference Activities The ICP lNFORMATlON NEWSLETTER has sponsored seven international meetings on developments in atomic plasma spectrochernical analysis since 1980 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 11-IV (Pergamon Press) as well as in special issues of Spectrochimica Acta Part B and Journal of Analytical Atomic Spectrometry. The 1994 Winter Confer- ence on Plasma Spectrochemistry will be held in San Diego California January 10 - 15 1994; its proceedings will be published by Fall 1994.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 18 runsfrom June 1992 through May 1993. 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. plasma experts. national meetings. plasma progress. 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 IJ Volume(s)- (June 19- - May 19- ) or CI 19 (January - December). Enclosed 0 Prepayment 0 Check or money order OVISA 0 Mastercard Account No. (All 13 or 16 digits) ) or 0 Send invoice. Date Cardholder Name Expiration date Card holder Signature . Amount Due $ Mail to Name Organization Address City State/Country ZI P/Postalcode Telephone Telex/f ax Note For each credit-card transaction a 4 % 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 Russia). 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. ,13 Purchase order (No.CONFERENCE ANNOUNCEMENT 199 5 FIRST MEDITERRANEAN BASIN CONFERENCE ON ANALYTICAL CHEMISTRY Cordoba Spain 5-10 November 1995 In order to promote collaboration among analytical scientists of the whole Mediterranean Basin the 1995 First Mediterranean Basin Conference on Analytical Chemistry will provide an adequate forum for reporting and thoroughly discussing the latest research results in basic and instrumental developments in Analytical Chemistry.Other aims of this Conference are - To promote new opportunities for young scientists in the Mediterranean Sea area (particularly for those in the Southern Bank) to attend international meetings in countries of the region tot attend training workshops on new analytical techniques to attend short courses on new techniques and trends in Analytical Chemistry and to establish new links for research in/or other countries of the region. - To stimulate the progress of Analytical Chemistry as a whole by solving analytical problems affecting the Mediterranean Area. The program has been designed to attract participants from industry universities and research centers.The program will comprise invited plenary and key-note lecturers contributed oral papers and posters distributed in several Symposia covering the following topics Education of Analytical Chemistry Environmental Analytical Chemistry Agriculture and Food Analysis Geoanalytical Chemistry and Benefitiation of Minerals Biomedical Analysis Archeometry and Art Objects Preservation Quality Assurance and Harmonization of Procduies. A few Short Courses Special Sessions on "hot" topics and an E,xhibition of Instrumentation has also been arranged. Invited lecturers who have already confirmed their contribution include M. ValcArcel I.B. Brenner D. Barcelo S. Caroli A. Laachach. O.X.F. Donnard M. M. Khater H. Muntau J. Albaiges B.Y. Meklati P. Quevauviller etc.CALL FOR PAPERS Titles of submitted oral or poster presentations are solicited with the preliminary registration card by 30 May 1995. Submission of final Conference Abstracts are requested not later than 30 June 1995. SOCIAL ACTIVITIES Varied social activities including a visit to Granada are being planned. FURTHER INFOlRMATION For further information and pre-registration forms please contact Prof. Alfred0 Sanz-Medel (Chairman) Department of Physical and Analytical Chemistry Faculty of Chemistry University of Oviedo C / Jufian Claveria s/n 3 3006 Oviedo SPAIN Phone 3 4 - 8 - 5 1 0 3 4 8 0 o 3 4 - 8 - 5 1 0 3 4 7 4 FAX 3 4 - 8 - 5 10.31257996 Winter Conference on Plasma Spectrochemistry Fort Lauderdale Florida January 8 - 7 3 7996 Name Organization Address City The 1996 Winter Conference on Plasma Spectrochemistry ninth in a series of biennial meetings sponsored by the ICP lnformation Newsletter features developments in plasma spectrochemical analysis by inductively coupled plasma (ICP) dc plasma (DCP) microwave plasma (MIP) and glow discharge (GDL HCL) sources.The meeting will be held Monday January 8 through Saturday January 13 1996 at the Bonaventure World Conference Center in Fort Lauderdale Florida. Continuing education short courses at introductory and advanced levels will be offered Friday through Sunday January 5 - 7. Spectroscopic instrumentation and accessories will be shown during a three-day exhibition. Objectives and Program The continued growth in popularity of plasma sources for atomization and excitation in atomic spectroscopy and ionization in mass spectrometry and the need to discuss recent developments of these discharges in spectrochemical analysis stimulated the organization of this meeting.The Conference will bring together international scientists experienced in applications instrumentation and theory in an informal setting to examine recent progress in the field. Approximately 500 participants from 25 countries are expected to attend. Approximately 300 papers describing applications fundamentals and instrumental developments with plasma sources are expected to be presented in lecture and poster sessions by more than 200 authors. Symposia organized and chaired by recognized experts will include the following topics 1) Sample introduction and transport phenomena 2) Flow injection spectrochemical analysis 3) Elemental speciation with plasma/chromatographic techniques 4) Plasma instrumentation including chemometrics expert systems on-line analysis software and remote-system automation 5) Sample preparation treatment and automation 6) Excitation mechanisms and plasma phenomena 7) Spectroscopic standards and reference materials 8) Plasma source mass spectrometry 9) Glow discharge atomic and mass spectrometry 10) Applications of stable isotope analyses and 1 1 ) Laser-assisted plasma spectrometry.Six plenary and 18 invited lectures will highlight advances in these areas. Afternoon poster sessions will feature applications automation and new instrumentation. Five panel discussions will address critical development areas in sample introduction instrumentation elemental speciation plasma source mass spectrometry and novel software and hardware directions.Plenary invited and submitted papers will be published in Fall 1996 after peer review as the official Conference proceedings. Schedule of Activities Preliminary Title and 50-Word Abstract Due for Contributed Papers Exhibitor Booth Reservation and Pre-Registration Deadline Conference Pre-Registration October 13,1995 Hotel Pre-Reservation October 13 1995 Late Pre-Registration Deadline December 8,1995 1996 Winter Conference Short Courses January 5 - 7,1996 1 996 Winter Conference on Plasma Spectrochemistry January 8 - 13,1996 July 3 1995 September 11 1995 Further Information For further information return this form to 1996 Winter Conference on Plasma Spectrochemistry %/CP Information Newsletter Department of Chemistry Lederle GRC Towers University of Massachusetts Box 34510 Amherst MA 01003-4510 USA.ATTN Dr. Ramon Barnes Conference Chairman Telephone (41 3) 545-2294 Telefax (413) 545-4490. & 0 Send further information. 0 I plan to attend accompanied by 0 / plan to present a paper (0 oral 0 poster 0 computer poster). Title 7996 WINTER CONFERENCE ON PLASMA SPECTROCHEMISTRY ~ Title State/Country Telefax Date ZIP/Postal Code EMAlLAn essential time-saving PC literature search tool for the analytical chemist What JAASbase is ... JAASbase i s a unique database of atomic spectrometry reference information containing full bibliographic references to journal articles and conference papers in the field of atomic spectrometry published since 1985.These references are selected by expert atomic spectroscopists who add supplementary information that allows you to search for the references you require. The backfile (covering 1985 to 1994) contains over 28,000 references. Update disks add around another 4,000 references a year. JAASbase has been designed to work with the database manager Idealist a fully indexed free-text retrieval system. How will JAASbase help you? If you are an analytical scientist with a need for rapid access to information on techniques used in atomic spectrometry JAASbase i s the tool you need. Particularly if you work in an applications laboratory with a restricted budget for primary journals and little or no access to library facilities - JAASbase gives you instant access at your bench. Whether your area of analysis i s food the environment quality control geology metallurgy or whatever JAASbase will quickly become an essential part of your working life. JAASbase Backfile (1 986-94) JAASbase Updates 1995 Idealist Software f 280.00/$49O.00 f 99.00/$174.00 f 2 1 0.00/$368.00 Plus VAT in the UK Available in disk size 3.5" or 5.25" 1995 Subscription Price To order please contact The Royal Society of Chemistry Turpin Distribution Services Limited Blackhorse Road Letchworth Herts SG6 1 HN United Kingdom. Telephone +44 (0) 1462 672555. Fax +44 (0) 1462 480947. Turpin Distribution Services Limited is wholly owned by The Royal Socic!ty of Chemistry. RSC members' should order from The Royal Society of Chemistry Membership Administration Thomas Graham House Science Park Milton Road Cambridge CB4 4WF United Kingdom. Telephone +44 (0) 1223 420066. Fax +44 (0) 1223 423623. €-Mail (In'ternet) RSC1 BRSC.ORG. THE ROYAL SOCIETY OF C H EM I STRY Information Services

ISSN:0267-9477    

DOI:10.1039/JA99510BP012

出版商:RSC    

年代:1995

数据来源: RSC

摘要:

Journal of Analytical Atomic Spectrometry (Including Atomic Spectrometry Updates) JAAS Editorial Board Chairman B. L. Sharp (Loughborough U K ) A. T. Ellis (Abingdon U K ) J M. Gordon (Cambridge U K ) S. J. Haswell (Hull U K ) S. J. Hill (Plymouth U K ) R. C. Hutton (Winsford U K ) D. Littlejohn (Glasgow UK) J. Marshall (Middlesbrough U K ) A. Sanz-Medel (Oviedo Spain) JAAS Advisory Board F. C. Adams (Antwerp. Belgium) R. M. Barnes (Amherst MA USA) L. Bezur (Budapest Hungary) M. W. Blades (Vancouver Canada) R. F. Browner (Atlanta GA. USA) S. Caroli (Rome Italy) A. J. Curtius (Norianopolis Brazil) J. B. Dawson (Leeds U K ) M. T. C. de Loos-Vollebregt (Delft The L. Ebdon (Plymouth U K ) M. S. Epstein (Gaithersburg MD USA) Fang Zhao-lun (Shenyang. China) W. Frech (UmeA Sweden) A.L. Gray (Egham U K ) S. Greenfield (Loughborough UK) G. M. Hieftje (Bloornington IN USA) B. V. L'vov (St. Petsrsburg Russia) R. K. Marcus (Clemson SC USA) J. M. Mermet (Villeurbanne France) T. Nakahara (Osaka Japan) Ni Zhe-ming (Beijing China) N. Omenetto (lspra Italy) C. J. Park (Taejon Korea) R. E. Sturgeon (Ottawa Canada) V. Sychra (Prague Czech Republic) R. Van Grieken (Antwerp Belgium) A. Walsh ,,K. B. (Victoria Australia) B. Welz (Uberlingen Germany) Netherlands) Atomic Spectrometry Updates Editorial Board Chairman *A. T. Ellis (Abingdon UK) J. Armstrong (Edinburgh UK) *J. R. Bacon (Aberdeen U K ) C. Barnard (Glasgow U K ) R. M. Barnes (Amherst MA USA) S. Branch (High Wycombe UK) R. Bye (Oslo Norway) J. Carroll (Middlesbrough UK) M. R. Cave (Keyworth UK) S.Chenery (Keyworth UK) *J. M. Cook (Keyworth U K ) *M. S. Cresser (Aberdeen UK) H. M. Crews (Norwich U K ) J. S. Crighton (Sunbury-on-Thames U K ) *J. 8. Dawson (Leeds UK) J. R . Dean (Newcastle upon Tyne U K ) *E. H. Evans (Plymouth UK) J. Fazakas (Budapest Hungary) A. Fisher (Plymouth U K ) *J. M. Gordon (Cambridge U K ) D. J. Halls (Glasgow U K ) *S. J. Hill (Plymouth UK) K. W. Jackson (Albany NY USA) R. Jowitt (Middlesbrough U K ) K. Kitagawa (Nagoya Japan) J. Kubova (Bratislava Slovak Republic) *J. Marshall (Middlesbrough UK) H. Matusiewicz (Poznan Poland) A. W. McMahon (Manchester UK) J. M. Mermet (Villeurbanne France) R. G. Michel (Storrs CT USA) *D. L. Miles (Keyworth UK) T. Nakahara (Osaka Japan) Ni Zhe-ming (Beving Chiria) P. R. Poole (Hamilton New Zealand) P.J. Potts (Milton Keynes UK) W. J. Price (Budleigh Salterton UK) C. J. Rademeyer (Pretoria South Africa) *M. H. Ramsey (London U K ) P. G. Riby (Greenwich UK) A. Sanz-Medel (Oviedo Spain) *B. L. Sharp (Loughborough U K ) I. L. Shuttler (Uberlingen Germany) S. T. Sparkes (Plymouth LIK) R. Stephens (Halifax Canada) J. Stupar (Ljubljana Slovenia) R. E. Sturgeon (Ottawa Canada) *A. Taylor (Guildford UK) G. C. Turk (Gaithersburg MD USA) J. F. Tyson (Amherst MA USA) P. Watkins (London UK) B. Welz (Uberlingen Germny) J. Williams (Egharn UK) J. B. Willis (Victoria Australia) *Members of the ASU Executive Committee Editor JAAS Janice M. Gordon The Royal Society of Chemistry Thomas Graham House Science Park Milton Road Cambridge CB4 4WF UK. Telephone + 44 (0) 1223 420066.Fax +44 (0) 1223 420247. E-mail RSCl @RSC.ORG (Internet) Senior Assistant Editor Brenda Holliday Editorial Secretary Lesley Turney US Associate Editor JAAS Dr. J. M. Harnly US Department of Agriculture Beltsville Human Nutrition Research Center Beltsville MD 20705 USA. Telephone 301 -504-8569 Assistant Editor Ziva Whitelock Advertisements Advertisement Department The Royal Society of Chemistry Burlington House Piccadilly London W1V OBN UK. Telephone +44 (0) 171 -287 3091. Fax + 44 (0) 171 -494 11 34. Information for Authors Full details of how to submit materials for publi- cation 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 publi- cation of original research papers communi- cations and letters concerned with the development and analytical application of atomic spectrometric techniques. The journal is pub- lished twelve times a year including comprehen- sive reviews of specific topics of interest to practising atomic spectroscopists and incorpor- ates the literature reviews which were previously published in Annual Reports on Analytical Atomic Spectroscopy (ARAAS).Manuscripts intended for publication must describe original work related to atomic spectro- metric analysis. Papers on all aspects of the sub- ject will be accepted including fundamental studies novel instrument developments and prac- tical analytical applications. As well as AAS AES and AFS papers will be welcomed on atomic mass spectrometry X-ray fluorescence/emission spectrometry and secondary emission spec- trometry.Papers describing the measurement of molecular species where these relate to the characterization of sources normally used for the production of atoms or are concerned for example with indirect methods of analysis will also be acceptable for publication. Papers describing the development and applications of hybrid techniques (e.g. GC-coupled AAS and HPLC-ICP) will be particularly welcome. Manuscripts on other subjects of direct interest to atomic spectroscopists including sample prep- aration and dissolution and analyte pre-concen- tration procedures as well as the statistical interpretation and use of atomic spectrometric data will also be acceptable for publication.There is no page charge. The following types of papers will be considered. Full papers describing original work. Communications which must be on an urgent matter and be of obvious scientific importance. Communications receive priority and are usually published within 2-3 months of 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 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 manuscript will be regarded as an undertaking that the same material is not being considered for publication by another journal. Manuscripts (three copies typed in double spacing) should be sent to Janice M. Gordon 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 regarding 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 monthly by 1 . .J 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 Distribution Services Ltd. Blackhorse Road Letchworth Herts. SG6 1 HN UK Tel. +44 (0) 1462 672555; Telex 825372 Turpin G; Fax +44 (0) 1462 480947. Turpin Distribution Services Ltd. is wholly owned by The Royal Society of Chemistry. 1995 Annual subscription rate EEA f512.00 USA $941 50 Canada f538.00 ( + GST) Rest of World f538.00. 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 Spectrometry (JAAS) Publications Expediting Inc. 200 Meacham Avenue Elmont NY 11003. 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. @The Royal Society of Chemistry 1995. All rights reserved. No part of this publication may be reproduced stored in a retrieval system or transmitted in any form or by any means electronic mechanical photographic recording or otherwise without the prior permission of the publishers.Journal of Analytical Atomic Spectrometry (Including Atomic Spectrometry Updates) JAAS Editorial Board Chairman B.L. Sharp (Loughborough UK) A. T. Ellis (Abingdon UK) J. M. Gordon (Cambridge UK) S. J. Haswell (Hull UK) S. J. Hill (Plymouth UK) R. C. Hutton (Winsford UK) D. Littlejohn (Glasgow UK) J. Marshall (Middlesbrough UK) A. Sanz-Medel (Oviedo Spain) P. D. P. Taylor (Geel Belgium) JAAS Advisory Board F. C. Adams (Antwerp Belgium) R. M. Barnes (Amherst MA USA) L. Bezur (Budapest Hungary) M. W. Blades (Vancouver Canada) R. F. Browner (Atlanta GA USA) J. L. Burguera (Merida Venezuela) S. Caroli (Rome Italy) J. A. Caruso (Cincinnati OH USA) H. M. Crews (Norwich UK) A. J. Curtius (Florianopolis Brazil) J. B. Dawson (Leeds UK) 0. F. X. Donard (Talence France) M. T. C. de Loos-Vollebregt (Delft The Netherlands) L. Ebdon (Plymouth UK) M.S. Epstein (Gaithersburg MD USA) Fang Zhao-lun (Shenyang China) W. Frech (Umes Sweden) A. K. Gilrnutdinov (Uberlingen Germany) G. M. Hieftje (Bloomington IN USA) R. S. Houk (Ames OH USA) R. Klockenkihmper (Dortmund Germany) B. V. L'vov (St. Petersburg Russia) R. K. Marcus (Clemson SC USA) J. M. Mermet (Villeurbanne France) T. Nakahara (Osaka Japan) Ni Zhe-ming (Beving China) J. W. Olesik (Columbus OH USA) N. Omenetto (lspra Italy) C. J. Park (Taejon Korea) P. J. Potts (Milton Keynes UK) R. E. Sturgeon (Ottawa Canada) V. Sychra (Prague Czech Republic) R. Van Grieken (Antwerp Belgium) P. Van Espen (Antwerp Belgium) B. Welz (Uberlingen Germany) Atomic Spectrometry Updates Editorial Board Chairman *A. T. Ellis (Abingdon UK) J. Armstrong (Edinburgh 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) S. Chenery (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. B. Dawson (Leeds UK) J. R. Dean (Newcastle upon Tyne UK) *E. H. Evans (Plymouth UK) J. Fazakas (Budapest Hungary) A. Fisher (Plymouth UK) *J. M. Gordon (Cambridge UK) D. J. Halls (Glasgow UK) *S. J. Hill (Plymouth UK) K. W. Jackson (Albany NY USA) R. Jowit t (Middlesbrough UK ) K. Kitagawa (Nagoya Japan) J. Kubova (Bratislava Slovak Republic) *J. Marshall (Middlesbrough UK) H. Matusiewicz (Poznan Poland) A. W. McMahon (Manchester UK) J. M. Mermet (Villeurbanne France) R.G. Michel (Storrs CT USA) *D. L. Miles (Keyworth UK) T. Nakahara (Osaka Japan) Ni Zhe-ming (Beijing China) P. J. Potts (Milton Keynes UK) W. J. Price (Budleigh Salterton UK) C. J. Rademeyer (Pretoria South Africa) A. Sanz-Medel (Oviedo Spain) *B. L. Sharp (Loughborough UK) I. L. Shuttler (Uberlingen Germany) S. T. Sparkes (Taunton UK) R. Stephens (Halifax Canada) J. Stupar (Ljubljana Slovenia) R. E. Sturgeon (Ottawa Canada) *A. Taylor (Guildford UK) G. C. Turk (Gaithersburg MD USA) J. F. Tyson (Amherst MA USA) P. Watkins (London UK) B. Welz (Uberlingen Germany) J. Williams (Egham UK) J. B. Willis (Victoria Australia) *Members of the ASU Executive Committee Editor JAAS Janice M. Gordon The Royal Society of Chemistry Thomas Graham House Science Park Milton Road Cambridge CB4 4WF UK.Telephone + 44 (0) 1223 420066. Fax + 44 (0) 1223 420247. E-mail RSC1 @RSC.ORG (Internet) Senior Assistant Editor Brenda Holliday Assistant Editor Ziva Whitelock Editorial Secretary Lesley Turney US Associate Editor JAAS Dr. J. M. Harnly US Department of Agriculture Beltsville Human Nutrition Research Center Beltsville MD 20705 USA. Telephone + 1 301 -504-8569 Asia-Pacific Associate Editor JAAS Prof. N. Furuta Department of Applied Chemistry Faculty of Science and Engineering Chuo University 1-1 3-27 Kasuga Bunkyo-ku Tokyo 11 2 Japan. Telephone 81 -3-381 7-1 906. E-mail nfuruta@apchem.chem.chuo.u.ac.jp F ~ x 81 -3-381 7-1 895. Advertisements Advertisement Department The Royal Society of Chemistry Burlington House Piccadilly London W1 V OBN UK.Telephone + 44 (0) 171 -287 3091. Fax + 44 (0) 171 -494 11 34. Information for Authors Full details of how to submit materials for publi- cation 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 publi- cation of original research papers communi- cations and letters concerned with the development and analytical application of atomic spectrometric techniques. The journal is pub- lished twelve times a year including comprehen- sive reviews of specific topics of interest to practising atomic spectroscopists and incorpor- ates the literature reviews which were previously published in Annual Reports on Analytical Atomic Spectroscopy (ARAAS).Manuscripts intended for publication must describe original work related to atomic spectro- metric analysis. Papers on all aspects of the sub- ject will be accepted including fundamental studies novel instrument developments and prac- tical analytical applications. As well as AAS AES and AFS papers will be welcomed on atomic mass spectrometry X-ray fluorescence/emission spectrometry and secondary emission spec- trometry. Papers describing the measurement of molecular species where these relate to the characterization of sources normally used for the production of atoms or are concerned for example with indirect methods of analysis will also be acceptable for publication. Papers describing the development and applications of hybrid techniques (e.g.GC-coupled AAS and HPLC-ICP) will be particularly welcome. Manuscripts on other subjects of direct interest to atomic spectroscopists including sample prep- aration and dissolution and analyte pre-concen- tration procedures as well as the statistical interpretation and use of atomic spectrometric data will also be acceptable for publication. There is no page charge. The following types of papers will be considered. Full papers describing original work. Communications which must be on an urgent matter and be of obvious scientific importance. Communications receive priority and are usually published within 2-3 months of 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 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 manuscript will be regarded as an undertaking that the same material is not being considered for publication by another journal. Manuscripts (three copies typed in double spacing) should be sent to Janice M. Gordon 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 regarding 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 monthly 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 Distribution Services Ltd. Blackhorse Road Letchworth Herts. SG6 lHN UK Tel. +44 (0) 1462 672555; Telex 825372 Turpin G; Fax +44 (0) 1462 480947. Turpin Distribution Services Ltd. is wholly owned by The Royal Society of Chemistry. 1995 Annual subscription rate EEA f512.00 USA $941.50 Canada f538.00 (+ GST) Rest of World f538.00. 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 1 1 003. USA Postmaster send address changes to Journal of Analytical Atomic Spectrometry (JAAS) Publications Expediting Inc. 200 Meacham Avenue Elmont NY 1 1 003. 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. @The Royal Society of Chemistry 1995. All rights reserved. No part of this publication may be reproduced stored in a retrieval system or transmitted in any form or by any means electronic mechanical photographic recording or otherwise without the prior permission of the publishers.

ISSN:0267-9477    

DOI:10.1039/JA99510FX029

出版商:RSC    

年代:1995

数据来源: RSC

摘要:

Journal of Analytical Atomic SDect romet r y I ' -. . ' 1111 UI lUlUlll111111 lUllllllllll 1.1 I. 1.1.1111111.11 ,....,.... .I. 1 llllllll I Ill llIlll'llllillllllllll JASPEP 1 O(7) 43N-46N 473-51 8 173R-198R (1 995) CONTENTS NEWS PAGES Book Review John Marshall 43N Diary of Conferences and Courses 43N Future Issues 45N PAPERS Third Rio Symposium on Atomic Spectrometry Caracas Venezuela November Liquid Sample Introduction Devices in Flow Injection Atomic Spectroscopy J. L. Burguera M. Burguera On-line Ion Exchange for the Removal of Sulfur Anion Interference on the Determination of Manganese in Geothermal Fluids by Flow Injection Electrothermal Atomic Absorption Spectrometry J. L. Burguera M. Burguera C. Rivas P. Carrero M. Gallignani M. R. Brunetto Fluoride as a Chemical Modifier for the Determination of Phosphorus by Electrothermal Atomic Absorption Spectrometry Jose Alvarado Ana Rita Cristiano Adilson Jose Curtius Determination of Mineral and Trace Elements in Total Diet by Inductively Coupled Plasma Atomic Emission Spectrometry Comparison of Microwave- based Digestion and Pressurized Ashing Systems Using Different Acid Mixtures Virginia E.Negretti de Briitter Peter Bratter Albrecht Reinicke Gerhard Schulze Walter Oliver L. Alvarez Nestor Alvarez 6-1 2 1994 473 479 483 487 Atomization Efficiencies of Bismuth Lead Manganese Chromium and Gallium Under Stabinzed Temperature Platform Furnace Conditions Yang Wei-rnin Ni Zhe-ming Flow-through Microwave Digestion System for the Determination of Aluminium in Shellfish by Electrothermal Atomic Absorption Spectrometry Marco A.Z. Arruda Mercedes Gallego Miguel Valclrcel Arsenic Determination in Environmental Biological and Food Samples by Inductively Coupled Plasma Mass Spectrometry Alexandra Usztity Antoaneta Krushevska Mihaly Kotrebai Ramon M. Barnes Dulasiri Amarasiriwardena Improvement in the Ion Exchange Chromatographic Separation of Rare Earth Elements in Geological Materials for Their Determination by Inductively Coupled Plasma Atomic Emission Spectrometry Juan C. Faritias Horacio P. Cabrera Maria T. Larrea CUMULATIVE AUTHOR INDEX 493 501 505 51 I 51 7 ~ ~ ATOMIC SPECTROMETRY UPDATES References 173R Typeset printed and bound by The Charlesworth Group Huddersfield England 01 484 51 70776th Surrey Conference on Plasma Source Spectrometry St.Helier Jersey UK 17-20 September 1995 Invited Lecturers Dr N Walsh (Royal Holloway) Dr C Gregoire (Geological Survey Canada) Professor R Barnes (University of Massachusetts) and Dr A Gray (Imperial College) Call for Papers Papers (oral and poster presentations) on topics associated with all aspects of plasma source mass spectrometry and on ICP-AES and ICP-MS studies in the Earth Sciences. Three copies of abstracts must be submitted before July 28 1995 Social Programme A n informal reception will take place on the Sunday and a conference dinner on Wednesday evening. A n accompanying persons’ package is available. Registration The residential package covers all meals coffee tea accommodation in single rooms and registration fee. A reduced fee is available for all bona f i d e students Further Details Dr Kym Jarvis NERC ICP-MS Facility CARE Silwood Park Ascot Berks UK SL5 7TE. Tel +44 (0)1344 294517/6; Fax +44 (0)1344 873997

ISSN:0267-9477    

DOI:10.1039/JA99510BX031

出版商:RSC    

年代:1995

数据来源: RSC

摘要:

