摘要:

Journal of Analytical Atomic Spectrometry {Including Atomic Spectrometry Updates) JAAS Editorial Board* Chairman B L Sharp (Loughborough UK) J. Egan (Cambridge UK) J M Mermet (Villeurbanne France) S J. Haswell (Hull UK) D A Hickman (London UK) J Marshall (Middlesbrough UK) D L Miles (Keyworth UK) R D Snook (Manchester UK) "The JAAS Editorial Board reports t o the Analytical Editorial Board Chairman A G Fogg (Loughborough UK) JAAS Advisory Board F C Adams (Antwerp Belgium) R M Barnes (Amherst MA USA) L Bezur (Budapest Hungary) R F Browner (Atlanta GA USA) S Caroli (Rome Italy) A J Curtius (Rio de Janeiro Brazin J B Dawson (Leeds UK) M T C de Loos-Vollebregt (Delft The K Dittrich (Leipzig Germany) L Ebdon (Plymouth UK) M S Epstein (Gaithersburg MD USA) Fang Zhao-lun (Shenyang China) W Frech (Umea Sweden) A L Gray(€gham UK) S Greenfield (Loughborough UK) G M Hieftje (Bloomington IN USA) G Horlick (Edmonton Canada) D Littlejohn (Glasgow UK) B V L'vov (Sf Petersburg Russia) T Nakahara (Osaka Japan) Ni Zhe-ming (€?eying China) N Omenetto (lspra Italy) R E Sturgeon (Ottawa Canada) V Sychra (Prague Czechoslovakia) R Van Grieken (Antwerp Belgium) A Walsh K B (Victoria Australia) B Welz (Uberlingen Germany) T S West (Aberdeen UK) Netherlands) A Sanz-Medel (Oviedo Spain) Atomic Spectrometry Updates Editorial Board Chairmarl "D.L. Miles (Keyworth UK) J. Armstrong (Dumfries UK) J. R. Bacon (Aberdeen UK) C. Barnard (Glasgow UIO R. M. Barn-es (Amherst MA USA) S. Branch (High Wycombe UK) R Bye (Oslo Norway) J. Carroll (Middlesbrough UK) M. R.Cave (Keyworth UK) "J. M. Cook (Keyworth UK) "M. S. Cresser (Aberdeen UK) H. M. Crews (Norwich UK) J. S . Crighton (Sunbury-on-Thames UK) J. R. Dean (Newcastle upon Tyne UK) A. W. McMahon (Harwell UK) J M. Mermet ( Villeurbanne France) R. G. Michel (Srorrs CT USA) T. Nakahara (Osaka Japan) Ni Zhe-ming (Belling China) P. R. Poole (Hamilton New Zealand P. J. Potts (Milton Keynes UIO W. J . Price (Ashburton UK) C. J. Rademeyer (Pretoria South Africa) "M. H. Ramsey (London UK) A. Sanz-Medel (Oviedo Spain) "B. L. Sharp (Loughborough UK) I. L. Shuttler (Uberlingen Germany) S. T. Sparkes (Plymouth UK) R.Stephens (Halifax Canada) J.Stupar (Llub/pna Slovenia) R . E. Sturgeon (Ottawa Canada) A. P. Thorne (London UK) G. C. Turk (Gaithersburg MD USA) J. F Tyson (Amherst MA USA) S .J. Walton (Crawley UK) P Watkins (London UN B. Welz ( Uberlingen Germany) J. Williams (Egham UKI J. B. Willis (Victoria Australia) *J. B. Dawson (Leeds UK) "J. Egan (Cambridge UK) *A. T. Ellis (Oxford UIO J. Fazakas (Bucharest Romania) D. J. Halls (Glasgow UK) "A. Taylor (Guildford UK) "D. A. Hickman (London UK) "S. J. Hill (Plymouth UK) K. W. Jackson (Albany NY USA) R. Jowitt (Middlesbrough UK) K. Kitagawa (Nagoya Japan) J. Kubova f Bratislava Czechoslovakd "J. Marshall (Middlesbrough UK) H. Matusiewicz (Poznan Poland) *Members of the ASU Executive Committee Editor JAAS Judith Egan The Royal Society of Chemistry Dr J M Harnly Thomas Graham House Science Park Milton Road Cambridge CB4 4WF UK Telex No 818293 Fax 0223 423623 Beltsville M D 20705 USA E-mail RSCI@UK AC RL GB (JANET) Assistant Editors Brenda Holliday and Ed/tonal Secretary Monique Warner US Associate Editor JAAS US Department of Agriculture Beltsville Human Nutrition Research Center Telephone 0223 420066 BLDG 161 BARC-EAST Telephone 301 -504-8569 Paula O'Riordan Advertisements.Advertisement Department The Royal Society of Chemistry Burlington house Piccadilly London W I V OBN UK Telephone 071-437 8656 Fax 071-494 1134 Information for Authors Full details of how to submit materials for publica tion in JAAS are given in the Instructions to Authors in Issue 1 Separate copies arc available on request The Journal of Analytical Atomic Spectrometry (JAASi is an international journal for the publica- tion of original research papers communications and letters concerned with the development and analytical application of atomic spectrometric techniques The journal is published eight times a year including comprehensive reviews of specific topics of interest to practising atomic spectrosco- pists and incorporates the literature reviews which were previously published in Annual Reports on Analytical Atomic Spectroscopy (ARAAS) Manuscripts inteqded for publication must de- scribe original work related to atomic spectromet- ric anaiysis Papers on all aspects of the subject will be accepted including fundamental studies novel instrument developments and practical ana- lytical applications As well as AAS. AES and AFS papers will be welcomed on atomic mass spec trometry and X-ray fluorescence/emission spec trometry Papers describing the measurement of molecular species where these relate to the char- acterization of sources normally used for the pro duction of atoms or are concerned for example with indirect methods of anaiysis will also be ac- ceptable for publication Papers describing the de velopment and applications of hybrid techniques ( e g GC-coupled AAS and HPLC-ICP) will be par ticularly welcome Manuscripts on other subjects of direct interest to atomic spectroscopists.in- cluding sample preparation aqd dissolution and analyte pre-concentration procedures as wet' as the statistica irterpretation and use of atomic spectrometric data will also be acceptable for pcib- lication There is no page charge The following types of papers will be consid- ered Full papers describing original work Commun/cations which must be on an urgent matter and be of obvious scientific irnportance Communications receive priority and are usually published within 2-3 months of receipt They are Intended for brief descriptions of work that has progressed to a stage at which it is likely to be valuable to workers faced with similar problems Reviews which must be a critical evaluation of the existing state of knowledge on a particular facet of analytical atomic spectrometry Every paper (except Communications) will be submitted to at least two referees by whose advice the Editorial Board of JAAS will be guided as to its acceptance or rejection Papers that are accepted must not be published elsewhere except by permission Submission ot d manu- script will be regarded as an undertaking that the sahe material is not being considered for publica- tion by another journal Manuscripts (three copies typed In double spacing) should be sent to Judith Egan Editor JAAS or Dr J M Harnly US Associate Editor JAAS All queries relating to the presentation and sub- mission of papers and any correspondence re- garding accepted papers and proofs should be directed to the Editor or US Editor (addresses as above) Members of the JAAS Editorial Board (who may be contacted directly or v/a the Editorial Office) would welcome comments suggestions and advice on general policy matters concerning JAAS - Fifty reprints are supplied free of charge Journal of Analytical Atomic Spectrometry (JAAS) (ISSN 0267-9477) is published eight times a year by The Royal Society of Chemistry Thomas Graham House Science Park Milton Road Cambridge CB4 4WF UK All orders accompanied with payment should be sent directly t o The Royal Society of Chemistry Turpin Distribution Services Ltd Blackhorse Road Letchworth Herts SG6 1 HN UK Tel +44 (0) 462 672555 Telex 825372 Turpin G Fax +44 (0) 462 480947 Turpin Distribution Services Ltd is wholly owned by The Royal Society of Chemistry 1992 Annual subscription rate EC €347 00 USA $740 00 Canada €408 (excl GST) Rest of World €389 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 t o Journal of Analytical Atomic Spectmmetry (JAASI Publications Expediting Inc 200 Meacham Avenue Elmont NY 11003 Second class postage paid at Jamaica NY 11431 All other despatches outside the UK by Bulk Airmail within Europe Accelerated Surface Post outside Europe PRINTED IN THE UK Q The Royal Society of Chemistry 1992 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 