DIARY OF CONFERENCES AND COURSES 1995 Dr William E. Jones. Telephone (519) 253 4232 ext 2001; Fax (519) 973 7098. Details can be found in J. Anal. At. Spectrom. 1995 10 18N. For further details contact Prof. Hasuck 41st International Conference on Analytical Sciences and Spectroscopy August 14-1 6 Kim (Secretariat) ASIANALYIS 111 Denartment of Chemistrv. College of The Third Asian Conference on Windsor Ontario Canada Analytical Sciences ASIANALYSIS I11 Details can be found in J. Anal. At. Spectrom. 1995 10 23N. August 20-24 For more information contact Seoul Korea Nah-al Sciences Seoul Nation; University Seoul 151-742 Korea. Telephone + 82(2)880-6638; Fax + 82(2)889-1568; E-mail hausukim@KRSNUCC 1 .BITNET Journal of Analytical Atomic Spectrometry July 1995 Vol. 10 43 NColloquium Spectroscopicum Internationale (CSI) XXIX August 27-September 1 Leipzig Germany Details can be found in J.Anal. At. Spectrom. 1993 8 50N. For further details contact Prof. Dr. H. Nickel Forschungszentrum Julich GmbH Institut fur Werkstoffe der Energietechnik/RWTH Aachen D-52425. Telephone (02461) 61 55 65; Fax (02461) 61 36 99. Colloquium Spectroscopicum Internationale (CSI) XXIX Post Symposium Laser Techniques in Analytical Atomic Spectrometry September 1-3 Berlin Germany Details can be found in J. Anal. At. Spectrom. 1995 10 39N For further information contact Dr. E. Hoffmann ISAS-LSMU D-12484 Berlin Germany. Telephone 49-30- 6391-3552; Fax 49-30-6392-3544 Colloquium Spectroscopicurn Internationale (CSI) XXIX Post Symposium ICP-MS September 1-4 WernigerodelHartz Germany Details can be found in J.Anal. At. Spectrom. 1994 9 46N. For further details contact Dr. L. Moenke Martin-Luther University Halle-Wittenberg Department of Chemistry Institute of Analytical and Environmental Chemistry Weinbergurg 16 D-06120 Halle Germany. Fax 0049-345-649065. Colloquium Spectroscopicum Internationale (CSI) XXIX Post Symposium Glow Discharges in Optical and Mass Spectrometry September 1-4 Dresden Germany Details can be found in J. Anal. At. Spectrom. 1995 10 39N For further information contact Dr V. Hoffmann IFW PF 270016 D-01171 Dresden Germany. Telephone 49-351-2322-397; Fax 49-351-2322-314; e-mail hoffmannaifw-dresden.d4OO.de Colloquium Spectroscopicum Internationale (CSI) XXIX Post Symposium Electrothermal Atomization in Analytical Atomic Spectroscopy September 3-5 Wiirzburg Germany Details can be found in J.Anal. At. Spectrom. 1995 10 40N For further information contact Dr. B. Welz Department of Applied Research Bodenseewerk Perkin-Elmer GmbH Postfach 101761 D-88647 Uberlingen Germany. Telephone + 49 (7551) 81-3791; Fax -t49 (7551) 1612. Euroanalysis IX September 1-7 Bo 1 ogna It a ly Details can be found in J. Anal. At. Spectrom. 1995 10 14N. Further information is available from Professor Luigia Sabbatini Euroanalysis IX Dipartimento di Chimica Universita di Bari Via Orabona 4 70126 Bari Italy. 8th International Conference on Coal Science September 10-15 Instituto Nacional del Carbon CSIC Apartado 73 33080 Ouiedo Spain Details can be found in J. Anal. At. Spectrom. 1994 9 61N.For further details contact Dr. Juan M. D. Tascon 8th ICCS Scientific Programme Chairman Instituto Nacional del Carbon CSIC Apartado 73 33080 Oviedo Spain. Telephone + 34.8.528.08.00; Fax + 34.8.529.76.62. Sixth Surrey Conference on Plasma Source Spectrometry September 17-20 Jersey UK Details can be found in J. Anal. At. Spectrom. 1995 10 19N. For further details contact Dr. K. Jarvis NERC ICP-MS Facility Centre for Analytical Res. in the Environment (CARE) Imperial College at Silwood Park Buckhurst Road Ascot Berkshire SL5 7TE UK. Telephone +44(0) 344 294517; Fax +44(0) 344 873997. European Workshop in Chemometrics September 17-22 Bristol UK Details can be found in J. Anal. At. Spectrom. 1995 10 24N. For further details contact Mrs. C. Hutcheon School of Chemistry University of Bristol Contock’s Close Bristol BS8 lTS UK.Telephone +44(0) 117-928 7645 ext. 4221; Fax +44-(0)117-925 1295. Federation of Analytical Chemistry and Spectroscopy Societies Conference October 15-20 Cincinnati Ohio USA Details can be found in J. Anal. At. Spectrorn. 1995 10 19N. For further information contact Joseph A. Caruso FACSS National Office 198 Thomas Johnson Dr. Suite S-2 Frederick MD 21702 USA. Telephone (301) 694-8122; Fax (301) 694-6860. Short Course COSHH October 31-November 1 Shefield UK Details can be found in J. Anal. At. Spectrom. 1995 10 34N. For further information contact Ms Baldham or Ms Rogers Division of Adult Contiuning Education University of Sheffield 196-198 West Street Sheffield S1 4CT UK. Telephone 01 14 2825391; Fax 01 14 2768653 First Mediterranean Basin Conference on Analytical Chemistry November 5- 10 Cordoba Spain For further details contact Prof.Alfred0 Sanz-Medel Department of Physical and Analytical Chemistry Faculty of Chemistry. University of Oviedo C/ Julian Claveria no 8. 3006 Oviedo (Spain). Telephone 34/85/ 103474-103485; Fax 34/85/103480. Short Course Environmental Auditing in Manufacturing and Process Industries November 7 Shefield UK Details can be found in J. Anal. At. Spectrom. 1995 10 34N. For further information contact Ms Baldham or Ms Rogers Division of Adult Continuing Education University of Sheffield 196-198 West Street Sheffield S1 4CT UK. Telephone 01 14 2825391; Fax 01 14 2768653 Biological Applications of Inorganic Mass Spectrometry November 8-9 Norwich UK Details can be found in J.Anal. At. Spectrom. 1995 10 20N. For further information contact Dr. Fred Mellon Institute of Food Research Norwich Laboratory Norwich Research Park Colney Norwich NR4 7UA UK. Telephone +44(0)1603 255 299 (direct line) +44 (0) 1603 255 000 (switchboard/paging); Fax + 44 (0) 1603 452578 + 44 (0) 1603 fred.mellon@BBSRC.AC.UK. 507723; E-MAIL 44N Journal of Analytical Atomic Spectrometry July 1995 Vol. 10Short Course Safe Storage of Hazardous Substances November 23 Shefield UK Details can be found in J. Anal. At. Spectrom. 1995 10 34N. For further information contact Ms Baldham or Ms Rogers Division of Adult Continuing Education University of Sheffield 196-198 West Street Sheffield S1 4CT UK. Telephone 01 14 2825391; Fax 01 14 2768653 Short Course Disposal of Hazardous Waste December 5 Shefield UK Details can be found in J.Anal. At. Spectrom. 1995 10 34N. For further information contact Ms Baldham or Ms Rogers Division of Adult Continuing Education University of Sheffield 196-198 West Street Sheffield S1 4CT UK. Telephone 01 14 2825391; Fax 01 14 2768653 International Symposium on Environmental Biomonitoring and Specimen Banking December 17-22 Honolulu Hawaii USA Details can be found in J. Anal. At. Spectrom. 1994 9 59N. For further information contact K. S. Subramanian Environmental Health Directorate Health Canada Tunney's Pasture Ottawa Ontario K1A OL2 Canada (phone 613-957-1874; fax 613-941-4545) or G. V. Iyengar Center for Analytical Chemistry Room 235 B 125 National Institute of Standards and Technology Gaithersburg MD 20899 USA (Telephone 301-975-6284; Fax 301-921-9847) or M.Morita Division of Chemistry and Physics National Institute for Environmental Studies Japan Environmental Agency Yatabe-Machi Tsukuba Ibaraki 305 Japan (Telephone 81-298-51-6111 ext. 260; Fax 8 1-298-56-4678). 1996 1996 Winter Conference on Plasma Spectrochemistry January 8-13 Fort Lauderdale Florida USA Details can be found in J. Anal. At. Spectrom. 1994,9,53N. For further information contact Dr. R. Barnes ICP Information Newsletter Department of Chemistry Lederle GRC Towers University of Massachusetts Box 34510 Amherst MA 01003-4510 USA. Telephone (413) 545 2294; Telefax (413) 545 4490. International Schools and Conferences on X-Ray Analytical Methods January 18-25 Sydney Australia Details can be found in J.Anal. At. Spectrom. 1994,9,47N. For further information contact AXAA '96 Secretariat GPO Box 128 Sydney NSW 2001 Australia. Telephone 61 2 262 2277; Fax 61 2 262 2323; Telex AA 176511 TRHOST. Analytica Conference 96 April 23-26 Munich Germany Details can be found in J. Anal. At. Spectrom. 1994,2,69N. For further information contact Messe Miinchen GmbH Messegelande D-80325 Munchen Germany. Telephone + 49 89 51 07-0; Telex 5 212 086 ameg d; Fax +49 89 51 07-177. Eighth Biennial National Atomic Spectroscopy Symposium July 17-19 University of East Anglia Norwich UK For further information contact Dr. S. J. Haswell School of Chemistry University of Hull Hull HU6 7RX UK. Telephone + 44 (0)482-465469; Fax +44 (0)482-466410. Journal of Analytical Atomic Spectrometry July 1995 Vol. 10 45N

ISSN:0267-9477    

DOI:10.1039/JA99510043Nb

出版商:RSC    

年代:1995

数据来源: RSC

摘要:

FUTURE ISSUES WILL INCLUDE- Some Observation on the On-line Anion-exchange Preconcentration for Microwave Plasma Torch Atomic Emission Spectrometry-Jin Qinhan Zhang Hanqi Feng Liang Aerosol Deposition Direct Sample Insertion for Ultra-trace Elemental Analysis by Inductively Coupled Plasma Mass Spectrometry-Robin Rattray Eric D. Salin Matrix Modifier Methods for the Determination of Bismuth and Silver in Nickel-based Alloys and Steels by Zeeman Electrothermal Atomization Spectrometry-Brynmor Mile Christopher C. Rowlands Alice V. Jones Is Palladium or a Mixture of Palladium and Magnesium Nitrate a More Universal Chemical Modifier for Electrothermal Atomic Absorption Spectrometry- Shan Xiao-Quan Wen Bei Mechanism of Vaporization of Sulfur in Electrothermal Vaporization Inductively Coupled Plasma Mass Spectrometry- D.Conrad Gregoire Hirohito Naka Determination of Chromium(v1) and Total Chromium by Inductively Coupled Plasma Atomic Emission Spectrometry after Preconcentration with Solvent Extraction and Back- extraction-Jamshid L. Manzoori Farzaneh Shemirani A Non-destructive Sampling Method of Metals and Alloys for Laser Ablation Inductively Coupled Plasma Mass Spectrometry-Angelika Raith Robert C. Hutton I. D. Abell J. Crighton Determination of Arsenic Species by High-Performance Liquid Chromatography-Ultrasonic Nebulizer-Atomic Fluorescence Spectrometry-Agnes Woller Zolian Mester Peter Fodor Determination of the Scandium Content of High-purity Titanium Using Inductively Coupled Plasma Mass Spectrometry and Glow Discharge Mass Spectrometry as Part of its Certification as a Reference Material-Andrea Held Philip D. P.Taylor C. Ingelbrecht Journal of Analytical Atomic P. De Bievre J. A. C. Broekaert M. Van Straaten Renaat Gijbels Trace Determination of Arsenic Species in Natural Waters by Coupled High- performance Liquid Chromatography- Inductively Coupled Plasma Mass Spectrometry-P. Thomas K. Sniatecki Analytical Characteristics of an Inductively Coupled Plasma Mass Spectrometer Coupled with a Thermospray Nebulization System- Hans Vanhoe Steven Saverwijns Magali Parent Luc Moens Richard Dams Cluster Formation Processes in Laser and Spark Plasmas of Rare Earth Oxide-Graphite Mixtures- Johanna Sabine Becker Hans-Joachim Dietze Extraction of Trace Elements in Coal Fly Ash and Subsequent Speciation by High-performance Liquid Chromatography with Inductively Coupled Plasma Mass Spectrometry - Wang Jiansheng Medha J.Tomlinson Joseph A. Caruso Spectrometry July 1995 Vol. 10 45NStable Isotope Approach to Fission Product Element Studies of Soil-to- Plant Transfer and In Vitro Modelling of Ruminant Digestion using Inductively Coupled Plasma Mass Spectrometry- Paul Robb Linda M. W. Owen Helen M. Crews Atomic Absorption Spectrometric Determination using a Multi-purpose Dialyser in a Flow-injection System- J. F. Van Staden C. J. Hattingh Comparison between Direct Current Radiofrequency and Glow Discharge Mass Spectrometry for the Analysis of Oxide-Based Samples- Stefan De Gendt R. E. Van Grieken W. Hang W. W. Harrison Comparison of the Depth Resolution for Direct Current and Radiofrequency Mode in Glow Discharge Optical Emission Spectrometry- Frank Prassler Volker Hoffmann Joachim Schumann Klaus Wetzig Thermospray Device of Improved Design for Application in Inductively Coupled Plasma Mass Spectrometry- Christoph Thomas Norbert Jakubowski Dietmar Stuewer Jose A.C. Broekaert Wavelength Modulation Diode Laser Atomic Absorption Spectrometry in Modulated Low-pressure Helium Plasmas for Element Selective Detection in Gas Chromatography- Aleksandr Zybin Christoph Schnurer- Patschan Kay Niemax A Permanent Iridium Thermochemical Modifier for Electrothermal Atomic Absorption Spectrometry- Cornelius J. Rademeyer Bernard Radziuk Natalie Romanova Nils Petter Skaugset Asbjorn Skogstad Yngvar Thomassen Spark Ablation as Sampling Device for Inductively Coupled Plasma Mass Spectrometry Analysis of Low-alloyed Steels-Aurora G.Coedo M. T. Dorado B. Fernandez Determination of Germanium in Environmental Samples by Electrothermal Atomic Absorption Spectrometry with Continuous Flow Hydride Generation in Dilute Perchloric Acid Solution-Ni Zhe-Ming He Bin COPIES OF CITED ARTICLES The Royal Society of Chemistry Library can usually supply copies of cited articles. For further details contact The Library Royal Society of Chemistry Burlington House Piccadilly London W1V OBN UK. Tel +44 (0) 71-437 8565; fax +44 (0) 71-287 9798; Telecom Gold 84; BUR210; Electronic Mailbox (Internet) LIBRARY@RSC.ORG. If the material is not available from the Society’s Library the staff will be pleased to advise on its availability from other sources. Please note that copies are not available from the RSC at Thomas Graham House Cambridge.Royal Society of Chemistry Analytical Division Atomic Spectroscopy Group Eighth Biennial National Atomic Spectroscopy Symposium 8th BNASS University of East Anglia UK 17-20 July 1996 Plenary Lecturers Invited Lecturers Call for Papers social Programme Workshop Further Details Dr S J Hill Professor N Furuta. Professor F Adam Professor J M Mermet and Professor G Hieftje Dr 0 Donard Dr S J Parry Dr S Faitweather-Tait Dr A Ellis Dr A G Howard Dr J Brenner Dr J Marshall Dr N J Miller-lhli Dr S Tanner and Professor D Littlejohn Contributed oral and poster presentations on recent developments in both pure and applied atomic spectroscopy - analytical applications theoretical studies or fundamentd advances in AAS AES AFS inorganic MS and XRF. Three copies of abstracts must be submitted before 28 February 1996. BNASS has an enviable reputation of being a friendly and dynamic meeting. A number of social events including a Symposium Dinner will form an integral part of the meeting. Immediately prior to the 8th BNASS there will be a Short Course on Sample Pre-treatment and Sample Introduction for Atomic Spectroscopy 17 July a.m. 1996. Ms Brenda Holliday. Royal Society of Chemistry Thomas Graham House Science Park Milton Road Cambridge CB4 4WF. UK. Tel +44 (011223 420066; Fax 4 4 (0)1223 420247; E-mail JA AS @ RSC.ORG 46 N Journal of Analytical Atomic Spectrometry July 1995 Vol. 10

ISSN:0267-9477    

DOI:10.1039/JA995100045N

出版商:RSC    

年代:1995

数据来源: RSC

摘要:

95/1598 95/1599 95/1600 95/160 1 95/1602 95/ 1603 95/1604 95/1605 95/1606 95/1607 971 608 95/1609 95/16 10 Nilsson U. Skerfving S. In uiuo X-ray fluorescence measurements of cadmium and lead. Scand. J. Work Enuiron. Health 1993 19 54. (Dept. Radiat. Phys. Malmoe Gen. Hosp. Malmoe Sweden). Mesjasz-Przybylowicz J. Balkwill K. Przybylowicz W. J. Annergarn H. J. Proton microprobe and X-ray fluorescence investigations of nickel distribution in serpentine flora from South Africa. Nucl. Instrum. Methods Phys. Res. Sect. B 1994,89 208. (Department of Botany University of Witwatersrand 2050 Johannesburg South Africa). Ayla J. M. Buergo M. A Xiberta J. Use of energy dispersive X-ray fluorescence (EDXRF) as an approxi- mate method of analysing ash and sulfur content in the coals of the Asturias Spain.Nucl. Geophys. 1994 819 99. (Dept. Cienc. Mater. e Ing. Metal. Esc. Tec. Super. Ing. Minas Oviedo Spain). Dos Santo J. M. F. Conde C. A. N. Application of gas proportional scintillation counters to the analysis of sulfur in coal. Nucl. Geophys. 1994 8 103. (Phys. Dept. Univ. Coimbra Coimbra P-3000 Portugal). Esche H. J. Determination of the chromium or zirconium content in leather by X-ray analysis. Ger. Offen. DE 4,218,426 (CI GOlN33/44) 24 Mar 1994 Appl. 04 Jun 1993; 3 pp. (Amtec Analysenmesstechnik GmbH Germany). Feret F. R. Application of XRF in the aluminium industry. Adv. X-Ray Anal. 1993 36 121. (Arvida Res. Dev. Centre Alcan Int. Ltd. Jonquiere Quebec Canada G7S 4K8). Suigiura C. La X-ray emission spectra of copper compounds and alloys.J. Phys. SOC. Jpn. 1994 63 1835. (Fac. Eng. Utsunomiya Univ. Utsonomiya 3 12 Japan). Compoca V. Caragheorgheopol Gh. Lazarovici D. Lazarovici C. Ruscu. R. Evaluation of a silicon photodiode as an X-ray and gamma-ray detector. Muter. Res. Soc. Symp. Proc. 1993 302 579. (Inst. At. Phys. 76900 Bucharest Romania). Nabais Conde C. A.. Margues Ferreira Dos Santos J. Sena Sao Miguel Benito A. Gas proportional scintil- lation counter for ionizing radiation with medium and large size radiation windows and/or detection volumes. PCT Int. App. WO 94 09,509 (Cl. HOlJ47/06) 28 Apr 1994 PT Appl. 100,968 15 Oct 1992; 18 pp. Urch D. S. Chemical state analysis chemical effects in soft X-ray spectra. Anal. Proc. (London) 1994 31 38. (Dept. Chem. Queen Mary and Westfield Coll. London UK El 4NS). Ban S.Hirayama H. Namito Y. Tanaka S. Nakashima H. Nakane Y. Nariyama N. Calibration of silicon PIN photodiode for measuring intensity of 7-40 keV photons. J. Nucl. Sci. Technol. 1994 31 163. (Natl. Lab. High Energy Phys. Tsukuba 305 Japan). Rao D. E. Cesareo R. Gigante G. E. Measurement of X-ray fluorescence cross-sections in heavy elements excited by 17.78 25.88 26.88 and 32.89 keV photons. Appl. Radiat. Isot. 1994 45 621. (Dip. Fis. Univ. Roma “La Sapienza” 00186 Rome Italy). Macgowan B. J. Mrowka S. Barbee T. W. Jr. Da Silva L. B. Eder D. C. Koch J. A Turner J. A. Underwood J. H. Development of robust multilayer optics for use in high-peak power radiation environ- ments. Muter. Res. SOC. Symp. Proc. 1993 306 145. (Lawrence Livermore Natl. Lab.Univ. California CA 94450 USA). 95/1611 9511612 95/1613 95/1614 951161 5 95/16 16 95/1617 95/1618 95/1619 95/1620 95/162 1 95/1622 95/1623 9511624 Morahashi S. Radiation detector elements. Jpn. Kokao Tokkyo Koho JP 06 37,345 [94 37,3451 (Cl. HOlL31/09) 10 Feb 1994 Appl. 921191,127 17 Jul 1992; 8pp. (Fujitsu Ltd Japan). Bernasconi G. Haselberger N. Markowicz A Valkovic V. Applications of a capillary X-ray micro- fluorescence system. Nucl. Instrum. Methods Phys. Res. Sect. B 1994 86 333. (IAEA Labs. A-2444 Seibersdorf Austria). Marumo K. Bench top X-ray fluorescence analyser. Its application to geological sample analyses. Shigen Chishitsu 1994 44 51. (Min. Resour. Dept. Geol. Surv. Japan Tsukuba Japan). Khan K. M. Analytical technique of absorption correc- tions for analysts of semi-thin specimens.J. Nut. Sci. Math. 1993 33 235. (Nucl. Phys. Div. Pakistan Inst. Nucl. Sci. Technol. Islamabad Pakistan ). Komatsu B. Myazaki K. Shimazaki A. Analysis of contamination elements. Jpn. Kokai Tokkyo Koho JP 06 88,792 [94 88,7921 (Cl. GOlN23/223) 29 Mar 1994 Appl. 92/238,535 07 Sep 1992; 5 pp. (Tokyo Shibaura Electric Co. Japan). Orihashi Y. Yuhara M. Kagami H. Honma H. Trace element analysis of silicate rocks by XRF. Tech. Rep. ISEI Ser. B 1993 13 29pp. (Inst. Study Earth’s Inter. Okayama Univ. Tottori 682-01 Japan). Nakamura M. Misawa Y. Nagai S. Analysis of metallic elements in semiconductor crystals. Jpn. Kokai Tokkyo Koho JP 06,109,718 [94,109,718] (Cl. GOlN33/00) 22 Apr 1994 Appl. 92/258,108 28 Sep 1992; 4 pp. (Hitachi Ltd.Japan). Iihara J. Kawai J. Sekine T. Yoshihara K. Characteristic features of KP X-rays depending on sodium contents in Na,O-SiO glasses. Int. J. PIXE 1993 3 177. (Fac. Sci. Tohoku Univ. Sendai 980 Japan). Sieber J. R. Quantitative XRF determinations of additive elements in greases for manufacturing specifi- cations. Adv. X-Ray Anal. 1993 36 155. (Res. Dev. Dept. Texaco Inc. Beacon NY USA). Stropnik B. Byrne A. R. Smodis B. Air pollution monitoring by ED XRF in the Salek Valley Part 1. Acta Chim. Slov. 1993 40 301. (“Jozef Stefan” Inst. Univ. Ljubljana Ljubljana 61 111 Slovenia). Mitarai T. Akagi S. Maeda M. Development of the technique to determine the end-point of the slag- making stage in copper converter. Converting Fire ReJn. Cast. Proc. Symp. 1994 169. (Saganoseki Smelter Refin.Nippon Min. Met. Co. Ltd. Saganoseki 879-22 Japan). Gao N. Cheng M.d. Hopke P. K. Receptor modelling of airborne ionic species collected in SCAQS. Atmos. Enuiron. 1994 28 1447. (Dept. Chem. Clarkson Univ. Potsdam NY 13699-5810 USA). Elnimir T. Moharram B. M. Studies on human exposure to environmental lead in Tanta. Radioisotopes 1994 43 197. (Radioanal. Res. Lab. Tanta Univ. Tanta Egypt). Adejumo J. A. Obioh I. B. Ogunsola 0. J. Akeredolu F. A. Olaniyi H. B. Asubiojo 0. I. Oluwole A. F. Akanle 0. A. Spyrou N. M. Atmospheric deposition of major minor and trace elements within and around three cement factories. J. Radioanal. Nucl. Chem. 1994 179 195. (Dept. Phys. Obafemi Awolowo Univ. Ile- Ife Nigeria). ATOMIC SPECTROMETRY UPDATES-REFERENCES Journal of Analytical Atomic Spectrometry July 1995 Vol.10 173R9 511 625 9511626 9511627 9511628 9511629 9511630 9511631 9511632 9511633 9511634 9511635 9511636 9511637 9511638 9511639 174R Oluyemi E. A. Asubiojo 0. I. Oluwole A. F. Toussaint C. J. N. Elemental concentrations and source identification of air particulate matter at a Nigerian site a preliminary study. J. Radioanal. Nucl. Chem. 1994 179 187. (Dept. Chem. Obafemi Awolowo Univ. Ile-Ife Nigeria). Sahin Y. Durak R. Kurucu Y. Erzeneoglu S. Peak area determination and energy dependence of gamma- and X-ray peak tailing. J. Radioanal. Nucl. Chem. 1994 177 403. (Fac. Sci. Atatuerk Univ. Erzurum 25240 Turkey). Kaneko K. Hirabayashi M. Kumashiro Y. Ihara H. Determination of impurities in refractory carbides nitrides and borides (IV group) by X-ray fluorescence spectrometry.X-sen Bunseki no Shinpo 1993 25 195. (Electrotech. Lab. Tsukuba 305 Japan). Sugihara K. Hata Y. Fujii S. Harada Y. Measurement of metallic impurities in SiOz and at the interface using TXRF. X-sen Bunseki no Shinpo 1993 25 255. (Matsushita Electron. Corp. Kyoto Res. Lab. Kyoto City 601 Japan). Nakai I. Moriguchi M. Suzuki T. Kawashima T. Shimojo N. Total reflection X-ray fluorescence determi- nation of trace amounts of As in mouse tissues with acute arsenic intoxication. X-sen Bunseki no Shinpo 1993 25 269. (Dept. Chem. Univ. Tsukuba Tsukuba 305 Japan). Bhat C. K. Singh B. R. Bhat C. L. Energy-dispersive X-ray fluorescence analysis of Kushan period coins. Curr. Sci. 1994 66 303. (Nucl. Res.Lab. Bhabha At. Res. Centre Jammu 180 004 India). Xu C.4. 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Univ. Coll. Swansea Swansea UK SA2 8PP). Mohamed M. M. Mossaad M. M. Nasra M. K. Nasr F. I. Fikry N. M. Direct introduction of solid and powder samples into a rotating arc plasma jet. Zndian J. Pure Appl. Phys. 1994 32 471. (Med. Res. Inst. Univ. Alexandria Alexandria Egypt). Bamiro F. O. Littlejohn D. Critical examination of the analytical significance of background intensities and RSD on detection limits of elements at different wavelengths in ICP-AES. Znt.J. Chem. 1993 4 129. (Dept. Chem. Sci. Univ. Agric. Abeokuta Nigeria). Journal of Analytical Atomic Spectrometry July 1995 Vol. 10 185R9511970 9511971 9511972 9511973 9511974 9511 975 9 511 976 9511977 9511978 9511979 9511 980 95/ 198 1 9511982 9511983 9511984 186R Hu J.-y. Hirokawa T. Nishiyama F. Kimura G. Kiso Y. Ito K. Shoto E. Analysis for trace rare earth elements in misch metal by means of ITP-PIXE method. Int. J. PIXE 1993 3 89. (Fac. Eng. Hiroshima Univ. Higashi-hiroshima 724 Japan). Eid M. A. Naim G. Mahdy A. A. Nada N. 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Hangzhou 310028 China). Torok Sz. Faigel Gy. Jones K. W. Rivers M. L. Sutton S. R. Bajt S. Chemical characterization of environmental particulate matter using synchrotron radiation. X-Ray Spectrom. 1994 23 3. (Central Res. Inst. Phys. P.O. Box 49 H-1525 Budapest Hungary). Labar J. L. Anomalous X-ray absorption of the Ma lines in the rare earth elements. X-Ray Spectrom. 1994 23 19. (Res. Inst. Tech. Phys. Hungarian Acad. Sci. H-1325 Budapest Hungary). Beckhoff B. Laursen J. Bent and flat highly oriented pyrolytic graphite crystals as small Bragg angle mono- chromators in thin-specimen energy dispersive XRF analysis. X-Ray Spectrom.1994 23 7. (Dept. Phys. Univ. Bremen P.O. 330 D-28334 Bremen Germany). Sweeney R. J. Jablonski W. Sie S. H. Determination of selected trace elements in silicates by electron and proton probe microanalysis. X-Ray Spectrom. 1994 23 91. (Univ. Tasmania G.P.O. 252C Hobart 7001 Australia). Kallithrakas-Kontos N. Katsanos A. A. Efficiency calibration of a Ge( In) semiconductor detector by thin- and thick-target PIXE. X-Ray Spectrom. 1994 23 96. (Dept. Sci. Tech. Univ. Crete GR-73 100 Chania Greece). Altynov V. A. Blokhin S. M. Effect of features of inner atomic shells excitation by accelerated ions on the 951198 5 9511986 9511 987 9511988 951C1989 951c1990 95/c199 1 95/c 1992 951c1993 95lC1994 95/c1995 Journal of Analytical Atomic Spectrometry July 1995 V01.10 shape of the emitted X-ray lines.X-Ray Spectrom. 1994 23 79. (Joint Inst. Nucl. Res. 141980 Dubna Russia). Stoyanchev R. Iliev Tz. Recalov K. Method for quantitative electron microprobe EDS X-ray analysis of small inclusions in matrices with similar composition. X-Ray Spectrom. 1994 23 105. (Inst. Phys. Chem. Bulgarian Acad. Sci. Sofia 11 13 Bulgaria). Valdr6 G. Scanning electron microscopy and X-ray energy dispersive spectroscopy of surface micro- transformations in Ca-P glasses. X-Ray Spectrom. 1994 23 120. (Dept. Mineral. Sci. Piazza di Porta S. Donato 1 1-40126 Bologna Italy ). Bakaleinikov L. A. Tropp E. A. Kinetic equation- based calculation of the electron distribution in the target exposed to the electron beam. X-Ray Spectrom. 1994 23 125. (A. F. Ioffe Phys.-Tech.Inst. RAN Polytechnicheskaya Str. 26 St. Petersburg 194021 Russia). Khadikar P. V. Joshi S. Mangalson N. F. Silk J. E. Effect of counter ions on X-ray absorption discontinuity. X-Ray Spectrom. 1994 23 137. (Chem. Dept. Devi Ahilya Univ. 3 Khatipura Indore-452007 India). Zhu G. Determination of barium content in industrial solid waste by air-acetylene flame atomic absorption spectrometry. Second Asian Symposium on Academic Activity for Waste Treatment and Resources (AAWTR) August 23-25 1994 Hangzhou China (Beijing Municipal Environ. Monitoring Centre Beijing 100044 China ). Ikatsu H. Tanaka M. Shinoda S. Determination of semimetals in treated wastewater by graphite furnace atomic absorption spectrometry after coprecipitation with lanthanum hydroxide.Second Asian Symposium on Academic Activity for Waste Treatment and Resources (AAWTR) August 23-25 1994 Hangzhou China (Center Environ. Sci. Technol. Okayama Univ. Japan). Sun F.-s. Ji X.-x. Study of determination of lead in environmental waters using DDDC-MIBK extraction and flame atomic absorption. Second Asian Symposium on Academic Activity for Waste Treatment and Resources (AAWTR) August 23-25 1994 Hangzhou China (Dept. Environ. Protection Suzhou Inst. Urban Construct. Environ. Protect. Postcode 21 5008 Suzhou Jiangsu China). Yin X.-f. Liu M. Determination of ultra-trace amounts of molybdenum in seawater by flow injection on-line preconcentration graphite furnace atomic absorption spectrometry. Second Asian Symposium on Academic Activity for Waste Treatment and Resources (AAWTR) August 23-25 1994 Hangzhou China (Dept.Chem. Zhejiang Univ. Hangzhou 310027 China). Chen H.-w. Xu S.-k. Fang Z.-1. Flame atomic absorption spectrometric determination of trace amount of copper in environmental samples using flow injection on-line adsorption preconcentration. Second Asian Symposium on Academic Activity for Waste Treatment and Resources (AAWTR) August 23-25 1994 Hangzhou China (Dept. Chem. Hangzhou Univ. Hanzhou 310028 China). Ni Z.-m. He B. Han H.-b. Determination of trace selenium and tellurium in environmental and biological samples. Second Asian Symposium on Academic Activity for Waste Treatment and Resources (AAWTR) August 23-25 1994 Hangzhou China (Res. Centre Eco-Environ. Sci. Acad. Sin. ). Potts P. J. Webb P. C. Thorpe 0.W. Watson J. S. Kilworth R. Field-portable X-ray fluorescence analysis the development of procedures for the chemical charac- terization of 'real' geological samples of irregular shape. Geoanalysis 94 Charlotte Mason Conference Centre Ambleside England September 18-22 1994 (Dept.95/C 1996 95/C 1997 95/C1998 9 5/C 1999 95/C2000 95/C2001 95/C2002 95/C2003 95/C2004 95/C2005 9 5/C2006 Earth Sci. Open Univ. Walton Hall Milton Keynes UK MK7 6AA). Rao T. G. Govil P. K. Merits of using Ba as heavy absorber in major element analysis of rock samples by XRF new data on ASK- 1 and ASK-2 reference samples. Geoanalysis 94 Charlotte Mason Conference Centre Ambleside England September 18-22 1994 (XRF Laboratory Natl. Geophys. Res. Inst. Hyderabad 500 077 India ). Renault J.McKee C. XRF analysis of environmental Pb using thin film principles. Geoanalysis 94 Charlotte Mason Conference Centre Ambleside England September 18-22 1994 (New Mexico Bur. Mines & Min. Resour. New Mexico Inst. Mining & Technol. Campus Station Socorro NM 87801 USA). Cawley J. West M. Wills R. Analysis and characteriz- ation of water treatment plant sludges by X-ray fluorescence spectrometry. Geoanalysis 94 Charlotte Mason Conference Centre Ambleside England September 18-22 1994 (Mater. Res. Inst. Sheffield Hallam Univ. Sheffield UK S1 1WB). Webb P. C. Potts. P. J. Watson J. S. Ramsey M. H. Evaluation of realistic precision and detection limits in XRF analysis for corss-method comparison. Geoanalysis 94 Charlotte Mason Conference Centre Ambleside England September 18-22 1994 (Dept.Earth Sci. Open Univ. Walton Hall Milton Keynes UK MK7 6AA). Elsenbroek J. H. Instrumentation and analytical tech- nique for the analyses of regional geochemical samples used at the South African Geological Survey. Geoanalysis 94 Charlotte Mason Conference Centre Ambleside England September 18-22 1994 (Geol. Surv. South Africa Private Bag X112 Pretoria 0001 South Africa ). Halliday A. N. Christensen J. C. Hall C. M. Jones C. E. Lee D.-C. Teagle D. Walder A. J. Entwistle A. Recent geological developments in inductively coupled plasma multiple collector mass spectrometry. Geoanalysis 94 Charlotte Mason Conference Centre Ambleside England September 18-22 1994 (Dept. Geol. Sci. Univ. Michigan Ann Arbor MI 48109 USA). Nesbitt R. W. Hirata T.Raith A. U-Pb dating of zircons by laser ablation ICP-MS. Geoanalysis 94 Charlotte Mason Conference Centre Ambleside England September 18-22 1994 (Dept. Geol. Univ. Southampton UK SO17 1BJ). Garbe-Schonberg C.-D. Reimann C. Pavlov V. A. Tree ring profiles from pine and birch from industrially polluted areas of the Barents region Russia and Norway as measured by ICP-MS laser ablation. Geoanalysis 94 Charlotte Mason Conference Centre Ambleside England September 18-22 1994 (ICP-MS Lab. Geol. Palaontol. Inst. Olshausenstr. 40 D-24118 Kiel Germany). Chenery S. Cook J. M. Lidiard H. Milton D. Williams C. T. Determination of trace elements in biologically derived materials as environmental indi- cators. Geoanalysis 94 Charlotte Mason Conference Centre Ambleside England September 18-22 1994 (Anal.Geochem. Group British Geol. Surv. Keyworth Nottingham UK NG12 5GG). Jeffries T. Perkins B. Pearce N. Comparisons of infra-red green and ultraviolet laser ablation ICP-MS in mineral analysis. Geoanalysis 94 Charlotte Mason Conference Centre Ambleside England September 18-22 1994 (Geochem. Group Inst. Earth Studies Univ. Wales Aberystwyth Dyfed UK SY23 3DB). Longerich H. P. Jackson S. E. Gunther D. Geoanalysis using a new ultra high sensitivity induc- tively coupled plasma mass spectrometer (ICP-MS) with solution nebulizaiton and laser ablation micro- probe (LAM) sample introduction. Geoanalysis 94 95/C2007 95/C2008 95/C2009 95/C20 10 95/C2011 95/C2012 95/C2013 95/C20 14 95/C2015 95/C2016 95/C2017 Charlotte Mason Conference Centre Ambleside England September 18-22 1994 (Dept.Earth Sci. and Centre Earth Resour. Res. Memorial Univ. Newfoundland St. John’s Newfoundland Canada A1B 3x5). Cave M. Reeder S. Application of multivariate statistical analysis to the reconstruction of pore-water chemistries. Geoanalysis 94 Charlotte Mason Conference Centre Ambleside England September 18-22 1994 (Anal. Geochem. Group British Geol. Surv. Keyworth Nottingham UK NG12 5GG). Coles B. J. Gleeson S. Wilkinson J. J. Ramsey M. H. Improved detection limits for transient signal analysis of fluid inclusion by ICP-AES using correlated background correction (CBC). Geoanalysis 94 Charlotte Mason Conference Centre Ambleside England September 18-22,1994 (Dept. Geol. Imperial Coll. Sci. Technol. and Med. Prince Consort Rd.London UK SW7 2BP). Olsen S. D. Brekke T. Filby R. H. Isaksen G. H. Trace metals in petroleum exploration samples by ICP-MS. Geoanalysis 94 Charlotte Mason Conference Centre Ambleside England September 18-22 1994 (RF-Rogoland Res. P.O. Box 2503 Ullandhaug 4004 Stavanger Norway ). Garnett D. Geoanalytical trends in Australia. Geoanalysis 94 Charlotte Mason Conference Centre Ambleside England September 18-22 1994 (Becquerel Labs. PMB 1 Menai NSW 2234 Australia). Giblin A. Detection of concealed ore-deposits in Australia using high quality groundwater analyses. Geoanalysis 94 Charlotte Mason Conference Centre Ambleside England September 18-22 1994 (CSIRO Div. Explor. Min. P.O. Box 136 North Ryde NSW 2113 Australia ). Liezers M. Improved isotope ratio measurements at low concentrations using enhanced performance quad- rupole ICP-MS.Geoanalysis 94 Charlotte Mason Conference Centre Ambleside England September 18-22 1994 (Fisons Instruments Elemental Analysis Road Three Ion Path Winsford Cheshire UK CW7 3BX). Porteous N. C. Walsh J. N. Jarvis K. E. Measurement of boron isotope ratios in groundwater studies. Geoanalysis 94 Charlotte Mason Conference Centre Ambleside England September 18-22 1994 (Geol. Dept. Royal Holloway Coll. Univ. London Egham Surrey UK TW20 OEX). Dulski P. Distribution of Y and REE in fluorite an ICP-MS study employing decomposition with AlCl solution. Geoanalysis 94 Charlotte Mason Conference Centre Ambleside England September 18-22 1994 (PB 4.3 GeoForschungszentrum Potsdam Telegrafen- berg A50 D-14473 Potsdam Germany).Jain J. Xie Q.4 Kerrich R. Determination of high field strength elements in geological samples by induc- tively coupled plasma mass spectrometry. Geoanalysis 94 Charlotte Mason Conference Centre Ambleside England September 18-22 1994 (Dept. Geol. Sci. Univ. Saskatchewan Saskatoon Saskatchewan Canada S7N OWO). Enzweiler J. Potts P. J. Jarvis K. Development of a rapid method for the determination of the platinum group elements by isotope dilution ICP-MS based on a sodium peroxide fusion and tellurium coprecipitation. Geoanalysis 94 Charlotte Mason Conference Centre Ambleside England September 18-22 1994 (Dept. Earth Sci. Open Univ. Walton Hall Milton Keynes UK MK7 6AA). Jarvis K. E. Totland M. M. Jarvis I. Ion exchange chromatography for the separation and preconcen- tration of the platinum group elements and gold for low level determination in geological samples. Geoanalysis 94 Charlotte Mason Conference Centre Journal of Analytical Atomic Spectrometry July 1995 Vol.10 187RAmbleside England September 18-22 1994 (NERC ICP-MS Facility Centre Anal. Res. Environ Imperial Coll. Silwood Park Ascot Berks UK SL5 7TE). 95/C2018 Malcus F. Johansson G. On-line trace metal precon- centration and matrix replacement for graphite furnace AAS. Geoanalysis 94 Charlotte Mason Conference Centre Ambleside England September 18-22 1994 (Dept. Anal. Chem. Univ. Lund P.O. Box 124 S-221 00 Lund Sweden). 95/C2019 Adkins R. L. Walsh N. Edmunds M. Trafford J. M. ICP-AES analysis of low levels of selenium in natural waters.Geoanalysis 94 Charlotte Mason Conference Centre Ambleside England September 18-22 1994 (Dept. Geol. Royal Holloway Univ. London Egham Hill Egham Surrey UK TW20 OEX). 95/C2020 Djane N.-K. Malcus F. Martins E. Sawula G. Johansson G. Field samplers for trace metal enrichment from natural waters using hollow fibres. Geoanalysis 94 Charlotte Mason Conference Centre Ambleside Geoanalysis 94 Charlotte Mason Conference Centre Ambleside England September 18-22 1994 (Dept. Geol. and Geophys. Univ. Edinburgh Edinburgh UK EH9 3JW). 95/C2030 Richardson J. M. Start-up of a new laboratory validation of 26 methods in 12 months Geoscience Laboratories Ministry of Northern Development and Mines Ontario Canada. Geoanalysis 94 Charlotte Mason Conference Centre Ambleside England September 18-22 1994 (Geosci.Labs. Ontario Geoservices Centre Sudbury Ontario Canada P3E 6B5). 95/C2031 van Meerten Th. G. Bode P. Reference materials and professional skills in the quality assurance of an accredited laboratory for instrumental neutron acti- vation analysis. Geoanalysis 94 Charlotte Mason Conference Centre Ambleside England September 18-22 1994 (Interfaculty Reactor Inst. Delft Univ. Technol Mekelweg 15 2629JB Delft Netherlands). England September 18-22 1994 (Anal. C%em. DW. 95/C2032 Beck R. Cohen D. New type of synthertic geochemical Univ. Lund Lund Sweden). standard-SmTEs. Geoanalysis 94 Charlotte Mason 95/C2021 Steinnes E. Enrichment of metals in the organic surface layer of natural soil identification of contributions from different mechanisms.Geoanalysis 94 Charlotte Mason Conference Centre Ambleside England September 18-22 1994 (Dept. Chem. Univ. Trondeim Norway). 95/C2022 Vaganov P. A. Rongsheng Z. Pets L. I. Neutron activation study of combustion products at power plants fired by solid fossil fuel. Geoanalysis 94 Charlotte Mason Conference Centre Ambleside England September 18-22 1994 (Fac. Geol. Univ. St. Petersburg 199034 Russia). 95/C2023 Kolesov G. M. Sapozhnikov D. Y. Nazarov M. A. Neutron activation determination of noble metals in samples of terrestrial and cosmic origin. Geoanalysis 94 Charlotte Mason Conference Centre Ambleside England September 18-22 1994 (V.I. Vernadsky Inst. Geochem. and Anal. Chem. Russian Acad. Sci. 117975 Kosygin St. 19 Moscow Russia). 95/C2024 Brunfelt A. 0.Neutron activation analysis of rocks and mineral separates. Geoanalysis 94 Charlotte Mason Conference Centre Ambleside England September 18-22 1994 (Mineral.-Geol. Museum Sarsgt 1 0562 Oslo Norway). 95/C2025 Steinnes E. Frontasyeva M. Epithermal neutron activation analysis of mosses used to monitor heavy metal deposition around an iron smelter complex. Geoanalysis 94 Charlotte Mason Conference Centre Ambleside England September 18-22 1994 (Dept. Chem. Univ. Trondheim AVH N-7055 Dragvoll Norway). 95/C2026 Bode P. Overwater R. M. W. Lakmaker 0. Analysis of very large samples - with sizes up to 50kg - by instrumental neutron activation analysis new oppor- tunities for geological analysis. Geoanalysis 94 Charlotte Mason Conference Centre Ambleside England September 18-22 1994 (Interfaculty Reactor Inst.Delft Univ. Technol. Mekelweg 15 2629JB Delft Netherlands). 95/C2027 Parry S. J. Neutron activation analysis for the determination of platinum group elements and gold in five new certified reference materials. Geoanalysis 94 Charlotte Mason Conference Centre Ambleside Conference Centre Ambleside England September 18-22 1994 (Water Res. Lab. Univ. NSW Manly Vale 209 3 Australia). 95/C2033 Govindaraju K. Potts P. J. Webb P. C. Watson J. S. Characterization of two new GIT-I WG silicate reference materials dolerite WS-E and micro-gabbro PM-S results of an international cooperative analysis pro- gramme. Geoanalysis 94 Charlotte Mason Conference Centre Ambleside England September 18-22 1994 (Geostandards CRPG 15 rue Notre Dame des Pauvres BP 20 54501 Vandoeuvre Cedex France).95/C2034 Rucklidge J. Accelerator mass spectrometry in environ- mental geoscience-a new frontier. Geoanalysis 94 Charlotte Mason Conference Centre Ambleside England September 18-22 1994 (IsoTrace Lab. Dept. Geol. Univ. Toronto Toronto Ontario Canada M5S 3B1). 