publishersJournal of Analytical Atomic Spectrometry {Including Atomic Spectrometry Updates) JAAS Editorial Board* Chairman B L Sharp (Loughborough UK) J.Egan (Cambridge UK) J M Mermet (Villeurbanne France) S J.Haswell (Hull UK) D A Hickman (London UK) J Marshall (Middlesbrough UK) D L Miles (Keyworth UK) R D Snook (Manchester UK) "The JAAS Editorial Board reports t o the Analytical Editorial Board Chairman A G Fogg (Loughborough UK) JAAS Advisory Board F C Adams (Antwerp Belgium) R M Barnes (Amherst MA USA) L Bezur (Budapest Hungary) R F Browner (Atlanta GA USA) S Caroli (Rome Italy) A J Curtius (Rio de Janeiro Brazin J B Dawson (Leeds UK) M T C de Loos-Vollebregt (Delft The K Dittrich (Leipzig Germany) L Ebdon (Plymouth UK) M S Epstein (Gaithersburg MD USA) Fang Zhao-lun (Shenyang China) W Frech (Umea Sweden) A L Gray(€gham UK) S Greenfield (Loughborough UK) G M Hieftje (Bloomington IN USA) G Horlick (Edmonton Canada) D Littlejohn (Glasgow UK) B V L'vov (Sf Petersburg Russia) T Nakahara (Osaka Japan) Ni Zhe-ming (€?eying China) N Omenetto (lspra Italy) R E Sturgeon (Ottawa Canada) V Sychra (Prague Czechoslovakia) R Van Grieken (Antwerp Belgium) A Walsh K B (Victoria Australia) B Welz (Uberlingen Germany) T S West (Aberdeen UK) Netherlands) A Sanz-Medel (Oviedo Spain) Atomic Spectrometry Updates Editorial Board Chairmarl "D.L. Miles (Keyworth UK) J. Armstrong (Dumfries UK) J. R. Bacon (Aberdeen UK) C. Barnard (Glasgow UIO R. M. Barn-es (Amherst MA USA) S. Branch (High Wycombe UK) R Bye (Oslo Norway) J. Carroll (Middlesbrough UK) M. R. Cave (Keyworth UK) "J. M. Cook (Keyworth UK) "M. S. Cresser (Aberdeen UK) H. M. Crews (Norwich UK) J. S . Crighton (Sunbury-on-Thames UK) J. R. Dean (Newcastle upon Tyne UK) A. W. McMahon (Harwell UK) J M.Mermet ( Villeurbanne France) R. G. Michel (Srorrs CT USA) T. Nakahara (Osaka Japan) Ni Zhe-ming (Belling China) P. R. Poole (Hamilton New Zealand P. J. Potts (Milton Keynes UIO W. J . Price (Ashburton UK) C. J. Rademeyer (Pretoria South Africa) "M. H. Ramsey (London UK) A. Sanz-Medel (Oviedo Spain) "B. L. Sharp (Loughborough UK) I. L. Shuttler (Uberlingen Germany) S. T. Sparkes (Plymouth UK) R.Stephens (Halifax Canada) J.Stupar (Llub/pna Slovenia) R . E. Sturgeon (Ottawa Canada) A. P. Thorne (London UK) G. C. Turk (Gaithersburg MD USA) J. F Tyson (Amherst MA USA) S . J. Walton (Crawley UK) P Watkins (London UN B. Welz ( Uberlingen Germany) J. Williams (Egham UKI J. B. Willis (Victoria Australia) *J. B. Dawson (Leeds UK) "J. Egan (Cambridge UK) *A.T. Ellis (Oxford UIO J. Fazakas (Bucharest Romania) D. J. Halls (Glasgow UK) "A. Taylor (Guildford UK) "D. A. Hickman (London UK) "S. J. Hill (Plymouth UK) K. W. Jackson (Albany NY USA) R. Jowitt (Middlesbrough UK) K. Kitagawa (Nagoya Japan) J. Kubova f Bratislava Czechoslovakd "J. Marshall (Middlesbrough UK) H. Matusiewicz (Poznan Poland) *Members of the ASU Executive Committee Editor JAAS Judith Egan The Royal Society of Chemistry Dr J M Harnly Thomas Graham House Science Park Milton Road Cambridge CB4 4WF UK Telex No 818293 Fax 0223 423623 Beltsville M D 20705 USA E-mail RSCI@UK AC RL GB (JANET) Assistant Editors Brenda Holliday and Ed/tonal Secretary Monique Warner US Associate Editor JAAS US Department of Agriculture Beltsville Human Nutrition Research Center Telephone 0223 420066 BLDG 161 BARC-EAST Telephone 301 -504-8569 Paula O'Riordan Advertisements. Advertisement Department The Royal Society of Chemistry Burlington house Piccadilly London W I V OBN UK Telephone 071-437 8656 Fax 071-494 1134 Information for Authors Full details of how to submit materials for publica tion in JAAS are given in the Instructions to Authors in Issue 1 Separate copies arc available on request The Journal of Analytical Atomic Spectrometry (JAASi is an international journal for the publica- tion of original research papers communications and letters concerned with the development and analytical application of atomic spectrometric techniques The journal is published eight times a year including comprehensive reviews of specific topics of interest to practising atomic spectrosco- pists and incorporates the literature reviews which were previously published in Annual Reports on Analytical Atomic Spectroscopy (ARAAS) Manuscripts inteqded for publication must de- scribe original work related to atomic spectromet- ric anaiysis Papers on all aspects of the subject will be accepted including fundamental studies novel instrument developments and practical ana- lytical applications As well as AAS.AES and AFS papers will be welcomed on atomic mass spec trometry and X-ray fluorescence/emission spec trometry Papers describing the measurement of molecular species where these relate to the char- acterization of sources normally used for the pro duction of atoms or are concerned for example with indirect methods of anaiysis will also be ac- ceptable for publication Papers describing the de velopment and applications of hybrid techniques ( e g GC-coupled AAS and HPLC-ICP) will be par ticularly welcome Manuscripts on other subjects of direct interest to atomic spectroscopists. in- cluding sample preparation aqd dissolution and analyte pre-concentration procedures as wet' as the statistica irterpretation and use of atomic spectrometric data will also be acceptable for pcib- lication There is no page charge The following types of papers will be consid- ered Full papers describing original work Commun/cations which must be on an urgent matter and be of obvious scientific irnportance Communications receive priority and are usually published within 2-3 months of receipt They are Intended for brief descriptions of work that has progressed to a stage at which it is likely to be valuable to workers faced with similar problems Reviews which must be a critical evaluation of the existing state of knowledge on a particular facet of analytical atomic spectrometry Every paper (except Communications) will be submitted to at least two referees by whose advice the Editorial Board of JAAS will be guided as to its acceptance or rejection Papers that are accepted must not be published elsewhere except by permission Submission ot d manu- script will be regarded as an undertaking that the sahe material is not being considered for publica- tion by another journal Manuscripts (three copies typed In double spacing) should be sent to Judith Egan Editor JAAS or Dr J M Harnly US Associate Editor JAAS All queries relating to the presentation and sub- mission of papers and any correspondence re- garding accepted papers and proofs should be directed to the Editor or US Editor (addresses as above) Members of the JAAS Editorial Board (who may be contacted directly or v/a the Editorial Office) would welcome comments suggestions and advice on general policy matters concerning JAAS - Fifty reprints are supplied free of charge Journal of Analytical Atomic Spectrometry (JAAS) (ISSN 0267-9477) is published eight times a year by The Royal Society of Chemistry Thomas Graham House Science Park Milton Road Cambridge CB4 4WF UK All orders accompanied with payment should be sent directly t o The Royal Society of Chemistry Turpin Distribution Services Ltd Blackhorse Road Letchworth Herts SG6 1 HN UK Tel +44 (0) 462 672555 Telex 825372 Turpin G Fax +44 (0) 462 480947 Turpin Distribution Services Ltd is wholly owned by The Royal Society of Chemistry 1992 Annual subscription rate EC €347 00 USA $740 00 Canada €408 (excl GST) Rest of World €389 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 t o Journal of Analytical Atomic Spectmmetry (JAASI Publications Expediting Inc 200 Meacham Avenue Elmont NY 11003 Second class postage paid at Jamaica NY 11431 All other despatches outside the UK by Bulk Airmail within Europe Accelerated Surface Post outside Europe PRINTED IN THE UK Q The Royal Society of Chemistry 1992 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/JA99207FX031

出版商:RSC    

年代:1992

数据来源: RSC

摘要:

JASPE2 7 ( 8 ) 53N-62N 11 57-1 306 349R-412R ( 1 992) December 1992 Journal of Analytical Atomic Spectrometry Including Atomic Spectrometry Updates CONTENTS NEWS AND VIEWS 53N 60N Conferences and Meetings 61 N Conference Reports-Mike Hinds Kenneth Jackson Phil Riby Stuart Chalk Judith Egan Papers in Future Issues PAPERS 11 57 - Investigations into the Application of Methane Addition to the Nebulizer Gas in Inductively Coupled Plasma Mass Spectrometry for the Removal of Polyatomic 1167 1173 1183 1187 1195 1201 1207 1221 1231 1239 1243 1249 1253 1257 1273 1281 1287 Interferences-Steve J Hill Michael J 'Ford Les Ebdon Anion Exchange for the Elimination of Spectral Interferences Caused by Chlorine and Sulfur in Inductively Coupled Plasma Mass Spectrometry-Jan Goossens Richard Dams Multi-element Detection for Supercritical Fluid Chromatography by Inductively Coupled Plasma Mass Spectrometry-Jeffrey M Carey Nohora P Vela Joseph A Caruso Simultaneous Determination of Antimony Arsenic and Selenium in Natural Waters by Means of Hydride Generation Coupled to ..Plasma Source Mass Spectrometry-Conny Haraldsson Marianne Pollak Peder Ohman Semiquantitative Analysis of Environmental Materials by Laser Sampling Inductively Coupled Plasma Mass Spectrometry-Eric R Denoyer Determination of Trace Impurities in Tantalum Oxide and Niobium Oxide by Laser Ablation Inductively Coupled Plasma Mass Spectrometry-Stan T G Anderson Robbie V D Robert Humphrey N Farrer Analysis of Samples Containing Large Amounts of Dissolved Solids Using Microsampling Flow Injection Inductively Coupled Plasma Mass Spectrometry-Adreas Stroh Uwe Vollkopf Eric R Denoyer Deviation of the Level Populations of Iron Atoms and Ions From the Boltzmann Distribution in an Inductively Coupled Plasma.Part 1. Spatial and Power Dependences-Kuniyuki Kitagawa Gary Horlick Deviation of the Level Populations of Iron Atoms and Ions From the Boltzmann Distribution in an Inductively Coupled Plasma. Part 2. Effect of an Easily Ionizable Element-Kuniyuki Kitagawa Gary Horlick Role of Auxiiiary Gas Flow in Organic Sample Introduction With Inductively Coupled Plasma Atomic Emission Spectrometry-Changkang Pan Guangxuan Zhu Richard F Browner Determination of Lead in Sea-water by Inductively Coupled Plasma Atomic Emission Spectrometry Com bined With Chelating Resin Preconcentration and Hydride Generation-Raul A Reimer Akira Miyazaki Flame Sample Introduction System for Inductively Coupled Plasma Atomic Emission Spectrometry-Vassili Karanassios L Usypchuck P Moss Eric D Salin Direct Determination of Aqueous Carbon Phosphorus and Sulfur Using a Kilowatt- plus Helium Microwave-induced Plasma System With Ultrasonic Nebulization-Mingin Wu Jon W Carnahan Electrothermal Vaporization and Ultrasonic Nebulization for the Determination of Aqueous Sulfur Using a Kilowatt-plus Helium Microwave-induced Plasma-Jorge Alvarado Mingin Wu Jon W Carnahan Palladium Nitrate-Magnesium Nitrate Modifier for Electrothermal Atomic Absorption Spectrometry.Part 5. Performance for the Determination of 21 Elements-Bernhard Welz Gerhard Schlemmer Jayateerth R Mudakavi Analytical Characteristics in Electrothermal Atomization Studies of Cadmium Copper Germanium.Molybdenum Lead and Vanadium From Pyrolytic and Tungsten Coated L'vov Platforms by Atomic Absorption Spectrometry-Zully Benzo Claudio Cecarelli Nereida Carrion. Maria A Alvarez Carlos Rojas Marrela Rosso Determination of Lead and Aluminium in Port Wine by Electrothermal Atomic Absorption Spectrometry-Agostinho A Alrneida M Lourdes Bastos M Isabel Cardoso Margarida A Ferreira Jose L F. C Lima M Elisa Soares Determination of Iron Cobalt Nickel and Copper in a Zirconium-based Glass by Electrothermal Atomic Absorption Spectrometry-James Jaganathan Kenneth J Ewing lshwar Aggatwal continued on inslde back cover Typeset by Burgess Thames View Abingdon Oxfordshire Printed in Great Britain by age Bros Norwich L K R O S ) 0267-9477 I 1992 1 8 - X1291 On-line Dilution System for Extending the Calibration Range of Flame Atomic Absorption Spectrometry-lgnacio Lopez Garcia Jeslis Arroyo Cortez Manuel Hernandez Cordoba 1295 Coupling of a Continuous Liquid-Liquid Extractor t o a Flame Atomic Absorption Spectrometer for the Determination of Alkaloids-Marcelina Eisman Mercedes Gallego Miguel Valcarcel COMMUNICATION 1299 Long-term Stability of a Mixed Palladium-Iridium Trapping Reagent for In Situ Hydride Trapping Within a Graphite Electrothermal Atomizer-Ian L Shuttler Michaela Feuerstein Gerhard Schlemmer 1303 ERRATA 1305 CUMULATIVE AUTHOR INDEX ATOMIC SPECTROMETRY 349R Industrial Analysis Metals Chemicals and Advanced Materials-John Marshall UPDATE John Carroll James S Cnghton Charles L R . Barnard 389R References I FACSS Announcement and Call for Papers