95/C2035 Watling R. J. Barrow I. Herbert H. K. Thomas A. Analysis of diamonds and indicator minerals for diamond exploration by laser ablation inductively coupled plasma mass spectrometry ( LA-ICP-MS). Geoanalysis 94 Charlotte Mason Conference Centre Ambleside England September 18-22 1994 (Chem. Centre (WA) 125 Hay St. E. Perth W. Australia 6004 Australia ). 95/C2036 Smith J. V. Synchrotron X-ray sources new appli- cations in microanalysis tomography absorption spec- trometry and diffraction.Geoanalysis 94 Charlotte Mason Conference Centre Ambleside England September 18-22,1994 (Dept. Geophys. Sci. and Centre Adv. Radiat. Sources Univ. Chicago Chicago IL 60637 USA). 95/C2037 Hall G. E. M. Great leap forward hydrogeochemical surveys. Geoanalysis 94 Charlotte Mason Conference Centre Ambleside England September 18-22 1994 (Geol. Surv. Canada 601 Booth St. Ottawa Canada K1A OE8). 95/C2038 Govindaraju K. Expanding IWG-GIT GEOSTAN data- bases. Geoanalysis 94 Charlotte Mason Conference Centre Ambleside England September 18-22 1994 (Centre de Rech. Petrograph. et Geochem. CNRS BP 20 54501 Vandoeuvre-Nancy France). September 18-22 1994 (Centre 95/C2039 Remond G. Packwood R. H. Standards for microbeam techniques application of ion implantation.Geoanalysis 94 Charlotte Mason Conference Centre Ambleside Environ. Imperial Coll. Silwood Park Buckhurst Rd. Ascot Berks. UK SL5 7TE). 95/C2028 de Souza H. A. F. Crabtree D. Miller S. Comparison of quantitative mineralogical methods. Geoanalysis 94 ~$~~~ ~ t ~ b e " 0 ~ ~ ~ ~ 1 9 ~ ~ ~ ~ e 0 ~ ~ b ~ ~ ~ ~ ~ Ontario Geoservices Centre Sudbury Ontario Canada P3E 6B5). probe analysis of trace element reference materials. England September 18-22 1994 (BRGM DR/GGP BP 6009,45060 Orleans Cedex 2 France). 95/C2040 Kane J. S. Beary E. S. Murphy K. E. Paulsen P. J. Impact of ICP-MS on certification programmes for geochemical reference materials. Geoanalysis 94 Charlotte Mason Conference Centre Ambleside 95/C2029 Hinton R. W. Witt-Eickschen G. Harte B. Ion England September 18-22 1994 (Natl.Inst. Stand. Technol. Gaithersburg MD 20899 USA). 188R Journal of Analytical Atomic Spectrometry July 1995 Vol. 1095/C2041 95/C2042 95/C2043 95/C2044 95/C2045 95/C2046 95/C2047 95/C2048 95/C2049 9 5/C20 50 95/C205 1 95lC2052 Perkins B. Pearce N. Jeffries T. Application of infra- red and ultraviolet laser ablation ICP-MS in mineral analysis. 1995 European Winter Conference on Plasma Spectrochemistry Cambridge UK January 8-1 3 1995 (Inst. Earth Studies Univ. Wales Aberystwyth Dyfed UK SY23 3BD). Turner P. J. Enhancements to ion sampling methods for ICP-MS. 1995 European Winter Conference on Plasma Spectrochemistry Cambridge UK January 8-13 1995 (Finnigan MAT Ltd. Paradise Heme1 Hempstead Herts UK HP2 4TG). Jakubowski N. Feldmann I.Stiiwer D. Analysis of steel samples by use of high resolution ICP and GD mass spectrometry. 1995 European Winter Conference on Plasma Spectrochemistry Cambridge UK January 8-13,1995 (Inst. Spektrochem. Angewandte. Spektrosk. P.O.B. 10 13 52 D-44013 Dortmund Germany). Greb U. Rottmann L. Hamester M. Jung G. Laser B. Application examples of high resolution ICP-MS. 1995 European Winter Conference on Plasma Spectrochemistry Cambridge UK January 8-13 1995 (Finnigan MAT GmbH Barkhausenstr. 2 D-28197 Bremen Germany). Reed N. M. Hutton R. C. Marriott P. Characteristics of a new high performance/high resolution ICP-MS instrument. 1995 European Winter Conference on Plasma Spectrochemistry Cambridge UK January 8-13 1995 (F.I. Elemental Analysis Ion Path Road Three Winsford Cheshire UK CW5 3BX).Cave M. Multi-element drift correction procedure for ICP-OES by background emission line monitoring and drift prediction by principle component analysis model- ling. 1995 European Winter Conference on Plasma Spectrochemistry Cambridge UK January 8-13 1995 (Anal. Geochem. Group British Geol. Surv. Keyworth Nottingham UK NG12 5GG). Perkins C. V. Gamaury S. Effect of integration time on RSDs in inductively coupled plasma emission spectrometry misconceptions and the reality. 1995 European Winter Conference on Plasma Spectro- chemistry Cambridge UK January 8-13 1995 (AT1 Unicam York St. Cambridge UK CB1 2PX). Koirtyohann S. R. Yates D. Effects of saturation and blooming on a segmented CCD array detector. 1995 European Winter Conference on Plasma Spectrochemistry Cambridge UK January 8- 13 1995 (Dept.Chem. Univ. Missoure Columbia MO 6521 1 USA). Vanhoe H. Parent M. Moens L. Dams R. Analytical characteristics of an inductively coupled plasma mass spectrometer coupled with a thermospray nebulization system. 1995 European Winter Conference on Plasma Spectrochemistry Cambridge UK January 8-13 1995 (Lab. Anal. Chem. Inst. Nucl. Sci. Univ. Ghent. Proeftuinstr. 86 B-9000 Ghent Belgium). Chenery S. Cook J. Poitrasson F. Sampling and analysis on a micrometre scale by laser ablation microprobe ICP-MS. 1995 European Winter Conference on Plasma Spectrochemistry Cambridge UK January 8-13 1995 (Anal. Geochem. Group British Geol. Surv. Keyworth Nottingham UK NG12 5GG). Raith A. Hutton R. C. Godfrey J. Quantitative analysis of glasses and steel rubbings using laser ablation ICP-MS.1995 European Winter Conference on Plasma Spectrochemistry Cambridge UK January 8-1 3 1995 (Fisons Instruments Elemental Analysis Ion Path Road Three Winsford Cheshire UK CW7 3BX). Goodall P. Johnson S. Laser ablation and high resolution ICP spectrometry for the determination of lanthanides and selected actinides. 1995 European Winter Conference on Plasma Spectrochemistry Cambridge UK January 8-13 1995 (Argonne Natl. Lab. (West) Idaho Falls Idaho USA). 95/C2053 Masters B. Sharp B. L. Preliminary studies of excimer laser ablation ICP-MS and its application to biological materials. 1995 European Winter Conference on Plasma Spectrochemistry Cambridge UK January 8-13 1995 (Dept. Chem. Loughborough Univ.Technol. Loughborough Leics. UK LE11 3TU). 95/C2054 Longerich H. P. Gunther D. Forsythe L. Jackson S. E. Capabilities of a new ultra-high sensitivity inductively coupled plasma mass spectrometer (ICP-MS) with solution nebulization and laser ablation microprobe (LAM) sample introduction. 1995 European Winter Conference on Plasma Spectrochemistry Cambridge UK January 8-13 1995 (Dept. Earth Sci. and Centre for Earth Resour. Res. Memorial Univ. Newfoundland St. John’s Newfoundland Canada A1B 3x5). 95/C2055 Cohen A. S. Jarvis K. E. Williams J. G. Precision and accuracy of silicate rock trace element analysis by ICP quadrupole mass spectrometry. 1995 European Winter Conference on Plasma Spectrochemistry Cambridge UK January 8-13 1995 (Dept. Earth Sci. Univ. Cambridge Cambridge UK CB2 3EQ).95/C2056 Evans R. D. Outridge P. M. Laser ablation ICP-MS analysis of Arctic marine mammal teeth historical changes in trace metal concentrations. 1995 European Winter Conference on Plasma Spectrochemistry Cambridge UK January 8-13,1995 (Outridge Environ. Sci. Centre Trent Univ. Peterborough Ontario Canada K9J 7B8). 95/C2057 Hall G. S. Kennsley M. 100 year lead-isotope ratio chronology from US copper pennies. 1995 European Winter Conference on Plasma Spectrochemistry Cambridge UK January 8-13 1995 (Dept. Chem. Rutgers State Univ. New Jersey P.O. Box 939 Piscataway NJ 08856-0939 USA). 95/C2058 Brenner I. B. Zander A. Kim S. Holloway C. Multielement analysis of geological and related non- conducting materials using spark ablaton ICP-AES and a sequential spectrometer.1995 European Winter Conference on Plasma Spectrochemistry Cambridge UK January 8-13 1995 (Gonzton Res. Center Varian Assoc. Inc. 3075 Hansen Way Palo Alto CA 94304 USA). 95/C2059 Pereiro R. Lunzer F. Costa J. M. Bordel N Sanz- Medel A. Evaluation of the direct coupling of HPLC techniques to MIP-AES for trace metal speciation. 1995 European Winter Conference on Plasma Spectrochemistry Cambridge UK January 8-13 1995 (Dept. Phys. Anal. Chem. Fac. Chem. Univ. Oviedo 33006 Oviedo Spain ). 95/C2060 Berndt H. Muller A. Schaldach G. Yanez J. High-performance flow atomic spectrometry an integ- rated system for on-line sample pretreatment and high efficiency nebulization in atomic spectrometry. 1995 European Winter Conference on Plasma Spectrochemistry Cambridge UK January 8-13 1995 (Inst.Spektrochem. Angewandte. Spektrosk. Bunsen- Kirchhoff-Str. 1 1 D-44139 Dortmund Germany). 95/C2061 Cairns W. R. I. Ebdon L. Hill S. J. Versatile desolvation system for use with coupled HPLC- ICP-MS. 1995 European Winter Conference on Plasma Spectrochemistry Cambridge UK January 8-13 1995 (Dept. Environ. Sci. Univ. Plymouth Plymouth UK PL4 8AA). 95/C2062 Ketterer M. E. Waiwood M. Fiorentino M. Ohlson B. Measurement of electron self-exchange rate constants using isotope tracers separatons and inductively coupled plasma mass spectrometry. 1995 European Winter Conference on Plasma Spectrochemistry Cambridge UK January 8-13 1995 (Dept. Chem. John Carroll Univ. Univ. Heights OH 44118 USA). 95/C2063 Larsen E. H. Sepciation of arsenosugars in marine reference materials by HPLC-ICP-MS.1995 European Journal of Analytical Atomic Spectrometry July 1995 1/02. 10 189R95/C2064 9 5/C206 5 95/C2066 95/C2067 95/C2068 95/C2069 95/C2070 95/C207 1 95/C2072 95/C2073 95/C2074 95/c2075 Winter Conference on Plasma Spectrochemistry Cambridge UK January 8-13 1995 (Dept. Food Chem. Nutr. Natl. Food Agency Denmark 19 Marrkharj Bygade DK-2860 Sarborg Denmark). Potter D. Planitz P. Kawabata K. Sakuta S. Inoue Y. Speciation studies in ICP-MS. 1995 European Winter Conference on Plasma Spectrochemistry Cambridge UK January 8-13 1995 (Hewlett Packard Inc. USA). De Gendt S. Van Grieken R. E. Ohorodnik S. K. Harrison W. W. Factors affecting the response of nonconductors in rf glow discharge MS. 1995 European Winter Conference on Plasma Spectrochemistry Cambridge UK January 8-13 1995 (Dept.Chem. Univ. Antwerp Universiteitsplein 1 B-2610 Antwerp Belgium ). Crews H. M. Strutt P. Baxter M. J. Determination of selenium species by HPLC-ICP-MS. 1995 European Winter Conference on Plasma Spectrochemistry Cambridge UK January 8-13 1995 (Min. of Agric. Fisheries and Food CSL Food Sci. Lab. Norwich Res. Park Norwich UK NR4 7UQ). Bogaerts A. van Straaten M. Gijbels R. Mathematical modelling of a dc glow discharge. 1995 European Winter Conference on Plasma Spectrochemistry Cambridge UK January 8-13 1995 (Dept. Chem. Univ. Antwerp Universiteitsplein 1 B-2610 Wilrijk- Antwerpen Belgium). Winchester M. R. Salit M. L. Development of a glow discharge atomic emission instrument for macro-scale elemental composition mapping of solid surfaces.1995 European Winter Conference on Plasma Spectrochemistry Cambridge UK January 8- 13 1995 (Anal. Chem. Div. Chem. Sci. Technol. Lab. Natl. Inst. Stand. and Technol. Gaithersburg MD 20899 USA). Saprykin A. I. Becker J. S. Dietze H.-J. Investigation of sputtering and ionization of solids by a radio frequency glow discharge mass spectrometry. 1995 European Winter Conference on Plasma Spectrochemistry Cambridge UK January 8-13 1995 (Zentralabteilung Chem. Anal. Forschungszentrum Jiilich D-52425 Julich Germany). Steers E. B. M. Glow discharge sources-a comparison of various carrier gases. 1995 European Winter Conference on Plasma Spectrochemistry Cambridge UK January 8-13 1995 (SECEAP Univ. North London Holloway London UK N7 8DB). Bengtson A.Eklund A. Use of an Ar emission line as internal standard in quantitative depth profile analysis by GD-OES. 1995 European Winter Conference on Plasma Spectrochemistry Cambridge UK January 8-13 1995 (Swedish Inst. Metals Res. Dr. Kristinas vag 48 S-11428 Stockholm Sweden ). Barschick C. M. McLuckey S. A. McKown H. S. Smith D. H. Thermodynamic properties of glow discharge generated ions. 1995 European Winter Conference on Plasma Spectrochemistry Cambridge UK January 8-13 1995 (Chem. Anal. Sci. Div. Oak Ridge Natl. Lab. Oak Ridge TN 37831-6375 USA ). Allen L. A. Pang H.-M. Warren A. R. Houk R. S. Simultaneous measurement of ion ratios in solids by laser ablation with a twin quadrupole inductively coupled plasma mass spectrometer.1995 European Winter Conference on Plasma Spectrochemistry Cambridge UK January 8-13 1995 (Ames Lab.,-US Dept. Energy Dept. Chem. Iowa State Univ. Ames IA 50011 USA). Fak H. Wolf S. Novel plasma interface for ICP optical emission. 1995 European Winter Conference on Plasma Spectrochemistry Cambridge UK January 8-13 1995 (SPECTRO Anal. Instrum. GmbH Boschstr. 10 47533 Kleve Germany). Haraldsson C. LyvCn B. Determination of mercury isotope ratios in natural waters. 1995 European Winter 95/C2076 95/C2077 95/C2078 95/C2079 95/C2080 95/C208 1 95/C2082 95/C2083 95/C2084 95/C208 5 95/C2086 95/C2087 190 R Journal of Analytical Atomic Spectrometry July 1995 Vbl. 10 Conference on Plasma Spectrochemistry Cambridge UK January 8-13 1995 (Dept. Anal. Mar. Chem. Univ. Goteborg and Chalmers Univ.Technol. S-412 96 Goteborg Sweden). Moens L. Vanhaecke F. Riondato J. Dams R. Study of figures of merit and the effect of plasma parameters in magnetic sector ICP-MS. 1995 European Winter Conference on Plasma Spectrochemistry Cambridge UK January 8-13 1995 Gray A. L. Williams J. G. Liezers M. Noise sources in ICP-MS and their significance for isotope ratio precision. 1995 European Winter Conference on Plasma Spectrochemistry Cambridge UK January 8-13 1995 (4 Dene Lane Farnham Surrey UK GUlO 3PW). Taylor P. D. P. de Bihre P. Validation of the analytical linearity and of the mass discrimination correction model exhibited by a multiple collector ICP-MS by means of a set of synthetic uranium isotope mixtures (IRMM-072). 1995 European Winter Conference on Plasma Spectrochemistry Cambridge UK January 8-13 1995 (Inst.Ref. Mater. Measure. Comm. Eur. Commun. JRC Retieseweg B-2440 Geel Belgium). Paulsen P. J. Beary E. S. Obtaining accurate analyses using ICP-MS isotope dilution. 1995 European Winter Conference on Plasma Spectrochemistry Cambridge UK January 8-13 1995 (Natl. Inst. Stand. and Technol. Gaithersburg MD 20899 USA). Robb P. Owen L. M. W. Crews H. M. Stable isotope approach to radionuclide mobility studies. 1995 European Winter Conference on Plasma Spectro- chemistry Cambridge UK January 8-13 1995 (Min. Agric. Fisheries and Food CSL Food Sci. Lab. Norwich Res. Park Colney Norwich UK NR4 7UQ). Batho A. Woolley C. James D. Matrix effects in an axially viewed high performance ICP-OES. 1995 European Winter Conference on Plasma Spectrochemistry Cambridge UK January 8-13 1995 (Thermo Electron Ltd.Warrington Cheshire UK). Evans E. H. Fisher A. Woods M. Jerome S. Determination of the actinide elements in environmental samples by chelation preconcentration isotope dilution ICP-MS. 1995 European Winter Conference on Plasma Spectrochemistry Cambridge UK January 8-1 3 1995 (Dept. Environ. Sci. Univ. Plymouth Drake Circus Plymouth UK PL4 8AA). Sabsabi M. Cielo P. Quantitative elemental analysis of metallic alloys by laser induced breakdown spec- troscopy. 1995 European Winter Conference on Plasma Spectrochemistry Cambridge UK January 8-13 1995 (Ind. Mater. Inst. Natl. Res. Council Canada 75 Blvd. de Mortagne Quebec Canada J4B 6Y4). Luge S. Schalk A Zach H. Broekaert J.A. C. Comparison of a graphite furnace and a tungsten filament for sample introduction in a stabilized capaci- tive plasma (SCP) as source for atomic emission spectrometry. 1995 European Winter Conference on Plasma Spectrochemistry Cambridge UK January 8-13 1995 (Fachbereich Chem. Univ. Dortmund D-44221 Dortmund Germany). Becker J. S. Dietze H.-J. Cluster formation processes in laser and spark plasma of rare earth oxide/graphite mixtures. 1995 European Winter Conference on Plasma Spectrochemistry Cambridge UK January 8-13 1995 (Zentralabteilung Chem. Anal. Forschungszentrum Julich GmbH D-52425 Julich Germany). Ediger R. D. Plastic discrimination using laser-induced plasma spectroscopy. 1995 European Winter Conference on Plasma Spectrochemistry Cambridge UK January 8-13 1995 (Perkin-Elmer Corp.761 Main Ave. CT 06859-0215 USA). Watling R. J. Herbert H. K. Young W. A. Novel applications of LA-ICP-MS in the field of geochemical95/C2088 95/C2089 95/C2090 95/C2091 95/C2092 95/C2093 95/C2094 95/C2095 95/C2096 95/C2097 95/C2098 exploration. 1995 European Winter Conference on Plasma Spectrochemistry Cambridge UK January 8-13 1995 (Chem. Centre (WA) 125 Hay St. East Perth WA 6004 Australia). Ruppert H. Hansen B. Schneider A. Optimized devices improve sample preparation for trace and ultratrace analysis of liquid and solid materials. 1995 European Winter Conference on Plasma Spectrochemistry Cambridge UK January 8-13 1995 (Inst. Geol. and Dynamic of the Lithosphere Univ. Gottingen Goldschmidtstr. 3 D-37077 Gottingen Germany). De Silva N.Cathum S. J. Guevremont R. Signal measurement approaches for direct powder introduc- tion plasma spectrometry. 1995 European Winter Conference on Plasma Spectrochemistry Cambridge UK January 8-13 1995 (Miner. Resour. Div. Geol. Surv. Canada 601 Booth St. Ottawa Canada K1A OE8). Wiederin D. R. Gjerde D. T. Smith F. G. ICP-MS sample introduction for preconcentrated analytes. 1995 European Winter Conference on Plasma Spectrochemistry Cambridge UK January 8-13 1995 (CETAC Technol. 5600 S. 42nd St. Omaha NE 68107 USA). Naka H. Kurayasu H. Determination of trace impurit- ies in silicon carbide by ICP mass spectrometry. 1995 European Winter Conference on Plasma Spectrochemistry Cambridge UK January 8-13 1995 (Sumitomo Metal Ind. Ltd. 1-8 Fuso-cho Amagasaki 660 Japan).Hoffmann E. Ludke C. Element determination in airborne particulates by ETV-ICP-MS. 1995 European Winter Conference on Plasma Spectrochemistry Cambridge UK January 8-13 1995 (Inst. Spektrochem. Angew. Spektrosk. (ISAS) Lab. Spektrosk. Meth. Umweltanal. (LSMU) 12484 Berlin Germany). Nickel H. Electrothermal vaporization and in situ modification of ceramic powders for a direct ETV-ICP- OES analysis. 1995 European Winter Conference on Plasma Spectrochemistry Cambridge UK January 8-13 1995 (Forschungszentrum Julich GmbH Inst. Werkstoffe Energietech. 1 and Rheinisch Westfalische Tech. Hochsch. Aachen D-52425 Julich Germany ). Iavetz R. Louie H. Matousek J. P. Preconcentration of volatile element hydrides by trapping for deter- mination by electrothermal vaporization-ICP-MS. 1995 European Winter Conference on Plasma Spectrochemistry Cambridge UK January 8- 13 1995 (Australia Gov.Anal. Lab. Pymble NSW 2073 Australia). Magyar B. Cousin H. Relative stability of molecule ions in ICP. 1995 European Winter Conference on Plasma Spectrochemistry Cambridge UK January 8-13 1995 (Lab. Inorg. Chem. Swiss Fed. Inst. Technol. ETH-Zentrum 8092 Zurich Switzerland). Tanner S. D. Fundamentals of inductively coupled cold plasma mass spectrometry. 1995 European Winter Conference on Plasma Spectrochemistry Cambridge UK January 8-13 1995 (SCIEX 55 Glen Cameron Rd. Thornhill Ontario Canada L3T 1P2). Gaillat A. M. Barnes R. M. Influence of gas thermodynamic and transport properties on tempera- ture and flow fields in an enclosed inductively coupled plasma. 1995 European Winter Conference on Plasma Spectrochemistry Cambridge UK January 8-1 3 1995 (Dept.Chem. Univ. Massachusetts Lederle GRC Tower Box 34510 Amherst MA 01003-4510 USA). Ebdon L. Looking back to look ahead in plasma spectrochemistry. 1995 European Winter Conference on Plasma Spectrochemistry Cambridge UK January 8-13 1995 (Plymouth Anal. Chem. Res. Unit. Dept. Environ. Sci. Univ. Plymouth Drake Circus Plymouth UK PL4 8AA). 95/C2099 Olesik J. W. Dziewatkoski M. P. McGowan G. J. Thaxton C. Inductively coupled plasma-sample inter- actions from microscopic measurements of signals produced by single sample drops to impact on practical analysis. 1995 European Winter Conference on Plasma Spectrochemistry Cambridge UK January 8-13 1995 (Lab.Plasma Spectrochem. Laser Spectrosc. Mass Spectrom. Dept. Geol. Sci. Ohio State Univ. 1090 Carmack Rd. Columbus OH 43210 USA). 95/C2100 Kawabata K. Why polyatomic ions are reduced by the Shield Torch System in ICP-MS. 1995 European Winter Conference on Plasma Spectrochemistry Cambridge UK January 8-13 1995 (Yokogawa Anal. Systems Inc. 2-1 1-29 Naka-cho Musashino-shi Tokyo 180 Japan). 95/C2 101 Niemax K. Groll H. Schnurer-Patschan C. Zybin A. Spectrochemistry with diode lasers. 1995 European Winter Conference on Plasma Spectrochemistry Cambridge UK January 8-13 1995 (Inst. Phys. Univ. Hohenheim 70565 Stuttgart Germany). 95/C2102 Nesbitt R. W. Hirata T. Hartley J. H. D. UV laser probe ICP-MS and its application in the earth sciences. 1995 European Winter Conference on Plasma Spectrochemistry Cambridge UK January 8-13 1995 (Dept.Geol. Univ. Southampton Southampton UK SO17 1BJ). 95/C2103 Caruso J. Elemental speciation with plasma mass spectrometry detection challenges and opportunities. 1995 European Winter Conference on Plasma Spectrochemistry Cambridge UK January 8-13 1995 (Dept. Chem. Univ. Cincinnati Cincinnati OH 45221 USA). 95/C2104 Marcus R. K. Radio frequency powered glow dis- charges elemental analysis across the solids spectrum. 1995 European Winter Conference on Plasma Spectrochemistry Cambridge UK January 8-13 1995 (Dept. Chem. Howard L. Hunter Chem. Labs. Clemson Univ. Clemson SC 29634-1905 USA). 95/C2105 Kingston H. M. Sample preparation for ICP-MS and ICP-OES. 1995 European Winter Conference on Plasma Spectrochemistry Cambridge UK January 8-13 1995 (Dept.Chem. Biochem. Duquesne Univ. Pittsburgh PA 15282 USA). 95/C2106 Haswell S. J. From sample to instrument the missing link. 1995 European Winter Conference on Plasma Spectrochemistry Cambridge UK January 8-13 1995 (School Chem. Univ. Hull Hull UK HU6 7RX). 95/C2107 Blades M. W. Solvent and solvent loading effects in the inductively coupled argon plasma. 1995 European Winter Conference on Plasma Spectrochemistry Cambridge UK January 8-13 1995 (Dept. Chem. Univ. British Columbia Vancouver British Columbia Canada V6T 1Z1). Cai X.-J. Uden P. C. Sullivan J. J. Quimby B. D. Block E. Headspace-gas chromatography with atomic emission and mass selective detection for the determi- nation of organoselenium compounds in elephant garlic.Anal. Proc. (London) 1994 31 325. (Dept. Chem. Univ. Massachusetts Lederle Grad. Res. Tower A Massachusetts Amherst MA 01003-4510 USA). Das A. K. Cervera M. L. de la Guardia M. Rapid microwave-assisted amplification for the spectrophoto- metric determination of iodine. Anal. Proc. (London) 1994 31 345. (Dept. Anal. Chem. Fac. Chem. Univ. Valencia 50 Dr. Moliner St. E-46100 Burjassot (Valencia) Spain). Ashino T. Takada K. Hirokawa K. Determination of trace amounts of selenium and tellurium in high-purity iron by electrothermal atomic absorption spectrometry after reductive coprecipitation with palladium using ascorbic acid. Anal. Chim. Acta 1994 297 443. (Inst. 95/2108 95/2109 95/2110 Journal of Analvtical Atomic SDectrometrv Julv 1995 Vol. 10 191 R95/21 11 95/21 12 95/21 13 95/21 14 95/2115 95/21 16 95/21 17 9512118 9512119 9512120 9512121 192R Mater.Res. Tohoku Univ. Katahira 2-2-1 Sendai 980-77 Japan ). Chen H.-w. Xu S.-k. Fang Z.4. Determination of copper in water and rice samples by flame atomic abosorption spectrometry with flow-injection on-line adsorption preconcentration using a knotted reactor. Anal. Chim. Acta 1994 298 167. (Flow Injection Res. Centre Inst. Appl. Ecol. Acad. Sin. Shenyang 110015 China). Evans S. Meisel T. Low blank determination of boron in geochemical materials. Anal. Chim. Acta 1994 298 267. (Inst. Anorg. Anal. Phys. Chem. Univ. Bern 3000 Bern 9 Switzerland ). ValdCs-Hevia y Temprano M. C. Fernandez de la Campa M. R. Sanz-Medel A. Sensitive atomic absorp- tion determination of lead by ethylation with sodium tetraethylborate( 111).Quim. Anal. (Barcelona) 1994 13,67. (Dept. Phys. Anal. Chem. Univ. Oviedo cIJuli8n Claveria no. 8 33006-Oviedo Spain). Bermejo-Barrera P. Soto-Ferreiro R. M. Aboal- Somoza M. Bermejo-Barrera A. Comparative study between the use of zirconium coated graphite tubes and palladium-magnesium nitrate as a chemical modi- fier for tin determination in tap water by atomic absorption spectrometry with electrothermal atomiz- ation. Quim. Anal. (Barcelona) 1994 13 15. (Anal. Chem. Nutr. Bromatol. Dept. Fac. Chem. Univ. Santiago de Compostela 15706 Santiago de Compostela Spain). Anzano J. M. Martinez-Garbayo M. P. Belarra M. A. Castillo J. R. Solid sampling in graphite furnace atomic absorption spectrometry. Direct determination of iron in pasta food.Quim. Anal. (Barcelona) 1994 13 73. (Dept. Anal. Chem. Univ. Zaragoza E-50009 Zaragoza Spain). Vazquez M. S. GutiCrrez A. M. Gtimez M. M. Palacios M. A. In uitro study of selenium copper and zinc absorptible fractions and selenium speciation in mussels. Quim. Anal. (Barcelona) 1994 13 144. (Dipt. Quim. Anal. Fac. Quim. Univ. Complutense 28040 Madrid Spain ). JimCnez de Blas O. Vicente Gonzilez S. Munoz Garrido R. Martin Pascual A Shnchez Martin M. A. Speciation and determination of arsenic and its metabolites in urine by atomic absorption spectroscopy with hydride generation and other coupled techniques. Quim. Anal. (Barcelona) 1994 13 138. (Dept. Anal. Chem. Nutr. Food Sci. Fac. Chem. Univ. Salamanca Salamanca Spain). Smirnov Y.M. Extended classification of holmium spectral lines using data obtained in crossing beams. Spectrochim. Acta Part B 1994 49 469. (Moscow Power Eng. Inst. 14 Krasnokazarmennaya St. Moscow 11 1250 Russia ). Docekal B. Krivan V. Franek M. Separation of analyte and matrix for the direct analysis of high-purity molybdenum-based materials by electrothermal atomic spectrometry methods - I. Radiotracer investigation of thermal extraction of impurities in a graphite cup. Spectrochim. Acta Part B 1994 49 577. (Sect. Anal. Hochstreinigung Univ. Ulm D-89069 Ulm Germany). Lazik C. Marcus R. K. Effect of excitation frequency on source characteristics in radiofrequency glow dis- charge atomic emission spectrometry - I. 2-30 MHz. Spectrochim. Acta Part B 1994 49 649. (Dept. Chem. Howard L.Hunter Chem. Lab. Clemson Univ. Clemson SC 29634-1905 USA). Akman S. Doner G. Interference mechanisms of sodium chloride on zinc and cobalt in graphite furnace atomic absorption spectrometry using a dual cavity platform. Spectrochim. Acta Part B 1994 49 665. (Istanbul Tek. Univ. Fen-Edebiyat Fak. Kimya Bolumii 80626 Maslak Istanbul Turkey). 