ISSN:0267-9477    

DOI:10.1039/JA99207BX033

出版商:RSC    

年代:1992

数据来源: RSC

摘要:

JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY DECEMBER 1992 VOL. 7 53N Conference Reports Second Rio Symposium on Atomic Absorption Spectrometry June 21 -24 1992 Rio de Janeiro Brazil At the close of the First Rio Sympo- sium conference co-organizer Profes- sor Adilson Curtius indicated that in 1992 there would be a Second Rio Symposium. Indeed this has occurred! Through the efforts of Professor Cur- tius and Dr. Bernhard Welz the Sec- ond Rio Symposium began on June 21 with a reception amid the tropical grounds of the Pontificia Universi- dade Catolica do Rio de Janiero (PUC-Rio). The symposium was divided into two parts. The first part titled ‘Atomic Absorption Spectrometry Furnace Flame and Hydride Techniques’ at- tracted 156 people. This was held at PUC-Rio from June 21-24 in a lec- ture theatre providing simultaneous translation from English into Portu- geuse.Opening remarks were given by Adilson Curtius and the co-organizer Bernhard Welz. Professor G. Knapp (Graz University of Technology Aus- tria) gave the first lecture on advances in sample preparation for trace metal analysis. Dr. D. Batistoni (National Atomic Energy Commission Argen- tina) reviewed the research done on the distribution of analytes in flames. This was followed by Dr. G. Schlem- mer’s (Bodenseewerk Perkin-Elmer GmbH Germany) discussion of new possibilities for FAAS through flow injection techniques and by precise stepper-motor control of the burner position with respect to the light path. There were a number of presenta- tions on ETAAS. A review of the STPF concept was presented by D.Bradshaw (Perkin-Elmer USA). Modifiers were discussed by Professors Ken Jackson (New York State School of Public Health USA) and R. A. Romero (Univeridad del Zulia Venezuela). Different methods to extend the linear range of Zeeman ETAAS determina- tions were presented by Professor Boris L‘vov (St. Petersburg Technical University Russia) and Dr. M. T. C. de Loos-Vollebregt (Delft University of Technology The Netherlands). These appear to be simple and easy to implement and we hope they will be used in commercial instruments. Two examples of different approaches to Professor Boris L’vov (L) and Dr. Adilson Curtius (Conference Organizer) at the Wel- come Reception Following this talk there were more presentations on flow injection atomic absorption spectrometry advances from Dr.F. J. (Chico) Krug (Centre of Nuclear Energy and Agriculture Pira- cicaba Brazil) Dr. Michael Sperling (Bodenseewerk Perkin-Elmer GmbH Germany) Professor Zhao-lun Fang (Institute of Applied Ecology Sheny- ang China) Glen Carnrick from Per- kin-Elmer USA (on behalf of W. S h i n and J. TYson) and L. c. Azer- edo (Federal Rural University of Rio de Janiero Seropedica Brazil). China) Dr. Michael Sperling (Perkin-Elmer Ger- many) and Dr. Zhao-lun Fang (Shenyang (L to R) Professor Jim Holcombe (Austin TX USA) Dr. Nancy Miller-lhli (USDA Beltsville MD USA) Judith Egan (Cam bridge UK) Dr Ken Jackson (Albany NY USA) Jan Date (Cambridge UK) Lecture theatre with some participants appreciating the simultaneous and Anstace Monk (British Council Rio de Janeiro Brazil) translation of all lectures into Portuguese54N JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY DECEMBER 1992 VOL.7 trace metal determination in kerosene and biological samples by ETAAS were given by Professor Curtius (PUC- Rio) and Dr. G. Schlemmer respec- t ivel y . Hydride generation and cold vapour’ techniques for the determination of mercury were discussed in presenta- tions by a representative from Varian Professor C. G. Bruhn (University of Concepcion Chile) and Dr. R. Cam- pos (PUC-Rio). An overview of mer- cury species determination was given by Dr. Wolfgang Frech (University of UmeA Sweden) with attention given to GC-AAS and GC-ICP-AES tech- niques. Arsensic determination by hy- dride generation with flow injection was discussed by Dr.M. T. C. de Loos- Vollebregt. The better part of a day dealt with solid sample analysis by ETAAS. Talks included recent advances using the introduction of weighed solid samples (Dr. M. Hinds Royal Canadian Mint) slurried samples (Dr. N. Miller-Ilhi US Department of Agriculture USA and D. Bradshaw) solids sputtered onto a platform (Dr. G. Muller-Vogt Universitat Karlsruhe Germany) and laser ablation in concert with ETAAS (Professor K. Dittrich University of Leipzig Germany). Professor G. Hermann (University of Giessen Germany) gave an excel- lent overview of coherent forward scattering atomic spectroscopy which was valuable in broadening the scope of the symposium. A poster session was also held. Thirty posters were displayed that covered a range of applications and prompted some interesting discussions during both the formal poster viewing and the organized discussion period that followed.Two courses were also held during the first part of the symposium. The first was on cation and anion determi- nations by spectroscopic techniques. The second focused on determination of trace and ultratrace elements. Over 80 participants who attended both the courses and the symposium talks set a gruelling pace for themselves. Dr. Albert Gilmutdinov (Kazan Russia) (L) and Dr. Ralph Sturgeon (Ottawa Canada) at the end of the Symposium in Buzios Following the conference sessions many participants took the time to tour the sights of Rio the beaches (and bathers) the views from Sugar Loaf and Corcovado and the exotic night- life.The conference dinner was a high- light with a Brazilian style barbeque. A wide variety of meats were served by waiters brandishing squewered por- tions of meat on sword-like spits. Portions of meat were sliced off onto your plate then the server rushed off to the next person. Dinner passed pleas- antly with no one being impaled. A small but lively samba band played during the meal and then kicked into high gear for three samba dancers. The dancers were quite lively and encour- aged audience participation as Bern- hard Welz and Boris L’vov dis- covered!! ! The second part devoted to Furnace Atomic Absorption Spectrometry took place at the exotic Nas Rocas Hotel from June 26-28. The hotel and environs were situated on and cov- ered a small tropical island in the resort area of Buzios (1 54 km north of Rio de Janiero).The session began with talks on flow injection ETAAS by Dr. G. Schlem- mer and Dr. 2. Fang. In another lecture Dr. B. Welz described how chloride volatilization from the fur- nace was monitored by an emission technique. The reality of absolute ana- lysis by ETAAS was discussed by G. Carnrick. Further research on temper- ature measurements inside the graph- ite furnace by CARS thermometry was presented by Dr. M. Sperling. Alternate uses for graphite furnace atomizers were advanced. Dr. R. Stur- geon (National Research Council Canada) gave an update on his furnace atomization plasma emission spectro- metry (FAPES) research and Professor G. Hermann discussed coherent for- ward scattering with a graphite atom- izer.Professor K. Dittrich gave an overview of how graphite furnace atomizers can be used as a sample introduction system for a variety of atomic spectrometry techniques. Probe atomization AAS was dis- cussed by Dr. J. Alvarado (Universi- dad Simon Bolivar Caracus Vene- zuela). Dr. F. J. Krug and Dr. C. G. Bruhn presented a series of talks on the use of the tungsten coil atomizer which appears to be a less expensive approach to determining some trace elements. The last day was devoted to funda- mental atomization studies. Professor L’vov began the session by discussing the effects of particles condensing within the analytical volume during atomization. Dr. V. Majidi (Univer- sity of Kentucky USA) showed how Rutherford back scattering can be used to probe reactions on the graphite surface.Dr. W. Frech discussed his group’s work on elucidating a mecha- nism for the A1 spikes phenomenon. Work on determining how oxygen pre- treatment affects atomization was pre- sented by Dr. G. Muller-Vogt. Dr. D. Rojas (Universidad de Los Andes Merida Venezuela) gave an interest- ing talk on her approach to studying the effects of heating rate on atomiza- (L to R) Dr. German Muller- Vogt (Kalsruhe Germany) Professor Klaus Dittrich (Leipzig Germany) Dr. Bernhard Welz (Perkin- Elmer Germany) and Dr. Gerd Hermann (Giessen Germany) at PUC International soccer game in BuziosJOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY DECEMBER 1992 VOL. 7 55N Delegates enjoying the conference dinner tion. Professor Albert Gilmutdinov (University of Kazan Russia) pre- sented two papers in which the distri- bution of analytes and other species within the atomizer was examined by spectral shadow filming and computer modelling.Dr. Dave Styris (Battelle- Pacific Northwest Laboratory USA) presented an atomization mechanism for tin using mass spectrometry. Pro- fessor Jim Holcombe (University of Texas USA) had the last word with his talk on the potential for direct solid analysis via low-pressure ETAAS. Although there was an interesting scientific programme participants managed to pull themselves away to enjoy the resort’s many activities swimming sailing kayaking sun bath- ing and lounging at the pool-side bar. The organizers were kind enough to reschedule the programme to permit a free afternoon for everyone to enjoy the sun and wear off the many calories acquired by the feasting from the well laden buffet tables.A soccer game was organized and pitted participants from Brazil against everyone else. Dr. Rein- aldo Campos led Team Brazil to a decisive and inevitable victory over Team Rest of the World. The resort bar was the main evening venue where hotel organizers staged lots of samba dancing and a variety of contests. The newly formed singing group Albert and Boris from Russia (A. Gilmutdinov and B. L‘vov) won the singing contest with second and third place going to Gerhard Schlem- mer and the participants from Argen- tina respectively. While in Brazil many of us imbided ‘caipirinha’ a local drink made from cachasa a sugar cane distillate and limes. A contest was held to see who could make the best caipirinha.Chico Krug’s recipe won the competition. He has agreed to share his recipe with us Take 1 of a tahiti lime and cube. Place the cubed lime in a 250 ml glass and add 1 tablespoon of sugar (or to taste). Press and mix the lime and sugar then add 50 ml of cachasa. Fill the glass with small pieces of ice and mix well. Chico advises that samba music should be playing and preparation should be done whilst rotating hips at a fre- quency of 2 Hz. For those without a ready supply of cachasa vodka can be used in its place to make ‘caipiroska’. Professor Adilson Curtius Dr. Bern- hard Welz and their organizing com- mittee did an outstanding job of hosting the Second Rio Symposium. Looking ahead the organizing com- mittee have embarked on an ambi- tious plan to expand the symposium to cover all areas of atomic spectrometry and to hold this symposium every two years in various South American centres. The next ‘Rio Symposium’ will be in Caracas Venezuela and will be organized by Professor J.Alvarado. We look forward to the next meeting. Mike Hinds Royal Canadian Mint 320 Sussex Drive Ontario Canada KIA OG8 Kenneth Jackson New York State Department of Public Health and School of Public Health Some of the delegates as everyone said farewell Albany NY USA Sixth Biennial National Atomic Spectroscopy Symposium (BNASS) July 22-24 1992 Plymouth UK The BNASS Conference Report 2-The Sequel. After the success of the 5th BNASS at Loughborough the story continues. A further tale of science and socializing.The setting downtown Plymouth a city under siege from world renowned atomic spectro- scopists and a number of us who were allowed in by mistake! At the opening ceremony on Wednesday afternoon Professor Les Ebdon (University of Plymouth) wel- comed the delegates to the newly re- named University of Plymouth and wished them a successful conference before handing over control of the event to Dr. Steve Hill (University of Plymouth). It seemed appropriate that the first plenary lecture of this meeting should be presented by Professor L’vov (Saint Petersburg Technical University) a man as Steve Hill said who really didn’t need an introducton to this audience. Professor L‘vov’s presentation dealt with the extension of dynamic range and linearization of calibration graphs in Zeeman graphite furnace atomic absorption spectrome- try.The dip in the absorption peak maximum resulting from the roll-over of the calibration curve was restored using a computer program. Following this informative presenta- tion the lectures were divided into two streams for the rest of the afternoon. This of course led to the usual problem56N JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY DECEMBER 1992 VOL. 7 of attempting to be in two places at one time. Stream A or as it became known the Strathclyde University and associ- ates group saw an invited lecture from Professor Littlejohn (University of Strathclyde) on the effect of chemical modifiers on the analysis of boron and silicon by ETAAS. The release of boron at temperatures as low as 1200 “C was a matter for some discussion since B203 is not normally released until above 1500 “C.Contributed lectures were also presented in this session by Dr. Ian Shuttler (Bodenseewerk Perkin-Elmer GmbH) ‘Extending the dynamic range of ETAAS measurements’ Dr. Jim Harnly (United States Department of Agriculture) ‘Continuum source AAS with a pulsed xenon arc lamp and a linear photodiode array detector’ and Dr. Robbin Nichol (University of Strathclyde) ‘Assessment of linear photodiode array detection for con- tinuum source atomic absorption spec- trometry with electrothermal atomiza- tion’. Stream B had the second invited lecture of the meeting from Dr. Cam- eron McLeod (Sheffield Hallam University) entitled ‘Field sampling and flow injection strategies for trace analysis and element speciation’.The contributed lectures came from Dr. Graeme Spiers (University of Guelph) ‘Multiline determinations for niobium in carbonite-hosted minerals utilizing a photodiode array equipped ICP-AES spectrometer’ Dr. P. Shaw (Varian) ‘The use of an intelligent automatic quality control protocol to obtain relia- ble data from an unattended high productivity sequential ICP-OES’ and Dr. A. T. Ince (DIAS UMIST) ‘Noise in atomic emission spectroscopy’. With the completion of the first round of lectures the delegates retired for some alcohol based refreshment and a chance to have a leisurely look at the posters. The posters considered a wide field of work including ICP ICP-MS laser ablation ETAAS and chromato- graphic separation and preconcentra- tion techniques.The evening was left free for the delegates to enjoy Plymouth and test some of their most excellent hostelries. Thursday started with Professor Mike Blades (University of British Columbia) presenting his plenary lec- ture entitled ‘Development and char- acterization of new optical and mass spectrometric methods for trace ele- ment analysis’. The use of furnace atomization plasma excitation spec- trometry (FAPES) as a technique for multi-element picogram range deter- minations was discussed as well as some exciting developments in the field of laser ablation with ion trap mass spectrometry. Again the lectures were split into two streams with the first invited lectures of the day coming from two familiar faces on the confer- ence scene Professor H. Falk and Professor J.Tyson. Professor Falk (Spectro Analytical Instruments) dis- cussed extreme limits of elemental detection using optical and mass spec- trometries. The discussion centred on single atom determination with re- spect to both trapping of the species and the use of time of flight mass spectrometry. Professor Tyson (University of Massachusetts) dis- cussed the use of flow injection mani- folds to produce on-line digestion of samples. After a break for coffee and a chance to try and absorb all of this information we were back to three contributed lectures in each stream. In stream A there was a contribution from Dr. E. B. M. Steers (University of North London) discussing the use of a