9512122 9512123 9512 124 9512125 9512126 9512127 9512128 9512129 9512130 95/21 3 1 9512132 95/21 33 Journal of Analytical Atomic Spectrometry July 1995 Vol. 10 Pollmann D. Pilger C. Hergenriider R. Leis F. Tschopel P. Broekaert J. A. C. Noise power spectra of inductively coupled plasma mass spectrometry using a cooled spray chamber. Spectrochim. Acta Part B 1994 49 683. (Inst. Spektrochem. Angew. Spektrosk. Postfach 10 13 52 D-44013 Dortmund Germany).Matveev 0. I. Omenetto N. On the possibility of direct evaluation of ionization rates induced by laser radiation in flames - I. Time-resolved ionization measurements. Spectrochim. Acta Part B 1994 49 691. (Comm. Eur. Commun. Joint Res. Centre Environ. Inst. 21020 Ispra (VA) Italy). Kawai J. Adachi H. Hayakawa S. Zhen S. Y. Kobayashi K. Gohshi Y. Maeda K. Kitajima Y. Depth selective X-ray absorption fine structure spec- trometry. Spectrochim. Acta Part B 1994 49 739. (Dept. Metall. Kyoto Univ. Sakyo-ku Kyoto 606 Japan). Karanassios V. Bateman K. P. Spiers G. A. Electrically heated wire-loop in-torch vaporization sample introduction system for inductively coupled plasma atomic emission spectrometry with photodiode array detection.Spectrochim. Acta Part B 1994 49 847. (Guelph-Waterloo Center for Grad. Work in Chem. Dept. Chem. Univ. Waterloo Waterloo Ontario Canada N2L 3G1). Karanassios V. Bateman K. P. Spiers G. A. Determination of mercury vapour in air using electri- cally heated gold-coated wire-loops in-torch vaporiz- ation sample introduction and inductively coupled plasma atomic emission spectrometry with photodiode array detection. Spectrochim. Acta Part B 1994 49 867. (Guelph-Waterloo Center for Grad. Work in Chem. Dept. Chem. Univ. Waterloo Waterloo Ontario Canada N2L 3G1). Kintor T. Radziuk B. Welz B. Electrothermal volatilization flame and graphite furnace atomic absorp- tion spectrometric investigations on the determination of calcium in gallium. Spectrochim. Acta Part B 1994 49 875.(Dept. Appl. Res. Bodenseewerk Perkin-Elmer GmbH D-88647 Uberlingen Germany). Torralba R. Bonilla M. PCrez-Arribas L. V. Palacios A. Ciimara C. Speciation and simultaneous determi- nation of arsenic(m) arsenic(v) monomethylarsonate and dimethylarsinate by atomic absorption using inverse least squares multivariate calibration. Spectrochim. Acta Part B 1994,49,893. (Dept. Ciencias Basicas E.U.I.T. de Obras Publ. Univ. PolitCcnica de Madrid Madrid Spain). Oishi K. Okumoto T. Iino T. Koga M. Shirasaki T. Furuta N. Elemental mass spectrometry using a nitrogen microwave-induced plasma as an ion source. Spectrochim. Acta Part B 1994 49 901. (Instrum. Div. Hitachi Ltd. 882 Ichige Katsuta Jbaraki 312 Japan ). Woo J.-C. Cho K. H. Tanaka T. Kawaguchi H. Emission study with a moderate power radiofrequency Grimm-type glow discharge source.Spectrochim. Acta Part B 1994 49 915. (KRISS (Korea Res. Inst. Stand Sci.) P.O. Box 3 Taeduck Science Town Taejon 305-606 South Korea). Grimm W. Hermann G. Determination of lead isotope distributions by means of a computer-controlled Zeeman scanning atomic absorption spectrometer (ZSAAS). Spectrochim. Acta Part B 1994 49 925. (Phys. Inst. Justus-Liebig-Univ. Geissen Heinrich- Buff-Ring 16 D-35392 Giessen Germany). Terashima S. Determination of mercury in one hundred and eighteen geochemical reference samples by cold vapour atomic absorption spectrometry. Geostand. Newsl. 1994 18 199. (Geol. Surv. Japan 1-1-3 Higashi Tsukuba Ibaraki 305 Japan). Aota N. Miyamoto Y. Kosanda S. Oura Y. Sakamoto K.Neutron activation analysis of fifteen GSJ igneous rock reference samples. Geostand. Newsl.,9512 134 9512135 9512136 9512137 9512 13 8 9512139 9512 140 9512 14 1 9512 142 9512 143 9512144 9 512 145 9512 146 1994 18 65. (Dept. Chem. Fac. Sci. Kanazawa Univ. Kakuma-machi Kanazawa 920-1 1 Japan). Zereini F. Skerstupp B. Urban H. 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Acta Part B 1994 49 947. (Res. Centre Eco-Environ. Sci. Acad. Sin. P.O. Box 2871 Beijing China ). Nonose N. S. Matsuda N. Fudagawa N. Kubota M. Some characteristics of polyatomic ion spectra in inductively coupled plasma mass spectrometry. Spectrochim. Acta Part B 1994 49 955. (Natl. Inst. Mater. and Chem. Res. 1-1 Higashi Tsukuba Ibaraki 305 Japan). Headrick K. L. Chakrabarti C. L. Bicheng A. Marchand B. Matrix interferences in the analysis of solution residues using a commercial cathodic sputter- ing atomizer for atomic absorption spectrometry. Spectrochim. Acta Part B 1994 49 975. (Ottawa- Carleton Chem. Inst. Dept. Chem. Carleton Univ. TN 37831-6378 USA ). Journal of Analytical Atomic Spectrometry July 1995 Vol.10 193R9512159 9512160 9512 16 1 9512 162 9512163 9512164 9512 165 9512166 9 512 167 9512 168 95/21 69 9512170 9512 17 1 194R 1125 Colonel By Dr. Ottawa Ontario Canada K1S 5B6). Karanassios V. Bateman K. P. Spiers G. A. 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Nickel and nickel alloy reference materials. Spectrochim. Acta Part B 1994 49 1039. (Dept. Geol Petrol. and Geochem. Univ. Likge B-4000 Tilman Liege 1 Belgium). Ursinyovi M. Palusovi O. Hladikovi V. Determination of cadmium lead and mercury in the total diet using atomic absorption spectrometry. Chem. Listy 1994 88 252.(Inst. Preventive and Clin. Med. Bratislava Limbova 14 Slovakia). Alvarez Prieto M. Cordeiro Naranjo C. Pina Luis G. Mora de la Cruz G. de la Fe Napoles C. Fleites Mestre P. Determination of selenium in blood and serum of patients with epidemical neuritis by ETAAS. Quim. Anal. (Barcelona) 1994 13 182. (Dept. Anal. Chem. Inst. Mater. and Reagents Univ. Havana Ciudad de La Habana Cuba). Nerin C. Pons B. Speciation of alkyllead in water sample. Quim. Anal. (Barcelona) 1994 13 196. (Dept. Quim. Anal. Centro Politec. Sup. Univ. Zaragoza M de Luna 3 50015 Zaragoza Spain). Dehghan K. Shi Z. Holbrook Woodrum T. Brewer S. Sacks R. Surface features of conductors eroded by sputtering in a magnetron glow discharge plasma. Appl. Spectrosc. 1994 48 553. (Dept. Chem.Eastern Michigan Univ. Ypsilanti MI 48197 USA). Park S.-N. Hahn J.-W. Rhee C. Effect of the slit function of the detection system and a fast-fitting algorithm on accuracy of CARS temperature. Appl. Spectrosc. 1994,48,737. (Div. Quantum Metrol. Korea Res. Inst. Stand. and Sci. P.O. Box 3 Taedok Science Town Taejon 305-606 South Korea). Niemczyk T. M. Thompson B. D. Angus J. E. Intensity enhancements in hollow cathode lamps due to the addition of nitrogen to the fill gas. Appl. Spectrosc. 1994 48 896. (Dept. Chem. Univ. New Mexico Albuquerque NM 87131 USA). Salit M. L. Collins J. B. Yates D. A. Heuristic and statistical algorithms for automated emission spectral background intensity estimations. Appl. Spectrosc. 1994,48,915. (Natl. Inst. Stand. Technol. Gaithersburg MD 20899 USA).Madrid Y. Borer M. W. Zhu C. Jin Q.-h. Hieftje G. M. 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Acta Part B 1994 49 745. (Dept. Chem. Indiana Univ. Bloomington IN 47405 USA).Gotz R. Elgersma J. W. Kraak J. C. Poppe H. Application of an electrospray interface as a new nubulizer for inductively coupled plasma atomic emis- sion spectrometry. Spectrochim. Acta Part B 1994 49 761. (Inst. Anal. Chem. Vienna Univ. Technol. Getreidemarkt 91151 1060 Vienna Austria). Tsai S.-J. J. Jan C.-C. Chang L.-L. Determination of lead and bismuth in nickel-base alloys by graphite furnace atomic absorption spectrometry using con- tinuum source background correction. Spectrochim. Acta Part B 1994 49 773. (Dept. Appl. Chem. Providence Univ. Taichung Hsien Taiwan 433 China ). de Andrade J. C. Bueno M. I. M. S. Continuous flow cold vapour procedure for mercury determination by atomic emission using the reverse flow injection approach. Spectrochim. Acta Part B 1994 49 787.(Inst. Quim. Univ. Estadual de Campinas CP 6154 13081-970 Campinas SP Brazil).9512185 9512186 9512187 9512188 9512189 9512 190 9512 1 9 1 9512 192 9512 193 9512194 9512 195 95/2 1 96 9512 197 Jacksier T. Barnes R. M. Analysis of electronic grade chlorine by sealed inductively coupled plasma atomic emission spectroscopy. Spectrochim. Acta Part B 1994 49,797. (Chicago Res. Centre Air Liquide Countryside IL 60525 USA). Zhang H. Hsiech C. Ishii I. Zeng Z. Montaser A. Revised fast flexible algorithms for determination of electron number densities in plasma discharges. Spectrochim. Acta Part B 1994 49 817. (Dept. Chem. George Washington Univ. Washington DC 20052 USA). van Veen E. H. Bosch S. de Loos-Vollebregt M. T. C. Kalman filter approach to inductively coupled plasma atomic emission spectrometry.Spectrochim. Acta Part B 1994 49 829. (Lab. Mater. Sci. Delft Univ. Technol. Rotterdamseweg 137 2628 AL Delft Netherlands). Weir D. G. Blades M. W. Response of the inductively coupled argon plasma to solvent plasma load spatially resolved maps of electron density obtained from the intensity of one argon line. Spectrochim. Acta Part B 1994 49 1231. (Dept. Chem. Univ. British Columbia Vancouver British Columbia Canada V6T lZl). Pollmann D. Leis F. Tolg G. Tschopel P. Broekaert J. A. C. Multielement trace determination in Al,OJ ceramic powders by inductively coupled plasma mass spectrometry with special reference to on-line trace preconcentration. Spectrochim. Acta Part B 1994 49 1251. (Inst. Spektrochem.Angew. Spektrosk. Postfach 10 13 52 D-44013 Dortmund Germany). Sesi N. N. MacKenzie A. Shanks K. E. Yang P. Hieftje G. M. Fundamental studies of mixed-gas inductively coupled plasmas. Spectrochim. Acta Part B 1994 49 1259. (Dept. Chem. Indiana Univ. Bloomington IN 47405 USA). Niu H.-s. Houk R. S. Langmuir probe measurements of the ion extraction process in inductively coupled plasma mass spectrometry-I. Spatially resolved deter- mination of electron density and electron temperature. Spectrochim. Acta Part B 1994 49 1283. (Ames Lab US Dept. Energy Dept. Chem. Iowa State Univ. Ames IA 50011 USA). Koirtyohann S. R. Precise determination of isotopic ratios for some biologically significant elements by inductively coupled plasma mass spectroscopy. Spectrochim. Acta Part B 1994,49 1305.(Dept. Chem. Univ. Missouri Columbia MO 6521 1 USA). Mermet J.-M. Quality of calibration in inductively coupled plasma atomic emission spectrometry. Spectrochim. Acta Part B 1994 49 1313. (Lab. Sci. Anal. (URA CNRS 435) Univ. Claude Bernard-Lyon 1 69622 Villeurbanne Cedex France). Nam S.-H. Masamba W. R. L. Montaser A. Helium inductively coupled plasma mass spectrometry studies of matrix effects and the determination of arsenic and selenium in urine. Spectrochim. Acta Part B 1994 49 1325. (Dept. Chem. George Washington Univ. Washington DC 20052 USA). Sturgeon R. E. Gregoire D. C. Electrothermal vaporiz- ation inductively coupled plasma mass spectrometric detection of As Sb Se Bi and Sn following preconcen- tration by in situ collection of their hydrides.Spectrochirn. Acta Part B 1994,49,1335. (Inst. Environ. Res. Technol. Natl. Res. Council of Canada Ottawa Ontario Canada K1A OR9). van Veen E. H. Bosch S. de Loos-Vollebregt M. T. C. Spectral interpretation and interference correction in inductively coupled plasma mass spectrometry. Spectrochim. Acta Part B 1994 49 1347. (Lab. Mater. Sci. At. Spectrom. Unit Delft Univ. Technol. Rotterdamseweg 137 2628 AL Delft Netherlands). AndrC N. Geersten C. Lacour J.-L. Mauchien P. Sjostrom S. UV laser ablation optical emission spec- 9512 19 8 9512199 9512200 9512201 9512202 9512203 9512204 9512205 9512206 9512207 9512208 9512209 trometry on aluminium alloys in air at atmospheric pressure. Spectrochim. Acta Part B 1994 49 1363. (CEAILSLA Bgt. 391 Centre d’Etudes de Saclay 91 191 Gif-sur-Yvette Cedex France). Falk H.Some theoretical considerations on the physical limitations of atomic beam time-of-flight mass spec- trometry. Spectrochim. Acta Part B 1994 49 1373. (SPECTRO Analytical Instruments GmbH Boschstr. 10 47533 Kleve Germany ). Marunkov A Chekalin N. Enger J. Axner 0. Detection of trace amounts of Ni by laser-induced fluorescence in graphite furnace with intensified charge coupled device. Spectrochim. Acta Part B 1994 49 1385. (V.I. Vernadsky Inst. Geochem. and Anal. Chem. Kosygin Str. 19 Moscow 117975 Russia). Chekalin N. Marunkov A Axner 0. Laser-induced fluorescence in graphite furnaces under low pressure conditions as a powerful technique for studies of atomization mechanisms investigation of Ag. Spectrochim.Acta Part B 1994 49 1411. (V.I. Vernadsky Inst. Geochem. and Anal. Chem. Kosygin Str. 19 Moscow Russia). Bolshov M. A. Rudnev S. N. Brust J. Analytical characterization of laser excited atomic fluorescence of bismuth. Spectrochim. Acta Part B 1994 49 1437. (Inst. Spectrosc. Russian Acad. Sci. 142092 Troizk Moscow Region Russia ). Bolshov M. A. Rudnev S. N. Candelone J.-P. Boutron C. F. Hong S. Ultratrace determination of Bi in Greenland snow by laser excited atomic fluores- cence spectrometry. Spectrochim. Acta Part B 1994 49 1445. (Inst. Spectrosc. Russian Acad. Sci. 142092 Troitzk Moscow Region Russia ). Anderle M. Lazzeri P. Moro L. Benetti P. Rossella M. Queirolo G. Investigation on laser ablation of InGaAs by means of resonance ionization and surfaces analysis spectrometries.Spectrochim. Acta Part B 1994 49 1453. (Centro Mater. Biofis. Med. Povo Trento It a1 y) . Groll H. Schnurer-Patschan Ch. Kuritsyn Yu. Niemax K. Wavelength modulation diode laser atomic absorption spectrometry in analytical flames. Spectrochim. Acta Part B 1994 49 1463. (Inst. Spektrochem. Angew. Spektrosk. Univ. Dortmund Bunsen-Kirchhoff-Str. 11 D-44139 Dortmund Germany). Berniolles S. Wu Z.-q. Tong W. G. Diode laser-based non-linear degenerate four-wave mixing analytical spec- trometry. Spectrochim. Acta Part B 1994 49 1473. (Dept. Chem. San Diego State Univ. San Diego CA 92182 USA). Wu Z.-q. Liu J.-y. Tong W. G. Sensitive absorbance measurement method based on laser multi-wave mixing. Spectrochim. Acta Part B 1994,49 1483. (Dept. Chem. San Diego State Univ.San Diego CA 92182 USA). Ljungberg P. Boudreau D. Axner 0. Full temporal density-matrix treatment of dual wavelength arbitrary bandwidth pulsed laser excitation of atoms with degenerate states in high collisional media. Spectrochim. Acta Part B 1994 49 1491. (Anal. Laser Spectrosc. Group Dept. Phys. Univ. Goteborg and Chalmers Univ. Technol. S-412 96 Goteborg Sweden). Matveev 0. I. Omenetto N. Anomalous spatial distribution of temporal and spectral behaviour within a pulsed dye laser beam. Spectrochim. Acta Part B 1994,49,1507. (Eur. Comm. Joint Res. Centre Environ. Inst. 21020 Ispra Italy). Omenetto N. Matveev 0. I. Time-resolved fluores- cence as a direct experimental approach to the study of excitation and ionization processes in different atom reservoirs.Spectrochim. Acta Part 3 1994 49 1519. (Eur. Comm. Joint Res. Centre Environ. Inst. 21020 Ispra Italy). Journal of Analytical Atomic Spectrometry July 1995 Vol. 10 195R9512210 9 5/22 1 1 9512212 9512213 95/22 14 9512215 951221 6 95/22 17 9512218 9512219 9512220 9512221 9512222 196R Turk G. C. Yu L.-j. Koirtyohann S. R. Laser- enhanced ionization spectroscopy of sodium atoms in an air-hydrogen flame with mass spectrometric detec- tion. Spectrochim. Acta Part B 1994 49 1537. (Chem. Sci. and Technol. Lab. Natl. Inst. Stand. Technol. Gaithersburg MD 20899 USA). Simeonsson J. B. Sausa R. C. Trace detection of ambient brominated compounds by laser-induced photofragmentation/fragment detection spectrometry. Spectrochim. Acta Part B 1994 49 1545. (US Army Res.Lab. AMSRL-WT-PC Aberdeen Proving Ground Whitaker T. Bekov G. Field ionization of alkali metal Rydberg states application as an ultraviolet radiation detector with absolute wavelength calibration. Spectrochim. Acta Part B 1994 49 1557. (Atomic Sciences Inc. 114 Ridgeway Center Oak Ridge TN 37830 USA ). Petrucci G. A Imbroisi D. Smith B. W. Winefordner J. D. Detection of OH in an atmospheric pressure flame via laser-enhanced ionization of indium. Spectrochim. Acta Part B 1994,49 1569. (Dept. Chem. Univ. Florida Gainesville FL 3261 1 USA). Hannaford P. Oscillator strength in atomic absorption spectroscopy. Spectrochim. Acta Part B 1994 49 1581. (CSIRO Div. Mater. Sci. and Technol. Private Bag 33 Rosebank MDC Clayton Victoria 3 169 Australia). Fonseca R. W. Pfefferkorn L.L. Holcombe J. A. Comparisons of selected methods for the determination of kinetic parameters from electrothermal atomic absorption data. Spectrochim. Acta Part B 1994 49 1595. (Dept. Chem. and Biochem. Univ. Texas at Austin Austin TX 78712 USA ). L’vov B. V. Polzik L. K. Borodin A. V. Fedorov P. N. Novichikhin A. V. Precision and detection limits in Zeeman graphite furnace atomic absorption spec- trometry. Spectrochirn. Acta Part B 1994 49 1609. (Dept. Anal. Chem. St. Petersburg Tech. Univ. St. Petersburg 195251 Russia). Voigtman E. Yuzefovsky A. I. Michel R. G. Stray light effects in Zeeman atomic absorption spectrometry. Spectrochim. Acta Part B 1994,49 1629. (Chem. Dept. LGRC Tower Univ. Massachusetts Box 34510 Amherst MA 01003-4510 USA). Yuzefovsky A. I.Su E. G. Michel R. G. Slavin W. McCaffrey J. T. Newton approximation method for linearization of calibration curves in Zeeman graphite furnace atomic absorption spectrometry. Spectrochim. Acta Part B 1994 49 1643. (Dept. Chem. Univ. Connecticut Storrs CT 06269 USA). Hermann G. Kling B. Koch B. Multi-element determi- nation with solid sampling by laser ablation using electrothermal atomization and continuum source coherent forward scattering spectrometry. Spectrochim. Acta Part B 1994 49 1657. (Phys. Inst. Justus-Leibig- Univ. Giessen Heinrich-Buff-Ring 16 35392 Giessen Germany). Zong Y. Y. Parsons P. J. Slavin W. Background overcorrection problems for lead in the presence of phosphate with various metals in Zeeman graphite furnace atomic absorption spectrometry.Spectrochim. Acta Part B 1994 49 1667. (Wadsworth Center New York State Dept. Health P.O. Box 509 Albany NY Epstein M. S. Turk G. C. Yu L. J. Spectral interference in the determination of arsenic in high- purity lead and lead-base alloys using electrothermal atomic absorption spectrometry and Zeeman-effect background correction. Spectrochim. Acta Part B 1994 49 1681. (Inorg. Anal. Res. Div. Chem. Sci. and Technol. Lab. Natl. Inst. Stand. Technol. Gaithersburg MD 20899 USA). van Dalen G. de Galan L. Direct determination of particulate elements in edible oils and fats using an MD 21005-50066 USA). 12201-0509 USA). Journal of Analvtical Atomic Svectrometrv. 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Fenxi Ceshi Xuebao 1995 14 68. (Dept. Chem. Hangzhou Univ. Hangzhou 3 10028 China). Yang X.-t. He H.-k. Theoretical method of calculation of the absorbance in ZAAS method of the constant and transverse magnetic field.Fenxi Ceshi Xuebao 1995 9512250 951225 1 9512252 9512253 9512254 9512255 9 512256 9 5/22 5 7 9512258 9512259 9512260 951226 1 9512262 9512263 9512264 14 24. (Inst. Rock and Miner. Anal. Min. Geol. and Miner. Resour. Beijing 100037 China). Ma Y.-x. Chen Z.-h. Chen M.4 He J. Determination of copper content in ore by atomic absorption spectrometry. Fenxi Yiqi 1995 1 62. (Res. Inst. of Kaiyuan Chem. Fertilizer Plant Kaiyuan 661000 China ). Chen Z.4 Jiang S.-g. Direct determination of ger- manium in blood by platform graphite furnace AAS. Fenxi Ceshi Xuebao 1995 14 60. (Millet Res. Inst. Hebei Acad. of Agric. and Forestry Hebei 050031 China ). Pian Z.-h. Liuwei D.-h. Wan T.-j. Shi S.-m. Gao T.-b. Chen D.-h. Study for determination of trace Cr Cd and Pb in the Chinese traditional medicine.Fenxi Shiyanshi 1995 14 63. (Natl. Inst. Control of Pharm. and Biol. Prod. Beijing 100050 China ). Wang A.-x. Wang F.4 Wang Z.-x. Determination of germanium by FIA-HG-GFAAS with the matrix modi- fier palladium and its mechanism. Fenxi Ceshi Xuebao 1995 14 72. (Center Instrum. Anal. Northeast Normal Univ. Changchun 130024 China ). Lindberg A. Magneto-optic spectroscopy on neon using laser-induced forward scattering. Appl. Spectrosc. 1994 48 1532. (Accelerator Lab. Dept. Phys. Univ. Helsinki P.O. Box 43 FIN-00014 Helsinki Finland). Sandford S. P. Thomas M. E. Ultrahigh-efficiency very narrow-passband tunable optical filter. Appl. Opt. 1994 33 8325. (NASA Langley Res. Center Hampton VI 23681 USA).Brown M. S. Jeffries J. B. Measurement of atomic concentrations in reacting flows through the use of stimulated gain or loss. Appl. Opt. 1995 34 1127. (Molecular Phys. Lab. 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Reichardt T. A. Klassen M. S. King G. B. Laurendeau N. M. Real-time acquisition of laser-induced fluores- cence decays. Appl. Opt. 1995 34 973. (Flame Diagn. Lab. Sch. Mech. Eng. Purdue Univ. West Lafayette Woyke T. Schiller C. Schmidt U. Schober T. Zoger M. 2 + Co as a new H storage and getter for Lyman-ci radiation sources. Appl. Opt. 1995 34 155. (Forschungszent. Jiilich D-52425 Julich Germany).Boukari H. Palik E. D. Gammon R. W. Closed-form expressions to fit data obtained with a multipass Fabry- Perot interferometer. Appl. Opt. 1995 34 69. (Inst. Phys. Sci. and Technol. Univ. Maryland College Park Maryland 20742 USA). Palik E. D. Boukari H. Gammon R. W. Line-shape studies for single- and triple-pass Fabry-Perot interfer- IN 47907-1288 USA). Journal of Analytical Atomic Spectrometry July 1995 Vol. 10 197 Rometer systems. Appl. Opt. 1995 34 58. (Phys. Sci. and Technol. Univ. Maryland College Park Maryland 20742 USA ). Nomizu T. Kaneco S. Tanak T. Ito D. Kawaguchi H. Vallee B. T. Determination of calcium content in individual biological cells by inductively coupled plasma atomic emission spectrometry. Anal. Chem. 1994 66 3000. (Dept. Mater. Sci. and Eng. Nagoya Univ.Nagoyua 464-01 Japan). 95/2266 Hasegawa H. Sohrin Y. Matsui M. Hojo M. Kawashima M. Speciation of arsenic in natural waters by solvent extraction and hydride generation atomic absorption spectrometry. Anal. Chem. 1994 66 3247. (Dept. Chem. Fac. Sci. Kochi Univ. Akebono-cho Kochi 780 Japan). 95/2267 Momplaisir G.-M. Lei T. Marshall W. D. Performance of a novel silica T-tube interface for the AAS detection of arsenic and selenium compounds in HPLC column eluate. Anal. Chem. 1994 66 3533. (Dept. Food Sci. and Agric. Chem. MacDonald Campus of McGill 21 11 1 Lakeshore Rd. Ste.-Anne- de-Bellevue Quebec Canada H9X 3V9). 95/C2268 Stuckenberg B. L. Eddy B. T. Rademeyer C. J. Chemical analysis of airborne particulate matter and the effect of particle size on results using X-ray fluorescence spectrometry.Analitika 94 Stellenbosch South Africa 8- 13 December 1994 (Mintek Private Bag X3015 Randburg 2125 South Africa). 95/C2269 Falk H. Elemental mass spectrometry - analytical capabilities and physical limitations. Analitika 94 Stellenbosch South Africa 8-13 December 1994 (Spectro Anal. Instrum. Boschstr. 10 D-47533 Kleve Germany). 95/2265 95/C2270 Julsing M. Watson A. E. Use of an ultrasonic nubulizer and sample preconcentration techniques for the analysis of water by inductively coupled plasma optical emission spectroscopy. Analitika 94 Stellenbosch South Africa 8-13 December 1994 (Spectro Anal. Instrum. S.A. (Pty) Ltd. South Africa). 95/C2271 Rademeyer C. J. Matrix modification in ETAAS by solid metal deposition. Analitika 94 Stellenbosch South Africa 8-13 December 1994 (Dept.Chem. Univ. Pretoria Pretoria 0002 South Africa). 95/C2272 Omenetto N. Use of lasers in atomic and molecular spectroscopy a critical appraisal of analytical potentials in different fields of application. Analitika 94 Stellenbosch South Africa 8-13 December 1994 (Comm. Eur. Commun. Joint Res. Centre Environ. Inst. 21020 Ispra (Varese) Italy). 95/C2273 Willis J. P. Techniques for elemental and ionic analysis of environmental samples-air particulates soils waters. Analitika 94 Stellenbosch South Africa 8-13 December 1994 (Dept. Geol. Sci. Univ. Cape Town Rondebosch 7700 South Africa). 95/C2274 Boon B. P. Microwave leaching of carbon and beach sand for chemical analysis. Analitika 94 Stellenbosch South Africa 8-13 December 1994 (Mintek Private Bag X3015 Randburg 2125 South Africa).95/C2275 Van Grieken R. De Bock L. Hoornaert S. Injuk J. Jambers W. Van Malderen H. Individual aerosol particle analysis new developments and environmental applications. Analitika 94 Stellenbosch South Africa 8-13 December 1994 (Dept. Chem. Univ. Antwerp ( U.I.A.) B-2610 Antwerp-Wilrijk Belgium ). 198 R Journal of Analytical Atomic Spectrometry July 1995 Vol. 10