high-resolution Fourier transform spectrometer for the study of glow discharges.There were also two X-ray fluorescence presentations one by Dr. P. J. Potts (The Open University) on the analysis of Rb and Sr using energy dispersive and wavelength dispersive fluorescence and the second by Dr. Steve Haswell (University of Hull) on trace element determinations in clini- cal samples by total reflection X-ray fluorescence (TXRF). Alternatively the delegates were treated to presenta- tions on china clay production control by DCP-AES by B. Fairman (Univer- sity of Plymouth) preconcentration and determination of gold by ICP using a microcolumn of sulfhydryl cotton and cyanide as an eluant by M. Gomez (Sheffield Hallam University) and finally characteristics of a helium discharge in HA-FANES by Dr. Phil Riby (University of Greenwich). Lunch time for a few relaxing mo- ments before the afternoon onslaught. The second plenary lecture of the day was presented by Dr.Barry Sharp (Loughborough University of Techno- logy) entitled ‘Samples signals and noise in inductively coupled plasma spectrometry’ and discussed the ori- gins of noise in ICP and the use of signal processing and system improve- ment to minimize it. The two invited lectures of the afternoon saw Dr. Steve Hill discussing the introduction of organic solvents into ICP-MS using desolvation membrane separators and a cooled spray chamber while Profes- sor Peter Stockwell (PS Analytical) discussed vapour generation and atomic fluorescence. Of the six contri- buted lectures in the afternoon sample introduction and desolvation was the subject of Dr.Alan Eastgate (Applied Research Laboratories) while the ad- vantages of ETV-ICP-MS for Pu deter- mination in urine and laser ablation for the determination of trace ele- ments in silicates were presented by Dr. Ros Cox (Atomic Energy Author- ity) and Dr. Bill Perkins (University of Wales) respectively. Professor Ian Brindle (Brock University) presented some work indicating the reduction of noise possible in hydride generation by the use of Kalman filtering while Dr. Morris dancing in the Great Tythe Barn at Buckland AbbeyJOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY DECEMBER 1992 VOL. 7 57N Phil Goodall (University of Plymouth) presented an alternative to traditional vapour generation techniques by the production of volatile Cd species from sodium tetraethylborate. The final pre- sentation of the day came from this years Kirkbright Bursary winner Eve- lyn Su (University of Connecticut) who presented work on the analysis of chlorine by graphite furnace laser ex- cited molecular fluorescence spectro- metry of indium monochloride.Before the exciting evening’s entertainment chance to imbibe and observe the final poster offering which included a num- ber of posters on ETAAS ICP-MS glow discharge chemometrics flow injection microwave introduction and of course slurry nebulization (well this was Plymouth after all!!). Thursday evening and the most legendary event of any BNASS meet- ing the conference dinner-many go but few escape unscathed!! This year the organizers selected venue was the Great Tythe Barn at Buckland Abbey.This had been a 13th century monast- ery (a rather ironic location for a BNASS conference dinner) although from 1581 it was the home of Sir Francis Drake however there wasn’t a single bowling green!! There was chance to enjoy a glass of elder flower wine and to take a walk round the grounds. The meal turned out to be most enjoyable especially with the company round the table (names have been deleted to protect the innocent). For those of us who were at the Loughborough meeting it came as no surprise that the after dinner enter- tainment was provided by Dr. Steve Haswell although it was somewhat of a shock to see him remove his trousers in front of the delegates fortunately he was wearing his Morris dancers attire underneath. The first part of the per- formance featured Steve telling a few jokes and singing (don’t give up the day job Steve!).With the help of the local Morris men a tradition Grego- rian chant was performed. It is funny really I never thought that Gregorian monks hit themselves over the head with BNASS document cases spon- sored by PS Analytical you learn something new everyday at this meet- ing The Morris dances were com- pleted with the involvement of Dr. Steve Hill who kindly offered to per- form. Was it true that Dr. Haswell had taught him a dance earlier and had changed it during the performance without telling him? This will not be revealed at present but it certainly would explain why Dr. Hill looked so concerned to end up in the centre of a group of men wielding sticks. The evening finished with a sampling of the local brew obviously a truly represen- tative sample had to be taken! Dr.Steve Hill (L) taking instructions in the art of Morris dancing from Dr. Steve Haswell (R) Fellow survivors of Thursday night’s excesses saw Professor Malcolm Cres- ser (Aberdeen University) present the fourth plenary lecture entitled ‘Atomic spectroscopy in environmental analy- sis-jam today or jam tomorrow?’ on Friday morning. This proved to be a very entertaining lecture as Professor Cresser used quotes from his former students while describing the develop- ment of atomic absorption spectros- copy with respect to environmental analysis. One of the more memorable quotes was ‘AA is a funny old techni- q u e . . . ~ ~ ~ spend hours and hours trying to digest things that don’t’.This seemed to show remarkable insight for an undergraduate. The two invited lectures ofthe morn- ing were presented by Professor Allan Ure (University of Strathclyde) ‘Chemistry of on-line preconcentration of aluminium gallium and indium ions with immobilized 8-quinolinol’ and Dr. Jim Crighton (BP Research) who described the construction of a heated GC-ICP interface for the analysis of poly(organosi1oxanes). The heated transfer line had originally caused problems since the plasma had trav- elled along the stainless-steel sheath and into the control box (this sounded particularly impressive). The problem was rectified by not connecting the heater supply until after the plasma had been ignited. The contributed papers of the morn- ing came from Dr. Charles Barnard (Glasgow Polytechnic) ‘Speciation of aluminium complexes with neurologi- cal ligands using atomic spectrometric detection’ Dr.Dave Barclay (CEM Microwave Technology) ‘The applica- tion of an on-line microwave digestion sample preparation procedure to multi-element determinations in atomic spectroscopy’ and Dr. Simon Apte (CSIRO) ‘Rapid determination of trace metals in saline waters by semi-micro solvent extraction graphite furnace AAS’. In stream B Dr. Mike Thompson (Birkbeck College) dis- cussed sampling theory preconcentra- tion laser ablation atomic spectrome- try chemometrics hostile environ- ments and man’s lust for gold. Dr. Mark Cave’s (British Geological Sur- vey) lecture described the use of prin- cipal components analysis (PCA) to investigate the factors controlling long term calibration drift in sequential ICP-OES while in the final lecture of the morning Dr.Robert Fry (Applied Research Laboratories) described the design of a high resolution Cchelle spectrometer. This produced a resolv- ing power of 5 pm (FWHM) at 228 nm. A break for lunch allowed everyone a chance to discuss the mornings pre- sentations before returning for the final session. The first of two plenary lectures of this session was presented by Professor K. Niemax (ISAS) who dealt with element analysis by laser ablation of solid samples. The work concentrated on the use of buffer gases to improve reproducibility. The in- vited lectures of the afternoon featured Dr. John Williams (Royal Holloway and Bedford New College) presenting an overview of ICP-MS with particular reference to the uses of isotope ratio analysis and Dr.Gerhard Schlemmer (Perkin Elmer GmbH) who discussed the use of flow injection techniques with electrothermal atomization. This lecture considered a technique which has received a lot of attention in recent years preconcentration-matrix separ- ation using microcolumns as well as trapping of hydride-forming elements. In line with the ICP-MS theme of stream A Dr. Maryanne Thomsen (Perkin-Elmer Ltd.) presented a paper entitled ‘Isotope ratio and isotope di- lution measurements in standard ref- erence materials using ETV-ICP-MS’. The final contributed paper in this stream came from Jim Hartley (University of Plymouth) and consi- dered the use of desolvated slurries as an introduction technique for ICP- MS.Meanwhile in stream B the graph- ite furnace enthusiasts had the oppor- tunity to listen to presentations by Dr. D. J. Halls (Glasgow Royal Infirmary)58N JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY DECEMBER 1992 VOL. 7 on the analysis of arsenic in urine and hair and by Dr. D. J. Burrell (MAFF Food Science Laboratory). Dr. Burrell made an attempt to convince the delegates that drinking was bad for you by discussing the analysis of lead in beer and wine and discussed the leaching of lead from crystal glasses into wine port and whisky. In order to encourage everyone to stay until the end of the meeting the final plenary lecture was indeed the final lecture of the meeting and was presented by Dr. Jim McLaren (National Research Council of Canada).This lecture featured analysis of fresh and saline reference waters using ICP-MS and was an enjoyable end to what had been an extremelyinforma- tive meeting. The final part of the technical programme were the awards for best student poster and oral presen- tation. The judges had a difficult time selecting the winners but in the end the prizes were given to Rosamund Cox (Atomic Energy Authority) for her presentation on the analysis of Pu in urine by ETV-ICP-MS and to Alexis Holden (University of Strathclyde) for her poster on silicon atomization. With the meeting closed the remain- ing delegates departed for the final social event of the week. The evening started with a cruise on the river Tamar. A chance to see the royal dockyard-was it true that the crane at the dockyward was used for removing nuclear cores from submarines or as was suggested on the boat for moving a well known editors luggage? After the cruise it was off to the Plymouth Dome to enjoy an interactive version of the history of Plymouth.A hardy bunch of conference golers decided to walk back to the University while visiting some of the more cultural purveyors of beers in the local area. This proved to be most entertaining since some of the more astute locals rapidly worked out that Mike Blades was not indeed English and drew our attention to the fact that the person sitting in the group was not as we thought Colin Watson but was indeed the lead singer of ZZ Top. It is amaz- ing what these famous people will do to sneak into our meetings. A small group were still enjoying themselves into the early hours of the morning after what had proved to be another very successful BNASS meeting.On behalf of all the delegates I would like to take this opportunity to thank the organizing committee who yet again did a superb job. I would also like to thank all the sponsors espe- cially those who were involved in the sponsorship of student bursaries (ASU ICI Wilton Materials Research Centre and Starna) without whom many of the students would not have have been able to attend. Phil Riby University of Greenwich Woolwich London UK SE18 Plenary lecturers. (L to R) Professor Malcolm Cresser (Aberdeen University); Dr. Kay Niemax (Institut fu’r Spektrochemie und an- gewandte Spektroskopie); Dr. Barry Sharp (Loughborough University of Technology); Professor Mike Blades (University of British Colum- bia); Professor Boris L ’vov (Saint Petersburg Technical University); and Dr.Jim McLaren (Natural Research Council of Canada) Delegates disembarking after a cruise on the Tamar Federation of Analytical Chemistry and Spectroscopy Societies (FACSS) XIX September 20-25 1992 Philadelphia PA USA Starting graduate school I thought ‘This is going to be hard but I can handle it’. Overall that has been the case but of the things I have really had to get used to attending conferences has been the one that felt very weird. The Federation of Analytical Chemistry and Spectroscopy Societies conference 1992 was the first time I had attended a whole conference. For- tunately it was not the first I had participated in. I presented a poster at the Pittsburgh conference 199 1 in Chi- cago IL but that was very hectic very big and I was only there for a few days.This year’s FACSS meeting showed me that hob-knobing with my peers is not so difficult after all. I arrived by train on the Friday before the conference so that I could attend one of the Society for Applied Spectroscopy’s short courses. Two days of lectures on Modern Graphite Furnace AAS made me appreciate it’s capabilities for the analytical labora- tory. The course was well put together and very enjoyable. It is a testament to the enthusiasm of the instructors that all the participants stayed awake through the lectures! Then came the main business of the week. The 79 1 papers and posters were presented over four and a half days. To say that there was enough to see is an understatement.At least six different streams running concurrently each morning and afternoon meant that the hardest part was choosing which stream to see. Many folks decided to just sit in one stream but I found many lectures of interest in different streams and so drifted from place to place. With so many different topics being discussed it was sometimes diffi- cult to focus on what people wereJOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY DECEMBER 1992 VOL. 7 59N talking about so I found the abstract book invaluable even after the lecture. It is difficult here to include all the interesting topics but a few that de- serve a mention are Adaptive Kalman Filtering Atomic Force Microscopy Neural Networks Gas Chromatogra- phy-Atomic Emission Detection Slur- ries for Graphite Furnace AAS Fiber- optic Spectrometers Flow Injection Analysis and Computer Simulations of Real Instruments. Needless to say by the end of the week I was tiring but the anticipation of my own presentation on Friday morning certainly kept my adrenaline high.It went without incident and Evelyn Guizhen Su winner of the FACSS Student Award with Professor Bob Michel her supervisor. Evelyn also received the Gordon F. Kirkbright Bursary A ward which enabled her to attend BNASS in Plymouth UK in Jury 1992 although it was not my best presenta- tion I am beginning to realize that it is getting up there and communicating to people about the fun stuff you have done is really what matters. Apart from the serious business of sharing knowledge and in the case of the exhibition selling instruments much time was spent talking with what I can now call my colleagues in the analytical community. This was primarily achieved at the morning and afternoon breaks where copious amounts of tea coffee and soft drinks were served.In addition many people relieved themselves of conference stress by enjoying the cheese and wine laid on each afternoon by some of the exhibitors where sufficient aqueous/ organic solution was consumed to float the QEII (without it’s hole)! Unfortunately the location of the Adams Mark hotel did not lend itself to much evening social activity al- though I did manage to see downtown albeit fleetingly. A group of us found one of the famous Bookbinder restau- rants which I recommend as long as the bill is on the company.For the most part attendees stayed at the hotel in the evenings with its two restaurants and nightclub which was comple- mented by the local Dennys and TGIFs. As you can probably tell from this commentary I had a really good time at FACSS 1992. I met many new Dr. Ed Brame (L) and Dr. Hardy Hoegger exhibits organizers. Ed was a co-founder of FACSS in 1968 and has been involved with the organization since then. From 1986- 1992 he was Exhibits Director people (including Judith Egan who urged me to write this) and was able to put a lot of faces to names that I knew from the literature. My thanks go out to Deborah Bradshaw Susan McIn- tosh Walter Slavin Nancy Miller-Ihli