ISSN:0267-9477    

DOI:10.1039/JA995100173R

出版商:RSC    

年代:1995

数据来源: RSC

摘要:

Liquid Sample Introduction Devices in Flow Injection Atomic Spectroscopy* Invited Lecture I Journal of I Analytical J. L. BURGUERA AND M. BURGUERA IVAIQUIM (Andean Institute for Chemical Research) Faculty of Sciences University of Los Andes P.O. Box 542 Mdrida 51 01-A Venezuela A general view concerning some of the advantages of using flow injection analysis manifolds as the interface between sample and/or reagents with different atomic spectroscopy techniques is presented. The development and current status of sample introduction devices in flow injection atomic spectroscopy is reviewed. The different time- and volume-based devices are presented with emphasis on their performance for reliability sample and reagent consumption degree of flexibility robustness and automation capabilities.Keywords Flow injection; automated analysis; sample introduction; atomic spectroscopy The determination of the concentration of a particular element in a sample irrespective of its chemical form is part of the broad analytical field of ‘elemental analysis’. For many years the procedures used in analytical chemistry were overwhelm- ingly dominated by reliance on the chemical reaction of the elements and the fields of gravimetric volumetric and electro- chemistry were widely used in this respect with very limited and primitive equipment. Usually the methods were time- consuming tedious and subject to numerous errors many of which could only be eliminated or corrected for by a high degree of skill and tender loving care on the part of the analyst to ensure precise and accurate results.’ More than any other technique in spectroscopy atomic spectroscopy (AS) has caught the imagination of analytical chemists during.recent years. The field of AS is actually not one technique but four AAS AES AFS,2 and XRF.3*4 These techniques provide some of the most sophisticated and elegant methods for the detection and determination of minor trace and ultra trace metals in clinical environmental agronomic and industrial samples. Among the spectroscopic techniques AAS ETAAS ICP-AES ICP-AFS and ICP-MS have found wide-spread acceptance as high-performance tools for elemen- tal analysis3 However ICP-MS is in some cases more valuable owing to its excellent sensitivity selectivity ability for isotope dilution and extended lineal dynamic range.’ Instruments for AS techniques have been developed with sophisticated computer programs which are able to perform highly reproducible procedures with a minimum of attention by the analyst.Atomic spectroscopy has the advantages of being specific sensitive widely applicable rapid and of wide- spread availability. Approximately 70 elements can be deter- mined directly and many more elements and compounds can be assayed by indirect procedures. Unfortunately sample composition often varies from one sample to the next which determines sample preparation and introduction. Ideally a sample introduction system for AS would transfer the sample reproducibly and efficiently to the atomization/excitation stage. The development of procedures for analytical AS dealing with solution solid and gaseous samples has been a long-term research theme;6 the major * Presented at the Third Rio Symposium on Atomic Spectrometry Caracas Venezuela November 6-12 1994.limitation being sample preparation which frequently requires the use of digestion chambers and reasonably large sample masses and reagent amounts. The batch methodology usually applied for AS evaluations is the most time-consuming step in the analysis procedure. An analysis of a sample can only be as good and less time consuming if the sample preparation is automated. Flow injection (FI)7 is a technique that has intro- duced total modernization of the sample handling steps that are automated to render a sample ready for introduction into the AS instrument without or with minimal intervention by the analyst.FI may be defined as the sequential insertion of discrete sample solutions into an unsegmented continuously flowing stream with subsequent detection of the analyte.8 The simplest flow analyser consists of a propelling unit which is used to impel forward the carrier stream; an injector or sample introduction device by means of which a well-defined volume of sample solution is injected or inter- calated into the carrier stream in a reproducible manner; a micro-reactor which consists of a piece of tubing or a mixing chamber where the sample zone disperses and reacts with the components of the carrier stream; and a dete~tor.~ The signal obtained in FI is transient in nature and analytical measure- ments on this signal can be based on different parameters such as peak height or area as in HPLC.Neither physical equilib- rium (flow homogenization) nor chemical equilibrium is neces- sarily attained at the instant of detection. FI offers several advantages in terms of considerable decrease in sample volume per measurement (normally using 10-50 pl) and reagent con- sumption high sample throughput (50-300 measurements per hour); reduced residence times (readout time about 3-40 s); shorter reaction times (3-60 s) easy switching from one analysis to another (manifolds are easily assembled and/or exchanged); reproducibility (usually < 2% RSD); reliability; low carryover; and a high degree of flexibility (it can be coupled with almost any detection system). Concerning the on-line coupling of an FI assembly to an atomic spectroscopic instrument FI systems can be regarded as an interface between samples and standards with the instru- ments providing useful analytical information about the quali- tative and quantitative composition of samples.The usefulness of integrating FI with AS was recognized very early in the development of FI Initial reports dealt with the use of the FI system as a mere alternative to manual introduc- tion of samples. In such systems the noise problems associated with the air bubbles in segmented sample insertion systems are eliminated the analyst can use sample volumes in the microlitre range per measurement and the sample flow rate is optimized to allow higher atomization rates in the nebulization process with a net increase in sample analysis throughput.However the main advantages of FI in resolving key steps when interfaced to atomic spectrometers are still under active research. These are the development of automated systems for the on-line chemical modification and manipulation of the analyte prior to its introduction into the spectrometer. This Journal of Analytical Atomic Spectrometry July 1995 VoZ. 10 473sample treatment may include minerali~ation,'~-~~ precipi- tation,19 preconcentration or analyte separation using ion- removal of interfering matrix c o m p o ~ n d s ~ ~ . ~ ~ liquid-liquid extraction,26-28 v ~ l a t i l i z a t i o n ~ ~ - ~ ~ etc. A necessary requirement when performing an analysis based on FI is by definition to insert reproducibly a well-defined zone of either sample or reagent into a carrier stream where the zone disperses in a controlled manner on its way toward and through the sensing system.Therefore a crucial and indispensable part of an FI analyser is the injector or sample introduction device. The present paper reviews selectively the different introduction devices used in FI-AS systems with emphasis on their performances in terms of reliability sample and reagent consumption degree of flexibility robustness and automation capabilities. FUNDAMENTAL ASPECTS OF A LIQUID SAMPLE INTRODUCTION SYSTEM Conceptually a sample introduction system (SIS) consists of a device interfaced with a detector by means of a liquid delivery unit which intercalates or injects sample and/or reagent plugs into the flow The entire SIS besides delivering discrete volumes of samples and/or reagents may also perform sampling cali- bration procedures and a series of sample/reagents treatment on-line.The different kinds of sample introduction devices can be divided into three ~ategories:~ (1) volume-based devices; (2) time-based devices; and (3) a combination thereof. In category ( 1 ) the insertion is based on the physical entrapment of a sample and/or reagent solution into a perfectly constant volu- metric cavity and its subsequent transfer in a reproducible manner into the non-segmented carrier stream. The inserted volume must be changeable at least in the range 20-200~1. The volume needed to fill the unit is inevitably larger than the inserted volume but it should not be significantly larger.These kind of devices have been utilized since the early stages of development of FI systems. In category (2) a certain volume of sample and/or reagent solution is drawn aspirated or displaced at a constant flow rate during a fixed period of time into a well-defined section of tubing from where the metered sections are introduced and mixed downstream into an FI system by a combination of hydrostatic and hydrodynamic forces. The sample/reagent volume needed to fill the system could be smaller than the volume of the respective tubing section and in theory the insertion of almost any volume is possible. However this volume may be limited by the electronic system and length of each suction tube section used. Sample introduction device (3) is more versatile and reduces dead volumes per analysis.Its robustness is actually a topic of intense research. VOLUME-BASED INTRODUCTION DEVICES In the early stages of development of FI systems an aqueous sample was introduced manually using a hypodermic syringe34 and a flap35 valve into a continuously moving unsegmented carrier stream of water or reagent solution; an injection principle which was also adapted to FI-AS36-38 and FI-ICP39 and FI-ICP-MS40,41 systems. The use of syringes7p36-38,42 h as gained some popularity because of the simplicity economy and rapid availability of the experimental setup; and the injection of the required volume of sample per measurement. There were however some severe limitations in their use (1) the volume of material injected depends on the position of the plunger which makes its use tedious; (2) the form of the injected plug depends on the speed with which the plunger is being depressed especially with liquids of different viscosity; (3) the rubber septum which is part of this kind of injector may not be compatible with all samples and carrier stream solutions resulting in a chemical attack of the septum's elasto- mer with possible chemical leaching; (4) after repeated injec- tions pieces of the septum eventually become detached and block the flow line; and ( 5 ) the introduction of the syringe needle causes a temporal flow change which leads to physical mixing of the adhered sample in the needle with the carrier stream interface.Rocks et al.43 described an inexpensive double three-way stopcock valve for sample introduction into the flowing stream of an FI-AAS system.It consisted of a borosilicate glass barrel fitted with a tapered PTFE key. The key has two right-angled bores which can be aligned each with three limbs as required. By choosing different lengths of sample loops the injected volume may be varied. As well the valve contains a bypass tube of higher hydrodynamic resistance so that the valve allows the carrier flow to continue when the valve loop is filled. This valve is difficult to adapt to different FI systems must be rotated manually and is also prone to leak or stick when exposed to a heavy work load. Because of their limitations as the scaling down of FI systems gained momentum these kind of injectors were quickly abandoned and today are of merely historical interest. The use of syringe based injectors were rapidly replaced by HPLC-type rotary valves.44 These valves have one or two external loops which can be replaced for changing the injected volume.Although it reproducibly intercalates a well defined zone of sample or reagent fluid into the carrier stream by switching the valve from a functional point of view the use of a syringe to fill the loop is tedious and too slow for practical assays and the risk of contamination of the sample from the metallic needle of most syringes is troublesome when assaying ultra trace elements. This led to inexpensive and ingenious designs of low-pressure rotary valve introduction devices of approximately the same volumetric scale as the commercially available HPLC v a 1 v e ~ .~ ~ ~ * ~ ~ ~ ~ Although the different rotary valve devices have been designed and mechanically manufac- tured differently the function of this type of valve is the intercalation of a fluid into the carrier stream. Their functional principle is based on the loading and intercalation positions. In the load position while the carrier stream flows through the valve in a bypass channel the sample fills the loop by aspiration with a syringe or a pump. When the valve is turned to the alternate position the sample plug is inserted into the carrier stream and therefore swept out of the volumetric cavity. Each rotary valve consists of three layers where a central moveable rotor is sandwiched between two stators. The rotor has two pairs of holes accommodating the sample and the internal bypass loop drilled to match two pairs of parts in the stator.Plexiglas clear PVC poly (vinylidene difluoride) (PVDF) and PTFE are the most used materials to construct these rotary valves; however in commercial valves the parts in contact with the solutions are made from inert fluorocarbons in order to avoid problems from corrosion. Numerous designs of home made and commercially available rotary valves have been tried often characterized by increasing levels of com- plexity. Two four six and eight-port valves have been con- s t r ~ c t e d ~ ~ ~ ~ ~ and used in different FI configurations which allows simultaneous sample/reagent introduction and split and nested sample loops to provide (1) a wide range of functions such as merging zones and zone sampling procedures (e.g.simple alternate sample introduction metering of separate volumes of sample and reagent triple zone introduction. and introduction of two adjacent zones); and (2) physical treatment or chemical modification of samples by ion-exchange precon- centration dialysis gas-diffusion digestion dilution filtration immobilized enzymes and chemical Up to now the majority of workers have favoured the use of the above described rotary valves probably because they are commercially available with variable degrees of automated control and can be readily used in combination with automatic 474 Journal of Analytical Atomic Spectrometry July 1995 Vol. 10samplers.52 However all systems employing rotary valves suffer from a common fault. Not only does the sample fill the volume of the sample loop but the entry and exit tubes must be filled with sample.Additional sample is used to flush out the residual of the previous specimen. Therefore the injection process is wasteful of sample requiring a sample consumption of at least twice the volume actually delivered to the AS instrument. This waste of sample volume becomes critical when most clinical samples are analysed. Loops may be bent or otherwise dam- aged giving erroneous results which necessitate immediate corrective action. Rotary valves are also prone to leakage when exposed to the heavy work load of a routine laboratory (usually between 5000 and 10000 measurements). Nevertheless the cost of most rotary valves is relatively low and replacement of worn-out parts of the injector can be easily made.Bergamin and C O - W O ~ ~ ~ ~ S ~ ~ - ~ ~ have initiated the double proportional sliding valve insertion commutator which is capable of performing merging-zone (or the insertion of several zones simultaneously which penetrate into each other down- stream7) and zone sampling procedures. This can be achieved in two different ways by intermittent pumpings6 or by the use of multiple inje~tion.'~ The simplest version of this kind of introduction device consists of two external plates with a moveable centre bar of metal polyethylene or Perplex held together by two spring-loaded screws. Holes are drilled through the commutator pieces in accordance with the flow diagram used. Silicone rubber sheets with holes are placed between the commutator plates to avoid leakage.For most applications the performance of these commutators seems to be comparable to those of rotary valves including the possibility of an easy automation of the sample introduction and on-line manipulation operations. With the hydrodynamic injection technique described by Ruzicka and Han~en,'~-'~ the introduced volume is well defined without the need of moving parts. The valve is replaced by two T junctions connected by a channel of known volume. This volume defines the sample volume to be introduced. The carrier stream is stopped and the sampling stream is simul- taneously turned on to fill the volume to be introduced. The sampling stream is then turned off and the carrier stream is turned on to complete the insertion cycle.Two peristaltic pumps are used to control the movement of sample and carrier solutions. Zagatto et ~ 1 . ~ ~ have described a hydrodynamic sample introduction procedure based on commutation which requires only one peristaltic pump operating continuously. Although the precision is good (usually RSD <1%) the inclusion of a commutator valve defeats one of the main purpose for which hydrodynamic sample introduction was developed i.e. to eliminate moving parts and concomitant wear. Despite its inherently favourable characteristics hydro- dynamic sample introduction has not been widely used in AS routine analyses probably owing to the difficulty in balancing hydrodynamic forces which causes a much worse precision (z 2.5%) than rotary valve introduction. TIME-BASED INTRODUCTION DEVICES Riley and co-workers60*61 have introduced the valveless time- based introduction method controlled dispersion analysis which consumes minimum amounts of sample and reagent.The probe transfer mechanism was a simple cam timer- operated device that raised and lowered an arm and rotated it through 90". The arm normally carried a sample probe and a reagent probe with provision for fitting an additional reagent probe if needed. In the simplest form of this system the peristaltic pump is driven by a stepping motor controlled by a microcomputer. The sample probe normally rests in a reagent container so reagent is pumped through the system between samples. When a sample is presented to the machine the pump is stopped and the probe is transferred to a sample container.The pump then rotates through a precise predetermined angle and again stops. The probe is returned to the reagent container and the pump restarted. The sample slug travels up the probe through the pump and onwards into the reactor tubing and finally to the detector no part of the sample being wasted. The introduction of air bubbles in this kind of sample introduc- tion device is not possible because the pump (driven by a stepping motor) is stopped while the probe is transferred either to the sample or reagent container. Notwithstanding the instrumental likeness to auto sample arms there are a number of essential differences between the two the most marked of which are the aspiration systems used by auto sampler arms withdraw the samples from the sampler vials and dispense them to the analyser cups or cuvettes; the time is not such a decisive factor; and high-precision syringes are the commonest option for measuring and transferring the liquid samples.Whereas in a valveless time-based device the sample and reagents are drawn by controlled movement of a peristaltic pump. The major drawback of this mode of sample introduc- tion is the momentaneous negative over-pressure created when the pump restarts which greatly deteriorates the reproducibility when used for AAS measurements. Jorgensen et a1.62 described a method to achieve a time- based introduction of sample using a two-position valve. The valve is opened to the sampling position for a precise time then is switched to the carrier position.The advantage cited for using a two-position valve is that the pump never stops thus the introduced volumes are more precise. The performance of this kind of system appears to be comparable to those of hydrodynamic sample introduction techniques and a valve. A different approach to sample introduction into a carrier stream with a time-based device and a simple timer circuit which can switch the current needed to activate a solenoid valve on and off at desired fixed intervals has been described by Burguera et ~ 1 . ~ ~ In this way the sample or carrier streams are either closed or opened,64 allowing the intercalation of variable and precise microlitre volumes of sample into the carrier stream with an average deviation of about 0.6%. While the carrier stream was propelled with a peristaltic pump the sample plug was introduced through a gas-pressurized reser- voir. With this sample introduction device calibration graphs can be constructed from a single solution65 and on-line dilution of samples is also possible.66 Further improvements such as the incorporation of a doubly stopping shutter (to close or to open any selected set of tubing at a fixed time) and an electronically controlled timer allow the performance of on-line programmed functions which may include sequential sample and reagent introduction merging zones zone trapping sample preconcentration and in uiuo sample uptake for measurements of metal species by AAS and ETAAS.16-'8,23,67-70 Gas diffusion units filters and ion-exchange micro-columns can be easily included to perform different on-line sample pretreatment procedures.Besides sample and reagents are not consumed during the stoppage of the sample zone the dead volume is reduced to a minimum value almost any desirable volume of sample and reagents can be readily inserted and the set-up is economical and easily adapted to a particular analytical application. VOLUME AND TIME-BASED DEVICES The hydrodynamic principle can be used to combine volu- metric sample metering with time-based insertion using two and three pumps which operate at different volumetric flow rates.7 All of these exploit the use of confluence points at which a well-defined sample zone is formed by means of the alternate motion of sample and carrier stream. This approach has not yet been adapted to systems where AS fulfils the role of the Journal of Analytical Atomic Spectrometry July 1995 Vol.10 475detector probably because the movement of the sample con- tainer has to be accurately sequenced with the operation of the pumps in order not to impair the performance of the system. This drawback could be eliminated in the future by electronically controlling the whole operation. Tyson et al. have described a variable tube dimension manifold.71 By switching the same injected volume by means of a rotary injection valve along tubes of different dimensions (length and internal) dispersion coefficients ranging from 6 to 40 in six discrete steps were obtained. The manifold has been applied to the determination of calcium chromium and nickel by FAAS. These kind of manifolds can be readily used to produce various calibrations of varying sensitivity by splitting the zone sample and confluence points at different dimen- s i o n ~ .~ ~ Although versatile the main limitations are (1) the number of connecting lines which at the same time make these kind of manifolds cumbersome; and (2) a decrease in peak height and peak area in proportion to the tubing length which greatly reduces the sensitivity of the analyses. A multipurpose flow insertion system composed of a combi- nation of a sliding insertion commutator with up to eight solenoid valves has been recently described by Reis et ~ 1 . ~ ~ The sample and standard solutions are introduced by discrete commutation in three or more modules each composed of two solenoid valves (three-way type).By sequentially coupling the different modules and electronically actioning the different valves the merging zones zone sampling intermittent flow sequential injections zone trapping and stopped flow functions can be performed. On-line programmed dilution and standard additions for simultaneous determinations of metal species on plant digests by ICP-AES were chosen to demonstrate some features of the system. CONCLUSIONS It is clear that FI focuses its attention on the weakest link of modern instrumentation which is the sample introduction and pretreatment processes. Although some inadequacies still exist FI improves the analytical performance of AS offering many unique advantages for the handling and on-line pretreatment of sample^.^^-^^ The recent development of improved sample and/or reagents introduction devices determines the trends of its essential features.Electronically controlled volume-based devices will increasingly continue to offer solutions to some of the sample preparation steps with low sample consumption per measurement for a number of years. However further research with fully automated time-based introduction devices will greatly simplify the different and common preparation steps necessary for converting matrices into an acceptable form for AS determinations with a simul- taneous decrease in sample and reagent consumption per analysis. REFERENCES 1 Robinson J. W. Atomic Spectroscopy M. Dekker New York 1990. 2 Burguera M. Burguera J. L. and Pacey G. E. in Flow Injection Atomic Spectroscopy ed.Burguera J. L. Marcel Dekker New York 1989 pp. 293-321. 3 Greenfield S. J. Anal. At. Spectrom. 1994 9 565. 4 Janssens L. Vincze L. Rubio J. Adams F. and Bernasconi G. J. Anal. At. Spectrom. 1994 9 151. 5 Sheppard B. S. and Caruso J. A. J. Anal. At. Spectrom. 1994 9 145. 6 Sneddon J. Sample Introduction in Atomic Spectroscopy Elsevier Amsterdam 1990. 7 Ruzicka J. and Hansen E. H. Flow Injection Analysis John Wiley New York 2nd edn. 1988. 8 Stewart K. K. General Introduction in Flow Injection Atomic 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 26 27 28 29 30 31 32 33 34 35 36 37 38 39 40 41 42 43 44 45 46 47 48 49 50 Spectroscopy ed. Burguera J. L. Marcel Dekker New York Valcarcel M. and Luque de Castro M. D. Flow Injection Analysis Principles and Applications Ellis Horwood Chichester 1987.Stewart K. K. Talanta 1981 28 789. Zagatto E. A. G. Krug F. J. Bergamin Fo. F. H. Jorgensen S. S. and Reis B. F. Anal. Chim. Acta 1979 104 279. Broekaert J. A. C. and Leis F. Anal. Chim. Acta 1979 109 73. Burguera M. Burguera J. L. and Alarcbn 0. M. Anal. Chim. Acta 1986 179 351. De la Guardia M. Salvador A. Burguera J. L. and Burguera M. J. Flow Injection Anal. 1988 5 121. Haswell S. J. and Barclay D. Analyst 1992 117 117. Burguera J. L. and Burguera M. J. Anal. At. Spectrom. 1993 8 235. Burguera M. Burguera J. L. Rondon C. Rivas C. Carrero P. and Brunetto M. R. J. Anal. At. Spectrom. 1995 10 343. Burguera M. and Burguera J. L. Lab. Robotics Autom. (LRA) 1993 5 277. Valcarcel M. Gallego M. and Martinez-JimCnez P. Anal. Proc. 1986 23 233.Valcarcel M. in Sample Zntroduction in Atomic Spectroscopy ed. Sneddon J. Elsevier Amsterdam 1990 pp. 289-327. Fang Z. and Welz B. J. Anal. At. Spectrom. 1989 4 543. Welz B. Sperling M. and Sun X. Fresenius’ J. Anal. Chem. 1993 346 550. Burguera J. Burguera M. Carrero P. Marcano J. Rivas C. and Brunetto M. R. J. Autom. Chem. 1995 in the press. Kamson 0. F. and Townshend A. Anal. Chim. Acta 1983 155 253. Burguera J. L. Burguera M. Rivas C. Gallignani M. Carrero P. and Brunetto M. R. presented at the Third Rio Symposium Caracas 1994. Valcarcel M. and Gallego M. in Flow Injection Atomic Spectroscopy ed. Burguera J. L. Marcel Dekker 1989 Memon M. A. Zhuang Z. X. and Fang Z. L. At. Spectrosc. 1993 14 50. Kuban V. Crit. Rev. Anal. Chem. 1991 22 477. Astrom O.Anal. Chem. 1982 54 190. Liversage R. R. Van Loon J. C. and de Andrade J. C. Anal. Chim. Acta 1984 161 275. Morita H. Kimoto T. and Shimomura S. Anal. Lett. 1983 16 1187. Burguera M. Burguera J. L. Brunetto M. R. De la Guardia M. and Salvador A. Anal. Chim. Acta 1991 261 105. Burguera M. and Burguera J. L. J. Anal. At. Spectrom. 1993 8 224. Ruzicka J. and Hansen E. H. Anal. Chim. Acta 1977 89 241. Ruzicka J. Hansen E. H. and Mosbaek H. Anal. Chim. Acta 1977 92 235. Rocks B. F. Sherwood R. A. and Riley C. Clin. Chem. 1982 28 440. Fukamachi K. and Ishibashi N. Anal. Chim. Acta 1980,119,383. Burguera J. L. Burguera M. and Gallignani M. An. Acad. Bral. Cienc. 1983 55 209. Jacintho A. O. Zagatto E. A. G. Bergamin F. H. Krug F. J. Reis B. F. Bruns R. E. and Kowalski B.R. Anal. Chim. Acta 1981 130 243. Bloxham M. J. Hilland S. J. H. and Worsfold P. I. J. Anal. At. Spectrom. 1994 9 935. Ebdon L. Fisher A. S. and Wrosfold P. I. J. Anal. At. Spectrom. 1994 9 611. Van Staden J. F. in Flow Injection Atomic Spectrocopy ed. Burguera J. L. Marcel Dekker New York 1989 pp. 49-101. Rocks B. F. Sherwood R. A. Turner Z. J. and Riley C. Ann. Clin. Biochem. 1983 20 72. Ruzicka J. and Hansen E. H. Flow Injection Analysis John Willey New York 1981 pp. 104-109. Karlberg B. and Pacey G. E. Flow Injection Analysis. A Practical Guide Elsevier Amsterdam 1989. Valcarcel M. and Luque de Castro M. D. in Andisis por Injeccidn en Flujo University of Cordoba Cordoba Spain 1984. Ruzicka J. Fresenius’ J. Anal. Chem. 1986 324 745. Martinez-Jimenez P. Gallego M.and Valcarcel M. Anal. Chem. 1987,59 69. Kuban V. Crit. Rev. Anal. Chem. 1992 23 15. Welz B. Sperling M. and Sun X. Fresenius’ J. Anal. Chem. 1993 346 550. 1989 pp. 1-17. pp. 157-224. 476 Journal of Analytical Atomic Spectrometry July 2995 Vol. 1051 52 53 54 55 56 57 58 59 60 61 62 63 64 65 Santelli R. E. Gallego M. and Valcarcel M. Talanta 1994 41 817. Van Staden J. F. and Van Rensburg A. Analyst 1990 115 605. Bergamin H. F. Zagatto E. A. G. Krug F. J. and Reis B. F. Anal. Chim. Acta 1978 101 17. Zagatto E. A. G. Krug F. J. Bergamin H. F. Jorgensen S. S. Reis B. F. Anal. Chim. Acta 1979 104 279. Zagatto E. A. G. Krug F. J. Bergamin H. F. and Jorgensen S . S. in Flow Injection Atomic Spectroscopy Marcel Dekker New York 1989 pp. 225-257. Ruzicka J. and Hansen E.H. Anal. Chim. Acta 1980 114 19. Ruzicka J. and Hansen E. H. Anal. Chim. Acta 1983 145 1. Clark G. D. Whitman D. A. Christian G. D. and Ruzicka J. Crit. Rev. Anal. Chem. 1990 21 357. Zagatto E. A. G. Bahia F. O. Gine M. F. and Bergamin H. F. Anal. Chim. Acta 1986 181 265. Riley C. Aslett L. H. Rocks R. Sherwood R. A. MacK Watson J. D. and Morgan J. Clin. Chem. 1983 29 332. Riley C. Rocks B. and Sherwood R. A. Talanta 1984 31 879. Jorgensen S. S. Petersen K. M. and Hansen L. A. Anal. Chim. Acta 1985 169 51. Burguera J. L. Burguera M. Rivas C. De la Guardia M. and Salvador A Anal. Chim. Acta 1990 234 253. Carrero P. Burguera J. L. Burguera M. and Rivas C. Talanta 1993 40 1967. Burguera J. L. Burguera M. Rivas C. De la Guardia M. Salvador A. and Carbonell V.J. Flow Injection Anal. 1990,7 11. 66 67 68 69 70 71 72 73 74 75 76 De la Guardia M. Morales-Rubio A. Carbonell V. Salvador A. Burguera J. L. and Burguera M. Fresenius’ J. Anal. Chem. 1993 345 579. Burguera J. L. Burguera M. Matousek de Abel de la Cruz A. Aiiez N. and Alarcon 0. M. At. Spectrosc. 1992 13 67. Burguera J. L. and Burguera M. Lab. Robotic Autom. (LRA) 1991 3 119. Burguera J. L. Burguera M. Carrero P. Rivas C. Gallignani M. and Brunetto M. R. Anal. Chim. Acta 1995 in the press. Burguera M. Burguera J. L. Rivas C. Carrero P. Brunetto M. R. and Gallignani M. Anal. Chim. Acta 1995 in the press. Tyson J. F. Anal. Chim. Acta 1986 179 131. Tyson J. F. in Advances in Atomic Spectroscopy ed. Sneddon J. JAI Press Greenwich CT 1992 vol. 1 pp. 161-228. dos Reis B. F. GinC M. F. Krug F. J. Bergamin H. F. J. Anal. At. Spectrom. 1992 7 865. McLeod C. M. J. Anal. At. Spectrom. 1987 2 549. Burguera J. L. and Burguera M. J. Trace Elem. Electrolytes Health Dis. 1993 7 9. Christian G. and Ruzicka J. Spectrochim. Acta Part B 1987 42 157. Paper 4/07094A Received November 21 1994 Accepted March 8 1995 Journal of Analytical Atomic Spectrometry July 1995 Vol. 10 477

ISSN:0267-9477    

DOI:10.1039/JA9951000473

出版商:RSC    

年代:1995

数据来源: RSC

摘要:

/ On-line Ion Exchange for the Removal of Sulfur Anion Interference on the Determination of Manganese in Geothermal Fluids by Flow Injection Electrothermal Atomic Absorption Spectrometry* Journal of Analytical Atomic Spectrometry J. L. BURGUERA M. BURGUERA C. RIVAS P . CARRERO M. GALLIGNANI AND M. R. BRUNETTO IVAIQUIM (Andean Institute for Chemical Research) Faculty of Sciences University of Los Andes P.O. Box 542 Mkrida 51 01-A Venezuela An efficient flow injection system with an on-line anion- exchange resin column (Dowex-1) incorporated into a time- based injector is described for the removal of sulfur anion spectral interference for the determination of manganese by electrothermal atomic absorption spectrometry. The positive interference effect caused by high concentrations of sulfur ions could not be reduced by using different matrix modifiers. However the elimination of this effect was possible by retaining the interferent species on the resin column and eluting the analyte with dilute nitric acid.The analyte plug was introduced into the graphite tube atomizer with a sampling arm assembly by means of positive displacement with air through a time-based solenoid valve. The entire system was controlled by a computer independent of the spectrometer. This approach to the elimination of sulfur anion interference has been applied to geothermal fluids with a high content of these species. The linear range was from 0 to 15 pg 1-' and the detection limit was 0.2 pg 1- (4 pg) of manganese. The results were precise (2.8-3.2% RSD) and were in good agreement with those obtained by atomic absorption chelation- extraction differences between mean values were < 7%.Keywords Flow injection; electrothermal atomic absorption spectrometry; on-line ion exchange; manganese; geothermal juids; time-based injector Hot springs or thermal spring waters are surface waters that have penetrated deep into the Earth encountered magmatic heat and then quickly risen again to the surface through faults or other natural conduits.' Hot springs contain different min- erals and other species in varying proportions. Depending on the chemical composition most thermal spring waters may be used for hydrotherapeutic treatments and through established relationships the concentration of metals such as Na K Mg Fe Rb and Mn can be used for geothermometry.Spring temperatures and the abundance of major and trace elements generally follow a geographic distribution. Particularly manga- nese concentration in hot springs varies from the pg 1-1 to the mg 1-' range.'.' Therefore in the first case a sensitive technique such as electrothermal atomic absorption spec- trometry (ETAAS) is required for monitoring these species without preconcentration of the sample. In real samples however the analyte element may be subject to strong concen- tration-dependent cross-interferences from concomitant elements and the optimum power of detection and best accuracy may not be achieved in the presence of a complex m a t r i ~ . ~ Interferences in ETAAS may be minimized to a various * Presented at the Third Rio Symposium on Atomic Spectrometry Caracas Venezuela November 6-12 1994.extent by applying for example the stabilized temperature platform furnace (STPF) concept or ion-exchange removal of in terferen t species. Ion-exchange techniques have been used for precon- centration speciation or conversion and matrix-interferent removal prior to flame atomic absorption spectroscopy (FA AS) inductively coupled plasma atomic emission spec- trometry (ICP-AES) and ETAAS.4-6 The first papers on the application of flow injection (FI) column preconcentration to FAAS and ETAAS were introduced by Olsen et al.' and Fang et a[.* Particularly the application of ion exchangers for the elimination of interferent species was first limited to off-line procedure^.^.'^ However a more flexible alternative is the separation of the interferents from the matrix by its retention in on-line FI systems." In preliminary experiments we found that there were inter- ferences from different sulfur anions.This paper describes an FI-ETAAS system whereby the on-line removal of S anions from the sample solution by its retention on an anion-exchange resin column was the most practical procedure to avoid matrix interferences. The aim was to permit the simple and fast separation of the S anion interference avoiding the oxidation of the hydrogen sulfide in contact with atmospheric oxygen and therefore the analyte coprecipitation with sulfur. EXPERIMENTAL Instrumentation The FI-ETAAS system and set-up used are shown sche- matically in Fig. 1. The FI manifold had six electronically controlled solenoid valves and the operating principle of each valve was as previously described by Carrero et a1." Each valve could independently either close or open any selected set of tubing at a fixed time.PTFE tubing (0.8 mm i.d.) was used for all the connections except for that of the columns. A Perkin-Elmer Model 2100 atomic absorption spectrometer equipped with a manganese hollow-cathode lamp operated at 20 mA and a wavelength of 279.5 nm with a spectral bandpass of 0.2 nm was used. Deuterium-arc background correction was used for all measurements. Time-resolved absorbance signals were recorded on an Epson LX-810 printer and the integrated absorbance values computed by the atomic absorption spec- trometer were used for evaluating the results.The basic settings used for the graphite tube atomizer are given in Table 1. The argon gas flow was 300 ml min-l during the entire procedure except during atomization when it was stopped for 3 s. The micro-ion-exchange columns were made from either uniform diameter glass tubing or from plastic Eppendorf pipette tips (tip cut to provide an outlet of approximately Journal of Analytical Atomic Spectrometry July 1995 VoZ. 20 479SAMPLE Fig. 1 Manifold set-up indicating the sequence program for valve operation. The dashed lines carry relevant streams in the individual stages A rinsing B interferent loading C sample loading and D washing operations; SAA sampling arm assembly; S spectrometer; 1-6 A and B and L1 and L indicate electronically controlled solenoid valves opened and closed set of tubing and sample and eluent trapping coils respectively Table 1 manganese in geothermal fluids Graphite tube atomizer programme for the determination of Step ~ 1 2 3 4 5 Parameter Dry Pyrolysis Atomize Clean Cool TemperaturePC 200 1000 2600 2700 20 Ramp time/s 10 10 0 1 1 Hold time/s 30 30 3 2 2 Internal gas flow/ ml min-' 300 300 0 300 300 0.8 mm id).The columns were all filled with the resin slurry and tightly packed with the ion exchanger to give uniform packing without any air gaps. A thin layer of glass-wool was placed at each end of the column to retain the resin and its connections to the FI system were made as previously reported by Fang and Welz.13 PTFE tubes with appropriate bore diameters were slipped either inside (on the wider end) or outside (on the tip) of the column. Reagents and Solutions The resin used was Dowex-1 X8 (mesh size 100-200; technical grade) commercially available in C1- form (Heidelberg Germany).The ultra pure water used in this work was obtained by the purification of de-ionized and distilled water (18 MQ cm) with a Millipore water-purification system. All reagents were of analytical-reagent grade except were indicated otherwise. Hydrochloric and nitric acids were of suprapur grade from E. Merck (Darmstadt Germany). A stock solution of manganese was prepared which con- tained 1 g 1-' Mn as MnC1 in 0.001 moll-' HC1; the working standards were prepared daily by appropriate dilution of the stock solution with water. For interference studies stock manganese solutions were prepared in anhydrous sodium sulfate or sodium sulfide nanohydrate solutions.As volatile H2S is the predominant form of sulfide in aqueous solutions below pH 7 the Na,S.9H20 was dissolved at pH 8.0 in sodium hydroxide-triethanolamine (TEA) solution. Geothermal waters were collected in two 11 polyethylene sample bottles which contained 20 ml of 1 mol 1-' TEA solution. The two bottles of the apparatus for collecting air- free water samples from hot springs had 20 cm lengths of wide- bore butyl rubber tubing over their necks and a screw clip placed halfway up the tube. Rubber stoppers fitted with PTFE tubing were placed in the ends of the wide-bore tubing. The shorter tube was under the surface and the long tube was exposed. Both bottles were filled with one bottle being purged with an extra 500 ml of water.The water in the purged bottle was allowed to cool in the absence of air. Extreme care regarding cleanliness of the sample collection equipment was taken thus it was thoroughly acid washed and rinsed before use. Collecting samples as previously described the constitu- ents of geothermal waters were not affected by exposure to air and sulfide oxidation and precipitation as sulfur or sulfates after exposition of samples to an aerobic environment was avoided. The addition of TEA is needed to mask the manga- nese@) and therefore to keep it in s01ution.l~ All glass and sampling flasks were rinsed with aqua regia and sequentially washed with water dilute HCl(l0 mmol 1-I) and copious quantities of purified water.Procedure The sequence function and duration of the FI-ETAAS mani- fold is described below. The carrier eluent and rinsing solutions (Fig. 1) were of water 0.002 mol 1-' HN03 and 1.5 mol I-' HN03 respectively. The purged bottle with sample was directly connected to the FI system. In sequence 1 (rinsing operation see Fig. 1A) the resin was converted into the NO3- form by drawing the rinsing solution through the resin column. The rinsing and eluent solutions were drawn to waste through the vacuum system the sample solution was stopped and the carrier solution was pumped to waste through the sampling arm assembly. The duration of this sequence was 30 s. In sequence 2 (interferent loading operation see Fig. lB) the activation of the solenoid valves 2 and 3 during an electronically defined sampling time allowed the sample solu- tion to be drawn through the resin column; in this way the 480 Journal of Analytical Atomic Spectrometry July 1995 Vol.10interferents were retained. The eluent and carrier solutions flowed as indicated in sequence 1 while the rinsing solution was stopped. The duration of this sequence was 60 s. In sequence 3 (sample loading operation Fig. lC) the activation of the solenoid valves 4 and 5 allowed the diversion of the carrier solution to carry the analyte solution trapped in the sample trapping coil to fill the tubing of the sample arm assembly. The eluent and the sample solutions were stopped as indicated in sequence 1 whereas the rinsing solution was stopped as indicated in sequence 2. The duration of this sequence was 50s.In sequence 4 (measurement operation) the sequential acti- vation of the solenoid valve 6 and the programming of the SAA unit allowed the deposition of 20pl aliquots of sample into the graphite tube atomizer synchronizing with the spec- trometer computer to run the atomizer temperature pro- gramme (Table 1). The duration of this sequence was 100 s per measurement. In sequence 5 (washing operation Fig. lD) the solenoid valve 1 was activated to divert the carrier solution through L2 and the column in order to elute the retained interferents. The rinsing and sample solutions were stopped as indicated in sequence 3. The duration of this sequence was 40 s. RESULTS AND DISCUSSION Preliminary Experiments In preliminary experiments we found that there were some positive interferences from the matrix.Interference from sulfur ions was evaluated by analysing standard solutions containing 1 g I-' Mn after addition of sulfide and sulfate anions separ- ately. The results obtained for 1000-5OOOOpg 1-l of both sulfur anions are shown in Table2. It should be mentioned here that the addition of such high amounts of interferent is not unrealistic. Such conditions are encountered in the geother- mal waters under study where the sulfide and sulfate concen- trations are 6.7 and 277.0mg 1-' re~pective1y.l~ Since the precision of the FI-ETAAS procedure is about 4-7% observed interferences of less than 5% were considered to be insignifi- cant. Thus the interference due to both sulfur ions were negligible when the sulfur content was below 1000 pg 1-'.However positive interferences occurred when the sulfur con- tent exceeded 5000 pg 1-'. The interference of sulfate was larger than that of sulfide. These results have shown that to obtain an accurate idea about the extent of the interferences in real matrices it is necessary to study a large range of interferent concentration because narrow ranges as published by some authors,I6 may possibly lead to wrong or at least incomplete conclusions. This interferent effect could not be diminished by matrix modification utilizing such additives as Table 2 Positive interferent effect of sulfur anions (as sulfate and sulfide) on the absorbance signal of Mn (1 pg 1-' of Mn) Ion Concentration/pg I-' x 1000 Sulfate 1 5 10 20 30 40 50 1 5 10 20 30 40 50 Sulfide Effect (YO) 4 20 28 35 38 40 42 1 6 11 18 22 24 26 palladium ( 5 pg) magnesium nitrite (50 pg) and ascorbic acid (0.5% m/v).A 20pl aliquot of the modifier solution was manually added on top of the sample in the tube atomizer. The observed interference is mainly due to a structured back- ground caused by both sulfur anions in the environment of the Mn resonance line. These results closely resemble those previously observed by Welz et al.I7 Although a more detailed investigation of this effect is needed it is out of the scope of the present investigation. Optimization of the Resin Column Characteristics In preliminary experiments without the resin column the coefficient of dispersion was 2.5 indicating that the FI system used was of low dispersion as required for a simple transport system.The effect of the length of the exchange column on absorbance of manganese was studied by using 0.5 1 2 and 3 cm conical shaped and uniform diameter ( x 2.5 mm id of glass) columns with and without sulfur ion species. Regardless of the column type D increased with the length of the resin column up to 4. However with a column of 0.5 cm the manganese response in the presence of sulfur ions increased. This effect could be due to the fact that the amount of resin in the column (about 25 mg) was insufficient to retain the adsorbable material present in the sample. When 1,2 and 3 cm long resin columns were employed the adsorption of sulfur ions was efficient but longer columns changed the effectiveness of sample suction and delayed the elution of interferents. In these cases longer aspiration times were needed which decreased the sampling rate.The performance of conical shaped columns was similar to that observed with uniform diameter glass columns; however if the interferent elution step is per- formed in the counter direction of the loading step the elution time is at least twice in the least ones. Therefore a conical shaped micro-column of 1 cm long was found to offer a good compromise between sample dispersion effectivity in the reten- tion of interferents and sampling throughput. Optimization of Hydrodynamic and Chemical Conditions Other factors affecting the performance of the columns were the interferent loading rate eluent volume and concentration. In the adsorption experiments a slow sample flow rate (from 1 to 3 ml min-') is preferred but it is time-consuming.As the sample flow rate was increased above 6ml min-' the signal slightly increased because of insufficient time for interferent adsorption. This effect was more pronounced (increases in the analytical signal from 12 to 18%) as the resin column length was shortened. With a flow rate of 4ml min-' the sulfur anions effect was completely suppressed by using a 1 cm long column. The use of eluent volumes below 1.5ml proved to be insufficient to displace sulfur ions from the column. To test this the absorbance of the manganese signals from sequential measurements were evaluated. Irreproducible results were obtained when eluent volumes below 2.0ml were used. Therefore to achieve complete elution of interferents the eluent volume should exceed 2.2 ml.As already mentioned dilute nitric acid was used as the eluent for the interferents. The concentration of nitric acid (0.002 mol I-') is a compromise between the elution time and the degree of performance of the anion-exchange resin and the degree of its preference for certain anionic species. A decrease in nitric acid concentration caused a delay in elution which is nearly constant when the eluent concentration lies in the range 0.001-0.004 mol 1-'. Lower concentrations of the eluent were preferred in view of a favorable competition between NO,- and all other adsorbable species for the active sites on the resin.18 Journal of Analytical Atomic Spectrometry July 1995 Vol. 10 481Table 3 Optimum hydrodynamic and chemical conditions Component Parameter Value Hydrodynamic Interferent loading rate 1.0 ml min-' 2.5 ml min-' Chemical Eluent (HNO,) 0.002 moll - ' Resin column Length 1 cm Conical shaped column Amount of resin 50 mg Eluent volume 1.5 ml Carrier flow rate concentration Table 4 Assay precision Mean [Mn]/pg I-' Within-run (n = 10) 5.2 2.5 5.3 Day-to-day (n = 6 ) RSD (Yo) 2.8 3.2 3.2 Table 5 Comparison of results obtained for manganese in geothermal fluids by the proposed method and by liquid-liquid extraction ETAAS; n=5 Sample This method Liquid-liquid extraction 1 2.5 & 0.0 2.7 f 0.3 2 5.9 & 0.1 6.6 & 0.8 3 12.0 f 0.2 11.6 & 1.5 4 8.0 f 0.2 7.8 f 1.2 The peristaltic pump was adjusted to give a delivery rate of 1 ml min-' for the carrier solution which displaces the sample zone contained in the sample trapping coil to fill the sampling arm assembly (Fig.1). This pumping rate had only a minor influence on the integrated absorbance signal. The best sensi- tivities were obtained for flow rates below 2.5 ml min-' which systematically dropped for higher flow rates. A low flow rate was also preferred because the time taken to fill the sampling arm assembly was more manageable. The tubing length of each component of the FI system had no detrimental effect on the overall performance except for the tubing from the exchange column to the sampling arm assembly (Fig. 1). This tubing length was kept as short as possible (2m long) to minimize the sample plug dispersion but to have the capacity to fill the desired volume of the sub- sample contained in the sampling arm assembly.According to the results previously described the FI con- ditions listed in Table 3 were chosen as optimal and therefore were used for all subsequent measurements. The linearity of the response to the AAS detector was investigated by injecting various amounts of the analyte. The results showed that the regression equation obtained by injecting 20pl volumes of aqueous standards using the FI system experimental conditions (Table 2) and the tube atomizer temperature programme (Table 1) was absorbance = 0.0163 [Mn] +0.003 r =0.9995 for the range 0-15 pg 1-' of manga- nese. A detection limit of 0.3 pg 1-' (6 pg) of Mn was obtained by taking three times the standard deviation of the integrated absorbance measurements.The characteristic mass m was 5.3 pg Mn per 0.0044 s. Within-run precision was assessed by using 10 replicates with two different concentrations of Mn in geothermal fluids. Day-to-day precision was estimated over 6 d. The results obtained in these precision studies are given in Table 4. Recovery studies were performed on four samples of geother- mal fluid. There was no loss of metal during the procedure and the average recovery for four additions of manganese was 98 +4% (range 95-104%). The accuracy of the procedure was further investigated by determining the manganese content in various geothermal fluids by the proposed procedure and by liquid-liquid extraction with APDC and quinolin-8-01 follow- ing its determination by ETAAS.19 The results are summarized in Table 5.Although good agreement is obtained for all samples by using both procedures obviously the liquid-liquid extraction approach is less suitable as it is cumbersome and has a larger standard deviation of the results. The main advantage of the method described here is that the accurate and precise determination of manganese in geo- thermal fluids with high content of sulfur anions is rapidly performed in a totally closed system with a minimum of sample manipulation and operator attention. This study was supported by the Consejo de Desarrollo Cientifico Humanistic0 y Tecnolbgico (CDCHT) of the Andes University MCrida Venezuela. REFERENCES 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 Ellis E. J. and Mahon W. A. J. Chemistry and Geothermal Systems Academic Press New York 1977.Ellis E. J. Chem. Geol. 1979 25 219. Sperling M. Yin X. and Welz B. J. Anal. At. Spectrom. 1991 6 295. Ruzicka J. Fresenius' 2. Anal. Chem. 1986 324 745. Nord L. and Karlberg B. Anal. Chim. Acta 1983 145 151. Pereiro Garcia M. R. Diaz Garcia M. E. and Sanz Medel A. J. Anal. At. Spectrom. 1987 2 699. Olsen R. Pessenda S. L. C. R. Ruzicka J. and Hansen E. H. Analyst 1993 108 905. Fang Z. Sperling M. and Welz B. J. Anal. At. Spectrom. 1990 5 639. Goosens J. and Dams R. J. Anal. At. Spectrom. 1992 7 1167. Brajter K. and Olbrych-Sleszynska E. Analyst 1986 111 1023. Kamson 0. F. and Townshend A. Anal. Chim. Acta 1983 155 253. Carrero P. Burguera J. L. Burguera M. and Rivas C. Talanta 1993,40 1967. Fang Z. and Welz B. J. Anal. At. Spectrom. 1989 4 543. Holzbecher Z. Divis L. Kral M. Sucha L. and Vlacil F. Handbook of Organic Reagents in Inorganic Analysis Ellis Horwood Chichester 1976. Burguera J. L. Aguas Termales en el Estado Mgrida Fac. de Ciencias Forestales Universidad de Los Andes MCrida Venezuela 1983 pp. 10-15. Kitagishi K. and Obata H. Report of the Environmental Science Mie Univ. 1985 10 171. Welz B. Bozsai G. Sperling M. and Radziuk B. J. Anal. At. Spectrom. 1992 7 505. Ruzicka J. and Hansen E. H. Flow Injection Analysis John Wiley New York 2nd edn. 1988 p. 23. Boniforti R. Ferraroli R. Frigieri P. Heltai D. and Queiraza G. Anal. Chim. Acta 1984 162 33. Paper 4/07092& Received November 21 1994 Accepted April 13 1995 482 Journal of Analytical Atomic Spectrometry July 1995 Vol. 10

ISSN:0267-9477    

DOI:10.1039/JA9951000479

出版商:RSC    

年代:1995

数据来源: RSC

摘要:

Fluoride as a Chemical Modifier for the Determination of Phosphorus by Electrothermal Atomic Absorption Spectrometry* JOSE ALVARADO AND ANA RITA CRISTIANO Universidad SimBn Bolivar Departamento de Quimica Apartado Postal 89000 Caracas 1080-A Venezuela ADILSON JOSE CURTIUS Departamento de Quimica Universidade Federal de Santa Catarina Florianbpolis S.C. Brazil The use of HF NaF KF CsF and NH4F as chemical modifiers for the determination of phosphorus by electrothermal atomic absorption spectrometry is described. All the fluorides studied were found to stabilize the phosphorus atomic absorption signals allowing for ashing temperatures higher than those with no modifier without losses of the analyte. The best results using these modifiers were obtained with NaF. However the sensitivity of the phosphorus signals was lower than when Pd was used as the modifier.The accuracy of the phosphorus determinations using the new NaF modifier was checked by analyses of NIST Standard Reference Materials (SRM 1570 Trace Elements in Spinach SRM 1571 Orchard Leaves SRM 1575 Pine Needles and SRM 1577a Bovine Liver) Keywords Electrothermal atomic absorption spectrometry; phosphorus determination; fluorides; chemical modijication The determination of phosphorus by electrothermal (graphite furnace) atomic absorption spectrometry (ETAAS) has at least three major drawbacks (1) The element's most sensitive absorption lines are at 167-168 and 177-179 nm. Use of these lines requires special instrumental considerations owing to the absorption of radi- ation by oxygen.' To overcome this limitation the direct atomic absorption determination of phosphorus can be performed using the non-resonant doublet which occurs at 213.55/213.62 nm.2 However measurements in this region are affected by an inherent low sensitivity.(2) Heating of phosphorus leads to the formation of volatile molecular species such as PO PO and P which leave the atomizer without dissociating at relatively low temperatures (approximately 300 OC).'.." If ashing cannot be carried out at higher temperatures matrix elimination by heating becomes a very difficult or impossible task and matrix interferences will be present. ( 3 ) The accuracy and precision of phosphorus determination are strongly dependent on the type of graphite and/or the physical conditions of the graphite tube atomizer used.'-' The above limitations can be suppressed or considerably reduced if the phosphorus determinations are performed under stabilized temperature platform furnace (STPF) conditions."." The accuracy and precision dependences on the atomizer are controlled by using new pyrolytic graphite-coated graphite tubes with pure pyrolityc graphite platforms.The sensitivity * Presented at the Third Rio Symposium on Atomic Spectrometry Caracas Venezuela November 6-12 1994. Journal of Analytical Atomic Spectrometry of the measurements is maximized by platform atomization and gas stop-flow conditions. Thermal stabilization of the analyte can be achieved by addition of a convenient chemical modifier to the phosphorus solution and standards. Chemical modifiers have been used to stabilize phosphorus thermally for its optimum ETAAS determinati~n.~*~,*.'~-'~ The most commonly used modifiers include lanthanum and pal- ladium. Unfortunately the use of lanthanum as a thermal stabilizer for phosphorus leads to analytical problems such as a strong memory effect and a reduced lifetime of the atomizer due to corrosion of the graphite,15 and palladium modifiers are expensive.This paper describes the use of fluorides as chemical modi- fiers for the determination of phosphorus by ETAAS. Among the modifiers tested NaF was found to be the best option. NaF is inexpensive free from memory effects does not corrode the graphite atomizer or platform and is comparable in its thermal stabilization effect to the more traditional modifiers palladium and lanthanum.EXPERIMENTAL Reagents and Standards Ammonium monophosphate (Merck analytical-reagent grade) sodium fluoride (Fisher ACS grade) ammonium fluoride (Riedel-de Haen ACS grade) caesium fluoride (Merck Selectipur grade) potassium fluoride ( Riedel-de Haen analytical-reagent grade) and 40% hydrofluoric acid (Merck analytical-reagent grade) were used to prepare working standard solutions. Nitric acid 65% (Riedel-de Haen DAB reagent grade) and hydrogen peroxide 35% (Riedel-de Haen chemically pure grade) were used for dissolution of NIST Standard Reference Materials. Distilled deionized water (18 Mil cm) was used throughout for sample preparation and dilution purposes. Instrumentation Atomic absorption measurements were performed using a Perkin-Elmer Model 2100 spectrometer equipped with a Perkin-Elmer Model HGA-700 electrothermal atomizer and a Perkin-Elmer AS-70 autosampler for sample injection.Pyrolytic graphite-coated graphite tubes and pure pyrolitic graphite platforms were used throughout. Sample digestion was achieved by means of a CEM Model MDS-2000 microwave oven using Teflon-capped vessels. Journal of Analytical Atomic Spectrometry July 1995 Vol 10 483Standards and Sample Preparation Phosphorus solutions A 5000 mgl-’ phosphorus solution was prepared by direct weighing of previously dried (NH4),HP04; nitric acid was added to give a final HN03 concentration of 0.2% v/v for stabilization purposes. Table 2 Instrumental conditions for determination of phosphorus by ETAAS. Wavelength 213.6 nm; slit 0.7 nm; lamp current 35 mA Fluoride solutions Solutions having different fluoride concentrations were pre- pared from the different fluoride compounds by direct weighing and convenient dilution with water.No acid was added to these solutions. Standard Reference Materials Standard Reference Materials from the National Institute of Standards and Technology (NIST) Trace Elements in Spinach (SRM 1570) Orchard Leaves (SRM 1571) Tomato Leaves (SRM 1573) Pine Needles (SRM 1575) and Bovine Liver (SRM 1577a) previously dried following the manufacturer’s instructions,16-20 were acid-digested by means of microwave heating. The microwave heating programme presented in Table 1 was based on the recommendations of Miller.,’ Approximately 0.3 g of each dried sample accurately weighed was placed inside the corresponding Teflon vessel and 0.5 ml of concentrated nitric acid plus 2ml of 35% H20 solution were added.The vessel was left open in a fume cupboard until the initially vigorous reaction had subsided (approximately 10min). Experience showed that this step was necessary to facilitate control of the pressure exerted by the gases produced during digestion on the walls and cap of the Teflon vessel. Evolution of gaseous species during the microwave heating of the SRM and the digestion mixture is evidenced by the shorter time needed to reach the pre-set pressure in the second step of the heating programme. Each vessel was then placed in the microwave oven and heated under the instrumental conditions described in Table 1.After completion of the heating cycle the vessels were allowed to cool to room temperature and vented; then each solution was transferred quantitatively into a 25 ml calibrated flask and diluted to volume with water. Five inde- pendent samples of each certified reference material were prepared in this fashion. Blanks were prepared in a similar manner. Procedure Optimum amount of modijier Graphs of absorbance versus amount of modifier were con- structed for injections of 10 pl volumes of 100 pg ml-’ phos- phorus solution in the presence of increasing amounts of the modifiers. In this manner the optimum amount of each modifier the amount which produced the maximum stabiliz- ation effect on phosphorus i.e. the maximum ashing tempera- ture allowed with no losses of the analyte could be selected.Each test was carried out at the ashing temperature at which the stabilizing effect of each fluoride used was clearly present. Table 1 Reference Materials Microwave heating programm for Dissolution of Standard Pressure/ Time*/ T.A.P.t/ Step lb inp2 Power/W min min 1 80 415 8 4 2 150 415 4 4 * Time needed to reach the pre-set pressure. t Time at pressure time for which the pre-set pressure is held. Step 1 2 3 4* 5 6 7* Temperature/ “C 90 120 300- 1350 50 2650 2600 20 Time/s Ramp 5 10 5 5 0 1 1 Hold 10 10 20 to 5 3 8 Gas flow/ ml min-’ 300 300 300 300 0 300 300 * Additional cooling steps according to Curtius et aL8 The instrumental conditions for these tests given in Table2 are those included in the default conditions in the spectrometer software except for the inclusion of two cooling steps as proposed by Curtius et a1.* The first cooling step was included between the ashing and atomizing steps and the second after the cleaning step (see Table 2).Cooling the atomizer after the ashing step maximizes the so-called ‘platform effect’ resulting in increased absorbance signals for phosphorus compared with the signals obtained with no cooling step. Inclusion of a cooling step after the cleaning stage eliminates the risk of injecting samples onto a hot platform. Maximum stabilizing effect To define the maximum ashing temperature allowed with no losses of the analyte ashing plots for 10 pl of a 100 pg ml-’ phosphorus solution in the presence of the optimum amount of each modifier were constructed. RESULTS The graphs obtained for the optimum amount of modifier tests are shown in Fig.l(a) and (b). It is clearly seen that there is a minimum amount of each modifier at which the phosphorus signals exhibit their maximum thermal stabilization. Amounts of modifier greater than these are not necessary for stabilization purposes. Smaller amounts do not provide the maximum stabilization capacity of the modifiers. Table 3 summarizes the optimum amount of each of the modifiers used. 0.1 0.2 0.3 0.4 0.5 O*OOt!l 2 4 6 8 1’0 1’2 1’4 1’6 1’8 :O Concentration (“A rn/v) Fig. 1 Optimal amounts of (a) NaF KF and CsF and (b) HF and NH4F as chemical modifiers for phosphorus lop1 of 100pgml-’ aqueous phosphorus solution; and ashing temperature 1000°C 484 Journal of Analytical Atomic Spectrometry July 1995 Vol.10Table3 Optimum amount of each modifier tested for the thermal stabilization of 10 p1 of a 100 pg ml-' phosphorus solution Modifier HF NH4F CsF KF NaF Optimum amount* (% m/v) 8.0 5.0 0.5 0.3 0.08 * Defined as the minimum amount of modifier needed to produce the maximum thermal stabilization of the phosphorus absorbance signal. 0.20 1 1 t I - 0.001 " 1 ' ' 1 ' 1 " I 600 800 1000 1200 1400 Temperat ure/"C Fig. 2 Ashing plots of phosphorus in the presence of optimal amounts of different modifiers; 10 pl of 100 pg ml-' aqueous phosphorus solution The ashing plots used to define the maximum stabilizing effect of each fluoride on the atomic absorption signal of phosphorus are shown in Fig. 2 and indicate that each fluoride provides thermal stability to the phosphorus signals.These plots also indicate the relative sensitivity of the phosphorus measurements in the presence of each modifier. Comparison of Figs. l(a) l(b) and 2 shows a significant difference in sensitivity for the plots referred to the same amount of phosphorus and same amount of fluoride modifiers at the same ashing temperature. This could be ascribed to the dependence of phosphorus signals on the physical conditions of the graphite a t ~ m i z e r . ~ - ~ This reasoning is based on the findings of Curtius et aL7 and our own work. Curtius et al. found an increased sensitivity for the determination of phos- phorus when using standard graphite tubes. We found higher absorbance signals for phosphorus when using corroded pyro- lytic graphite-coated graphite tubes as compared with new tubes.Data for plotting Fig. l(a) and (b) were obtained using already used graphite tubes and platforms. New graphite tubes and platforms were not used for these tests as the main purpose was to find the optimum amount of modifier. However to define the modifier that provided the maximum stabilization effect and the highest sensitivity for the phosphorus measure- ments new graphite tubes and platforms were used to collect the data for plotting each graph shown in Fig. 2. From Fig. 2 it is evident that the maximum thermal stabilization and highest relative sensitivity were achieved using either NaF or KF as chemical modifier. Of these NaF was selected as the Table 4 Maximum ashing temperatures for phosphorus aqueous solu- tions using the chemical modifiers ~~ ~~~ Modifier None HF NH4F CsF KF NaF Ashing temperature/ "C 300 1150 1200 1150 1350 1350 more convenient chemical modifier as the optimum amount of this salt needed to obtain the maximum stabilization is much less than that for KF (see Table 3).Table 4 summarizes the maximum ashing temperatures allowed using the new modifiers. For comparison purposes the maximum temperature without modifier is also included. Having established that NaF is among the fluorine com- pounds studied the more convenient chemical modifier for phosphorus its performance was compared with that of pal- ladium which alone or in combination with calcium is one of the best modifiers proposed for phosphorus determination by ETAAS.8 For these tests ashing plots for 10 p1 of a 100 pg ml-' phosphorus solution containing 10 p1 of 0.08% w/v NaF solu- tion and of 10 pl of a 20 pg ml-' phosphorus solution contain- ing 10 p1 of 1300 pg ml-' palladium nitrate modifier solution were constructed.The different phosphorus concentrations of the solutions studied reflected the fact that phosphorus measurements using palladium as a chemical modifier were more sensitive than those using NaF. The two phosphorus concentrations used allowed for a clear direct comparison of the ashing plots on a single absorbance scale as shown in Fig. 3 which clearly indicates that NaF is as good a thermal stabilizer as Pd for phosphorus. Both modifiers allow the use of ashing temperatures of the order of 1350"C high enough for the destruction of a wide variety of sample matrices.The decrease in sensitivity experienced by the phosphorus signal in the presence of NaF when compared with the results using Pd cannot be readily explained and is currently under study. These studies are aimed at understanding the stabilization mechanism of phosphorus by fluoride which could possibly shed some light on why the phosphorus absorbance signals are less sensitive in the presence of fluoride than in the presence of palladium. So far we do not have enough data to make a reasonable interpretation. Determination of Phosphorus in Standard Reference Materials The performance of NaF as a chemical modifier in the determi- nation of phosphorus in real samples was evaluated by analyses of several SRMs. The ashing plots obtained using the digest of the certified materials proved that the stabilizing effect of sodium fluoride was not only exerted on phosphorus aqueous solutions.An ashing temperature of 1350 "C was used in these determinations. Dissolution of the SRMs was achieved using acid digestion assisted by microwave heating. As mentioned under Experimental during dissolution of the SRMs it is necessary to control the inner pressure of the vessels used to contain the samples to be digested by means of microwave heating. Biological samples such as those selected in this work generate considerable amounts of gaseous species during digestion. Leaving the vessels open during the first stage of the digestion 0.200 1 I 1000 1500 0.000 5;o TemperaturePC Fig. 3 Comparison of NaF (10 pl of 0.08% m/v aqueous solution) and Pd (10 pl of 1300 pg ml-' aqueous solution) as chemical modifiers for phosphorus (10 pl of 100 pg ml-' aqueous solution for NaF and 10 pl of 20 pg ml-' aqueous solution for Pd) Journal of Analytical Atomic Spectrometry July 1995 Vol.10 485Table 5 Results and standard deviations for the determination of phosphorus in Standard Reference Materials (n = 5 ) Value obtained s Certified value f s Material (YO m/m) (YO m/m) SRM 1570 0.538 k0.012 0.55 _+ 0.02 Trace Elements in Spinach SRM 1571 0.21 1 -t 0.017 0.21 kO.01 Orchard Leaves SRM 1573 0.347 +0.010 0.34 +_ 0.02 Tomato Leaves SRM 1575 0.124 + 0.007 0.1250.02 Pine Needles SRM 1577a 1.03 k 0.02 1.11 k0.04 Bovine Liver reaction helps to minimize the risk of vessel failure (the safety membrane will rupture and the sample will be lost) owing to excessive pressure which otherwise could occur if the sample is microwave heated in closed vessels from the very beginning of the digestion process.The programme presented in Table 1 shows a longer time period to reach the pre-set pressure of 801b inv2 than that needed to reach the higher pressure of 1501b in-2 set for the second step. The shorter time needed to reach the pre-set pressure in this step is a consequence of the evolution of gases. Treatment of the SRMs according to the procedure described and using the microwave heating programme presented in Table 1 gave solutions with no visually detectable solids in suspension and without problems of vessel failure. The results obtained by analysing these SRMs in comparison with aqueous standards and using NaF are given in Table 5.As can be seen there is a close match between the certified values and the values obtained in this work. The greatest disparity (about 7%) occurs for SRM 1577a Bovine Liver. As this material has the highest phosphorus content among the SRMs assayed the opposite would be expected. However it also has the most complex matrix among the standards studied. It is possible that the microwave heating dissolution procedure applied is very efficient for the dissolution of vegetable materials but not materials of animal origin although the solutions obtained apparently showed complete dissolution. In general the good agreement between the phosphorus concentrations found and the certified values indicates that NaF can be used for accurate determinations of phosphorus in real samples.CONCLUSIONS The determination of phosphorus by ETAAS undoubtedly needs the assistance of chemical modification. Of HF NaF KF CsF and NH,F chemical modifiers for phosphorus NaF was shown to be the most efficient stabilizing the phosphorus signals to the same extent as the traditional modifiers Pd and La albeit with lower sensitivity but without the corrosion and memory effect problems inherent in their use Additionally NaF presents no impurity problems is easily dissolved in water (no need for extreme digestion conditions) and is readily available at relatively low cost. Using NaF as chemical modifier good agreement was obtained with the certified phosphorus contents of several Standard Reference Materials.One of the authors (J.A.) acknowledges the funding of this project by the Consejo Nacional de Investigaciones Cientificas y Tecnolbgicas CONICIT under project S1-2233 and grant MPS-RP-VII 260076 and financial support from the Decanato de Investigaciones at Universidad Simon Bolivar. REFERENCES 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 Chiricosta S. Saija G. Calapaj R. and E. Bruno At. Spectrosc 1989 10 183. Manning D. C. and Slavin S. At. Absorpt. Newsl. 1969 8 132. Persson J. A. and Frech W. Anal. Chim. Acta 1980 119 75. Whiteside P. J. and Price W. J. Analyst 1977 102 618. Ediger R. D. Knott A. R. Peterson G. E. and Beaty R. D. At. Absorpt. Newsl. 1978 17 28. Welz B. Curtius A. J. Schlemmer G. Ortner H. M.and Birzer W. Spectrochim. Acta Part B 1986 41 1175. Curtius A. J. Schlemmer G. and Welz B. J . Anal. At. Spectrom. 1986 1 421. Curtius A. J. Schlemmer G. and Welz B. J. Anal. At. Spectrom. 1987 2 115. Curtius A. J. Schlemmer G. and Welz B. J. Anal. At. Spectrom. 1987 2 311. Slavin W. Manning D. C. and Carnrick G. R. At. Spectrosc. 1981 2 137. Slavin W. Manning D. C. and Carnrick G. R. Talanta 1989 36 171. Tsalev D. L. At. Spectrosc. 1991 12 169. Tittarelli P. and Mascherpa A. Anal. Chem. 1981 53 1466. Langmyhr F. J. and Dahl I. M. Anal. Chim. Acta 1981,131 303. Welz B. Schlemmer G. and Mudakavi J. R. J. Anal. At. Spectrom. 1988 3 695. Certificate of Analysis Standard Reference Material 1570 (Trace Elements in Spinach) National Institute of Standards and Technology. Certificate of Analysis Standard Reference Material 1571 (Orchard Leaves) National Institute of Standards and Technology. Certificate of Analysis Standard Reference Material 1573 (Tomato Leaves) National Institute of Standards and Technology. Certificate of Analysis Standard Reference Material 1575 (Pine Needles) National Institute of Standards and Technology. Certificate of Analysis Standard Reference Material 1577a (Bovine Liver) National Institute of Standards and Technology. Miller R. O. presented at the International Soil Testing and Plant Analysis Symposium August 22-27 199 1 Florida USA. Paper 4/07582J Received December 13 1994 Accepted March 1 1995 486 Journal of Analytical Atomic Spectrometry July 1995 Viol. 10

ISSN:0267-9477    

DOI:10.1039/JA9951000483

出版商:RSC    

年代:1995

数据来源: RSC

摘要:

Determination of Mineral and Trace Elements in Total Diet by Inductively Coupled Plasma Atomic Emission Spectrometry Comparison of Microwave-based Digestion and Pressurized Ashing Systems Using Different Acid Mixtures* Journal of Analytical Atomic Spectrometry VIRGINIA E. NEGRETTI DE BRATTER PETER BRATTER AND ALBRECHT REINICKE Hahn-Meitner Institut Berlin Department of Trace Elements in Health and Nutrition Glienicker StraJe 100 D-14109 Berlin Germany GERHARD SCHULZE Technical University of Berlin FB 05 Institute of Inorganic and Analytical Chemistry Strape des 17 Juni 135 0-10623 Berlin Germany WALTER OLIVER L. ALVAREZ AND NESTOR ALVAREZ Centro de Control de Cancer Gastrointestinal 'Luis Anderson' La Concordia San Cristdbal Edo. Tachira Venezuela The effectiveness of different acid mixtures for the de-mineralization of total diet samples of different origin and composition by means of a closed microwave-based technique and a pressurized-ashing technique were investigated.The aim was to obtain complete acid solubilization for the subsequent accurate determination of AI Ca Cu Fe K Mg Na P and Zn by means of inductively coupled plasma atomic emission spectrometry (ICP-AES). The sampling and sample preparation steps for the trace element analysis are described. The special care taken in the sampling design to ensure the representativeness of the sample for the population studied is also mentioned. The regions and population groups were selected from the high mountain valleys where a high incidence of stomach cancer exists and a low altitude valley at the foot of the Andes which is a low stomach cancer incidence region both located in the state of Tachira Venezuela.Total diets including breakfast lunch supper snacks and drinks from the whole-day intake of 140 adults were collected. The collection of the total diet was made according to the double- portion technique. The most reliable digestion procedure for the determination of Al Ca Cu Fe K Mg Na P and Zn in total diet by means of ICP-AES was a microwave-based technique using HNO alone or with the mixture HNO + H,O (2 + 1). In comparison a pressurized-ashing technique is faster although lower values for K (13 and 11%) were obtained. Despite low sensitivity for the ICP-AES measurements the microwave-based digestion using HN03 + H,S04 (4 + 1) also gave good agreement for the determination of Al Ca Cu Fe K Mg Na P and Zn by means of ICP-AES.Because of the simple and rapid procedure the pressurized-ashing technique using the mixture HNO,+H,O (2+ 1) was selected to perform the digestion of the total diet samples collected. The results of the mean daily intake of the population investigated showed for the high mountain valleys (high stomach cancer incidence area n = 77) as compared with the low altitude valleys (low stomach cancer incidence area n = 33) significantly higher daily intake with respect to Na (2082 versus 1471 mg) K (1190 uersus * Presented at the Third Rio Symposium on Atomic Spectrometry Caracas Venezuela November 6-12 1994. 731 mg) P (640 versus 381 mg) and a significantly lower daily intake with respect to Ca (925 versus 1379 mg) and Cu (2.78 versus 4.66 mg).No differences were obtained with respect to Al Fe Mg and Zn. Keywords Inductively coupled plasma atomic emission spectrometry; total diet; pressurized ashing digestion; microwave-based digestion; mineral and trace elements For the determination of mineral and trace elements in real rather than aqueous samples by means of inductively coupled plasma atomic emission spectrometry (ICP-AES) fast and reliable digestion procedures are needed. Total diet is a complex matrix because of its variable food composition and special care has to be taken during the sample digestion with respect to the varying fat and fibre contents. The influence of the concentration and nature of the acid used for the sample decomposition on the relative emission intensity during ICP-AES analysis has been described for a number of elements.'-' The effectiveness of digestion techniques using different acid mixtures for the de-mineralization of biological samples has also been described but there have been few reports on the analysis of total diet by means of ICP- AES.8-" The use of microwave energy as the heat source in acid digestion of fat-rich foods has also been reported but only for the determination of Se and Hg by means of atomic absorption spectrometry.12 The effect of microwave radiation on mineral acidsI3 has also been investigated.In the present work the effectiveness of different acid mix- tures for the de-mineralization of total diet samples of varying origin and composition by means of a closed microwave-based technique and a pressurized-ashing technique was investigated. The aim was to obtain complete acid solubilization for the subsequent accurate determination of Al Ca Cu Fe K Mg Na P and Zn by means of ICP-AES.Another aim of the work was to compare the concentration of mineral and trace elements in the diet of populations living in geographical regions with different cancer incidence rates. Because sampling is a critical aspect of chemical analysis the sampling and sample pre-treatment were designed specifically for the particular trace element analysis. Care was also taken Journal of Analytical Atomic Spectrometry July 1995 Vol. 10 487in the sampling design to ensure the representativeness of the sample for the population studied to allow a valid statistical interpretation of the results obtained.Sample collection Total diets including breakfast lunch supper snacks and drinks from the whole-day intake of 140 adults were collected. EXPERIMENTAL Sampling Epidemiological background The Andean states of Venezuela (Tachira Merida and Trujillo) show the highest incidence and mortality14 due to cancer of the stomach in the whole country. Since 1981 a Program of Mass Screening on Gastric Cancer (GCP) has been carried out in the state of Tachira Venezuela. The GCP follows the Japanese model of screening through double contrast fluoro- photography (indirect radiology) followed by gastroscopy and biopsy in patients with gastric wall lesions. This screening is offered to the whole rural population for people 35 years of age and over every two years.A study of the population of the state allowed classification of the regions with high and low incidence of this neoplasm. The high-incidence areas are located in the Andes at an altitude of over 800m above sea level. The low-incidence regions are in the plains that surround the mountains with an altitude below 400 m. In the highlands mortality reaches 109 per 100 000 inhabitants. In the plains mortality is under 25 per 100 000 (age standardized). This epidemic type of stomach cancer could be related to diet and environmental conditions.” For this reason the department of Oncology of the Ministry of Health and Social Assistance of Venezuela and the Gastrointestinal Cancer Control Centre (‘Centro de Control de Cancer Gastro- intestinal’) in San Cristobal Tachira initiated a co-operative study with the Hahn-Meitner Institute in Berlin Germany in order to investigate the factors that could cause the high incidence of stomach cancer in the state of Tachira.Description of the geographical region The regions and the population groups to be studied were selected based on the epidemiological results of the GCP performed by the Gastrointestinal Cancer Control Centre and with the support of the German National Cancer Research Centre in Heidelberg. The state of Tachira belongs to the Andes and shows a variety of climates and biological environments. The selected regions were the high mountain valleys where the high incidence of stomach cancer exists and a low altitude valley at the foot of the Andes which is a low stomach cancer incidence region.Description of the population group One hundred and fifty subjects were recruited from amongst the people participating in the screening programme. Several subjects were dismissed from the group. Finally 44 gastric cancer patients and 50 controls from the high-risk areas and 46 controls from the so-called low-risk areas were studied. Every cancer patient was paired with a control of the same age and sex. The population studied belonged to the low socio-economic classes IV and V. Classification was performed according to the stratification method of Mendez Castellano et by means of interviews and home visits. Trained social workers from the Gastrointestinal Cancer Control Centre explained the purpose of the study to all prospective participants. This resulted in a participation rate of the selected population of 98%. The participants were requested to collect the samples in plastic containers previously treated to avoid any contami- nation of the elements of interest. The collection of the total diet was made according to the double-portion technique. Trained nutritionists and social workers instructed the partici- pants on the technique of collection.During an interview a nutritional questionnaire was filled out to check the repres- entative value of the collected samples. The samples were recorded and every component separately weighed. Until homogenization the collected total diets were deep-frozen at - 10 “C. Sample Pre-treatment Standard specifications for cleaning of the sampling equipment All sampling equipment was cleaned to avoid any contami- nation of the elements of interest. The plastic containers were cleaned with a stock cleaning solution of 10% HN03 (65% Suprapur Merck Darmstadt Germany) prepared using doubly distilled water.Every container and its respective cover (these were kept together throughout the whole procedure) were first individually rinsed several times with doubly distilled water and then both were filled with the stock cleaning solution. Each cover and its cup were left standing overnight in a dust-free environment with the acidified doubly distilled water. The next day each container and cover was rinsed individually with doubly distilled water several times; all contact with the inside of the container as well as with the inside of the cover was avoided.The quartz equipment used for the sample preparation were cleaned by means of a distillation acid vapour device (Kurner Rosenheim Germany) using HN03 (65% Suprapur Merck). After a 2-h treatment the quartz containers were individually rinsed several times with doubly distilled water. Sample homogenization The solid components of the meals were first cut with a titanium knife. After addition of a portion of the liquid component of a given person’s meal (soup or water) the solids were pre-homogenized with a mixer (Krups Solingen Germany) provided with a specially designed titanium cutter (Material Workstation of Section N Hahn-Meitner Institute Berlin Germany). The final fine homogenization was per- formed by manual mixing of all the pre-homogenized compo- nents using pre-cleaned plastic equipment.After stirring the drink samples each drink was gently dried in an oven at 50°C. Sample lyophilisation An aliquot of 300 g of the homogenized meals plus the whole of the dried drinks were individually lyophilised (Lyovac GT2 Leybold-Heraeus Koln Germany). A check on the homogeniz- ation was performed and a detailed protocol of the drying steps was kept. Sample pulverization The lyophilised sample was pulverized in a Teflon container with Teflon balls until a particle diameter of approximately 20 pm was achieved (‘Pulverisette 6‘ Fritsch Mar Oberstein Germany). Until required preparation for analysis the samples were deep-frozen at - 20 “C in low-density polyethylene containers.488 Journal of Analytical Atomic Spectrometry July 1995 Vol. 10Sample Analysis Sample digestion The pulverized total diet sample was first gently dried at 50 "C. After shaking a 100 mg sample of the collected total diet was taken to be digested whereas a higher sample mass of the Standard Reference Materials (SRMs) was used in order to fit the element concentrations found into the calibration range. After evaluation of different acid mixtures used by other workers for the digestion of biological sample^,'^*'^-^' the following mixtures for the digestion were investigated HNO (alone) HNO + H,02 (2 + l) HNO + H2S04 (4 + 1) and HNO,+HCl(2+ 1). The sample was left to stand overnight in 1000 pl of HNO (65% Suprapur Meck) in the quartz container of the digestion device.The next day the other reagents (H2S04 98% Suprapur Merck; HCl 30% Suprapur Merck; and H202 30% Selectipur Merck) were added in the proportions listed above. 180min at 110°C; then an increase over 60min to 180°C followed by 180 min at 180 "C. Digestion techniques A comparison of the effectiveness of acid digestion using both the closed microwave-based and the pressurized-ashing techniques was performed. Microwave-based technique. A Type PMD (Kurner) microwave system was used. The acidified sample was introduced into the quartz container which was then closed with a security cover. The maximum microwave power of the apparatus is 750 W. The dial settings for the microwave power are from 0 to 10. A three-stage procedure was performed 3 min at setting 2 5 min at 4 and 2min at 8.After each step had finished the sample was cooled for the same time as it had been irradiated. Pressurized-ashing technique. A pressurized-ashing system with six sample positions (Seif Unterschleipheim Germany) each suitable for maximum sample masses of 100 mg and another with two sample positions each for maximum sample masses of 500mg was used. The quartz container with the acidified sample was inserted into a Teflon support and first covered with a quartz and then with a Teflon top. The temperature programme (Heraeus) applied was as follows a continuous increase in the temperature over 60 min to 110 "C followed by Table 1 ICP-AES operating conditions for the determination of Al Ca Cu Fe K Mg Na P and Zn in total diet Parameter Argon flow rates/l min-' Intermediate gas Outer gas (coolant) Aerosol carrier gas Sample flow rate/ml min-l Analyte line and wavelength/nm A1 396.152 Ca c u 3 24.7 54 Fe Na 589.592 P Zn 213.856 K 766.490 Mg Value 0.3 12 0.8 1 393.366 259.940 279.079 2 14.9 14 Sample and calibration solutions The digested sample was transferred into a polyethylene tube (Sarsted Numbrecht Germany) and filled with de-mineralized water until a mass of l o g was reached.This dilution was found to be optimal for the ICP-AES analysis. The specific gravity of the acid mixture was used for calculating the final element content in the sample volume analysed. Acid m a t c h e d ' ~ ~ ~ . ~ ~ XISAG-5 multi-element standard (Spex Edison NY USA) was used for the preparation of six cali- bration solutions which were subjected to the same procedures as the samples.The calibration ranges for the elements of interest were as follows Zn 0.08-4.0 P 8.0-400 Fe 0.08-4.0 Mg 0.8-4.0 Cu 0.08-4.0 Ca 4.0-200 A1 0.04-2.0 Na 140-7000 and K 8.0-400 mg kg- ' . Instrumentation A Jobin-Yvon (Instruments SA Longjumeau France) induc- tively coupled plasma atomic emission spectrometer JY 70 Plus system with a plasma generator of 1.2 kW and frequency 40.68 MHz equipped with a Meinhard-type cross-flow nebul- izer was used for the simultaneous determination of Al Ca Cu Fe K Mg Na P and Zn. Samples and standards were measured five times. A mass-flow controller was used for the aerosol carrier and intermediate gases. Other parameters for the operating conditions are shown in Table 1.RESULTS A N D DISCUSSION Analytical Aspects The influence of the acid composition of the sensitivity of the element signal was checked. The results are given in Table 2. With regard to the influence of the acid mixture on the sensitivity of ICP-AES determination the best results are those obtained from the digestion with HNO alone and with The SRM 1548 Total Diet [National Institute of Standards and Technology (NIST) Gaithersburg MD USA] was used to check the single-set ~alibration.~'.~~ This SRM was also used for quality control purposes and to evaluate the effective- ness of the procedures. For the latter the SRM underwent each digestion technique for each acid mixture (Table 3). The detection and determination limits for the elements determined using the HNO + H202 mixture (2 + 1) are shown in Table 4.The check of the day-to-day variation by analysing an XISAG-5 standard solution at the middle of the concen- tration range yielded the following relative standard deviations (the standard solution underwent all sample preparation steps) for Zn 6; P 1.9 Fe 1.8 Mg 2; Cu 0.9; Ca 1.6; A1 6; Na 0.9 and K 1.0%. The SRMs 1577a Bovine Liver and 1566 Oyster Tissue were also used to check the accuracy of the results. The values for Fe and Zn were confirmed by analysing undigested aliquots of the collected total diet using instrumental neutron activation HNOj+H,Oz (2+1). Table 2 Influence of the acid mixture on the sensitivity (Asignal/Aconcentration) of ICP-AES determined by measuring the matrix-matched calibration solution.The values are given in YO and calculated in relation to the highest sensitivity (100%) obtained. Values in parentheses are the relative standard deviation of different measurements (n= 3) Zn P Fe Mg c u Ca A1 Na K Acid (2%) (2%) ( 2 %) (1.5%) (2.6%) (2%) ( 5 % ) (2.6%) (2%) HNOJ 100 82 100 100 100 100 95 100 100 HNO + HZOZ 96 76 97 98 98 100 97 94 97 HNO + H,S04 81 100 87 87 83 93 91 89 91 HNO + HC1 94 80 95 95 99 100 100 91 94 Journal of Analytical Atomic Spectrometry July 1995 Vol. 10 489Table 3 Effectiveness of different acid mixtures for the de-mineralization of the NIST SRM 1548 Total Diet by means of the pressurized-ashing technique (PA) and the closed microwave-based technique (MW). The SRM underwent each digestion technique for each acid mixture (n = 3).Values are given in mg kg-' Element Fe Mg c u Ca Zn P Na K A1 HNO HNO + H2S04 (4+ 1) HNO + HCI (2+ 1) PA 36.8 f 1.5 577 f 13 2.6 f0.2 1820f40 33f2 3230 f 60 6000 f 200 5290 f 180 28.6 f 1.3 MW 34.9 f 0.4 585 f 5 2.8 20.5 1810f30 29.2 f 0.5 3250f 150 6320f 140 5620 & 90 30f 10 PA 37*3 557 f 18 2.48 f 0.09 1760+60 30.60 f 0.18 3370 k 90 6200 f 300 5400 f 200 3 0 f 4 MW 34+3 565 f 8 2.48 f 0.19 1730 f 30 30.2 f 1.3 3200 f 80 6300 & 300 5600 f 200 3155 PA 36f2 560 & 20 2.49 f 0.17 1740 f 40 30.4 f 1.2 3020 f 60 5790 & 160 5180 k 110 27.4 f 0.6 MW 35.5 * 1.1 600 f 19 2.44 0.05 1810f40 29.8 f 1.4 3300 f 300 6280 f 150 5700 f 200 29.7 f 0.2 PA 36f2 550 f 30 2.57 + 0.1 3 1750f90 30f2 3250 & 100 5400 f 300 4700 + 200 25.6 i 1.8 MW 33.0+_ 1.5 560 f 30 2.41 f 0.12 1770 f 60 26.1 k 1.0 3290 f 70 6000 f 270 5 300 k 200 26.1 f 0.4 Certified value 32.6 f 3.6 556 27 2.6 f 0.3 1740 f 70 30.8 f 1.1 3240 f 40 6250 f 260 6060 f 280 33 (not certified) Table 4 Detection limit (pg kg-') and determination limit (pg kg-') of the elements of interest by ICP-AES using an HN03 + H202 (2 + 1) matrix-matched blank Element Zn P Fe Mg Cu Ca A1 Na K Detection limit* 37 2400 7.3 1.64 2.5 0.72 12 40.5 490 Determination limit* 146 9620 29.3 6.6 10.12 2.9 48 162 1950 Based on the present experiments the most reliable digestion procedure for the determination of Al Ca Cu Fe K Mg Na P and Zn in total diet by means of ICP-AES is the microwave- based technique using HNO alone (Table 5 ) or with the mixture HN03 + H202 (2 + 1).In comparison the pressurized- ashing technique is faster although lower values for K (13 and 11 % with the two acid mixtures respectively) were obtained. Because the procedure is simple and rapid it was decided to perform the determination of Al Ca Cu Fe K Mg P and Zn in the collected total diet by means of ICP-AES using the mixture HN0,+H202 (2+ 1) for digestion of the sample in the pressurized-ashing system. * Detection limit XDL = 3SJm and determination limit Xdet = 12SL/m where m=slope S,=standard deviation of the blank of the acid-matched standard solution and n = 5. analysis (INAA) as an independent method for the quality control of the measurements. It is shown in Table 3 that HN03 alone and HNO + H,02 (2+1) are the most effective both for pressurized-ashing and for the microwave-based digestion.Nevertheless lower values for K were obtained when pressurized-ashing was used. It was assumed that the Teflon cover of the pressurized-ashing system absorbed K but more experiments must be carried out to corroborate this phenomenon. Lower values of A1 were obtained for all the digestion procedures but only a small relative deviation occured when using the closed microwave-based digestion with HN03 alone or the mixture HN03+H202 (2+1). It must be pointed out that the given value for A1 is not certified. Despite a low sensitivity for the ICP-AES measurements the microwave- based digestion using HN03 +H,S04 (4+ 1) also gave good agreement for the determination of Al Ca Cu Fe K Mg Na P and Zn by means of ICP-AES. Mineral and Trace Element Composition of the Total Diet in the Tachira Region The mean daily intake of solid food per person was 900 g and the mean daily volume of drinks was 1 1.The fat content varied from 3 to 50% and the fibre content from 1.6 to 1.8%.34 In Table 6 the mean daily intakes of the elements as calculated from the analysis of the total diet are shown. The average consumption of individual foods was computed in terms of mg per person per day. The results of the mean daily intake of the population investigated show for the high mountain valleys [high cancer incidence area (n=77)] as compared with the low altitude valleys [low cancer incidence area (n = 33)] significantly higher daily intake with respect to Na (2082 versus 1471 mg) K (1190 versus 731 mg) P (640 versus 381 mg) and a significantly lower daily intake with respect to Ca (925 versus 1379mg) and Cu (2.78 versus 4.66 mg).No differences were obtained with respect to Al Fe Mg and Zn. Finally it has to be kept in mind that the influence of the daily intake of several elements investigated in this work represents only one aspect of the multifactorial pathogenesis of stomach cancer. Table5 Interpretation of the effectiveness of different acid mixtures Tor the de-mineralization of SRM 1548 Total Diet by means of the pressurized-ashing technique (PA) and the closed microwave-based technique (MW). 0 Result was within the certified value; 0 result was lower than the certified value; 0 result was comparable with the non-certified value HNO HNO + H2S04 (4+ 1) HNO + HCl (2+ 1) Element Fe Mg c u Ca Zn P Na K A1 PA MW 0 0 0 0 0 0 0 0 0 0 0 0 0 0 -13% 0 -13% 0 - 9 % o PA MW 0 0 0 0 0 0 0 -11% 0 -9% Q 0 0 0 0 0 0 0 0 - 6% Q PA MW 0 0 0 0 0 -7% 0 -15% 0 -17% 0 - -7% 0 0 0 0 0 0 0 0 0 10% 0 PA MW 0 0 0 0 0 0 0 0 O -15% 0 0 -14% 0 -22% -13% -22% 0 -21% 0 Certified value/mg kg- I 32.6 k 3.6 556 f 27 2.6 f 0.3 1740 f 70 30.8 1- 1.1 3240 f 40 6250 & 260 6060 f 280 33 (not certified) 490 Journal of Analytical Atomic Spectrometry July 1995 Kd.10Table 6 Results of the mean daily intake (mg per day per person) of minerals and trace elements of the population investigated in the state of Tachira. 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ISSN:0267-9477    

DOI:10.1039/JA9951000487

出版商:RSC    

年代:1995

数据来源: RSC