Judith Egan Mitch Johnson Ed Voigtman Eileen Skelly-Frame the rest of the Tyson research group and especially Julian Tyson for making that week in September one I will never forget.I would also like to thank the SAS for the award to attend the short course on Modern Furnace AAS. Stuart Chalk University of Massachusetts Amherst MA USA Memorial Symposium for Peter Keliher (FACSS) September 20 1992 Philadelphia PA USA As Peter Keliher had been so actively involved in the FACSS organization having served on the Governing Board (including a term as chairman) as an assistant programme chair and as the exhibits director it was appropriate to honour his memory particularly as the meeting had returned to the Philadel- phia area. Dr. Julian Tyson the symposium organizer had invited representatives of the many areas in which Peter had been involved to take part from the analytical research community in- cluding colleagues collaborators and students as well as contributors co- authors and editors from the areas of publishing in which Peter had been so active.The following organizations had been very generous with sponsor- ship amounting to just over $2000 Academic Press; American Chemical Society American Microchemical So- ciety; Atomic Spectrometry Updates (RSC); and the Chemistry Depart- ment Villanova University. Dr. Joe Brenner (Geological Survey Israel) was an external Ph.D. exam- iner for Villanova and is a Member of the Editorial Board of The Micro- chemical Journal and hence had close links with Peter. He opened the ses- sion with a fitting tribute followed by a lecture entitled ‘Composition of Phy- sical and EIE Effects due to High Concentrations of Ca Mg Na and Li for Ultrasonic Nebulization.’ The editorship of The Microchemi- cal Journal is now in the hands of Dr.Joe Sneddon (McNeese State Univer- sity LA USA) who gave the next paper on ‘Studies on an Excimer Laser Ablated Plasma.’ When Dr. Sue Franz (Spectro Inco- porated Fitchburg MA USA) arrived in the US to study for her Ph.D. she spoke very little English and was a long way from home. Peter and his family became her family and held a special place in Sue’s life. She obvi- ously did well under Peter’s guidance and her paper on ‘The Concept and Use of Hollow Cathode Lamp Excited Atomic Fluorescence Spectrometry in an Inductively Coupled Plasma’ dis- cussed the last work she had carried out under Peter’s supervision. Dr.Dan Gerth (Lancaster Labora- tories PA USA) Peter’s last student then gave two presentations on chrom- ium speciation via LC and ICP-AES. The continuous variation was used to characterize the stoichiometry of the Cr species extracted with the reagent pyridine-2,6-dicarboxylic acid. The application of the analysis to heavily contaminated soils was discussed. Peter had a long-standing collabora- tion with Lancaster Laboratories. One of these talks should have been given by Professor Saul Shupack a former colleague of Peter’s in the Chemistry Department at Villanova but unfortu- nately he was taken ill so Dan nobly gave two papers. Another interesting paper was given by Dr. Seif Nikdel (Florida Depart- ment of Citrus FL USA) on how60N JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY DECEMBER 1992 VOL.7 Dr. Julian Tyson (R) presenting a plaque in memory oj- Peter Keliher to Dr. Joe Foley rep resenting Villan ova University adulteration of orange juice is detected in Florida using atomic spectroscopy and neural networks. Seif had worked as a research assistant in Peter’s group in the mid-1970s. We were assured that orange juice from Florida is pure orange juice. A philosophical view of ‘Current Economic Influences on Analytical In- strument Development’ was given by Dr. Andy Zander (Varian CA USA) plus a recollection that Peter could unscramble a Rubik’s cube at an in- credible rate which must say some- thing! Whilst Andy was pursuing Ph.D. studies with Professor Tom O’Haver at Maryland he collaborated with Peter on work concerned with the use of the echelle spectrometer in a continuous source AA instrument with wavelength modulation.Dr. Charles Wohlers (Energy and Environmental Engineering Cam- bridge MA USA) Peter’s first gradu- ate student then discussed ‘How to Write your own CLP Software’. There then followed two presenta- tions outlining Peter’s involvement with publishing of reviews. Louise Voress from the American Chemical Society gave a history of ‘The Funda- mental Review of Atomic Emission Spectroscopy’ which appears in Ana-. lytical Chemistry in the even years. In the last Analytical Chemistry review Peter authored in 1990 he included the following sentiments.’ ‘ “To every thing there is a season and a time to every purpose”.The various members over the years of the Villanova author group have been writing this review since 1980. It has been our privilege to survey selectively the field of emission spectrometry every two years and we have certainly seen many exciting de- velopments over the years. We have tried to write balanced objective re- views in a style that makes each review as readable (sometimes with a bit of humour) as possible. We appreciate the opportunity that Analytical Chemistry has given us but it is now time to pass the mantel on to others’. Peter attended Imperial College University of London working in Tom West’s group for his Ms.C. and D.I.C. degrees in 1967 and Ph.D. in 1969. This was the beginning of his strong transatlantic links which he had always been keen to maintain. He had joined the Editorial Board of ARAAS in 1983 and was eager to help launch in 1986 its successor the Atomic Spectrometry lJpdates (ASU) Dr. Sue Franz Ph.D. student of Peter Keliher which appear in JAAS. This was the reason I had attended the FACSS meeting in Philadelphia in 1985 prior to the launch. Peter had kindly given the RSC a free booth in the exhibition insisting that this would be extremely useful. He was of course right and I have attended FACSS ever since and view it as an essential meeting in the spectroscopist’s calendar. It is there- fore ironic that the second paper on publishing should be given by myself back in Philadelphia for the first time since 1985. The background to the publication of ARAAS and its evolu- tion into ASU and JAAS were ex- plained. The last presentation in the sympo- sium was by Leonard C. Klein of FMC Corporation Princeton NJ the Secre- tary of the American Microchemical Society (under whose auspices The Microchemical Journal is published by Academic Press) who outlined the history of the Society and spoke briefly about his involvement in the process by which Peter took over the editor- ship of the journal. He confirmed that Peter did an excellent job in revitaliz- ing the journal. It was obvious from everyone who contributed to the Symposium that they had fond memories of Peter and that he had been a special person to them all. Finally as a permanent tribute to Peter Keliher Julian Tyson presented a plaque on behalf of FACSS to Dr. Joe Foley a representative of Villa- nova University. The Symposium had been thoughtfully put together and reflected Peter his character work and his friendships. Reference 1 Keliher P. N. Ibrahim H. and Gerth D. J. Anal. Chern. 1990 62 184R. Judith Egan Editor

ISSN:0267-9477    

DOI:10.1039/JA992070053N

出版商:RSC    

年代:1992

数据来源: RSC

摘要:

60N JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY DECEMBER 1992 VOL. 7 Conferences and Meetings CANAS ’93. Colloquium Analytische Atomspektroskopie March 1 5- 19 1993 OberhoJ Thurin- ger Wald Germany The Colloquium will include presenta- tions on all aspects of analytical atomic spectrometry and related disci- plines of inorganic elemental analysis. Fundamental and analytical applica- tions of the following areas will be covered AAS ETA flame hydride and cold vapour techniques; AES; AFS; XRF; and inorganic MS. The conference language will be German although contributions in English are welcome. No translation facilities will be provided. The venue is the Hotel ‘Am Schutzenberg’ in Oberhof Thuringer Wald. For further details contact Professor Dr. K. Dittrich Universitat Leipzig Fachbereich Chemie WB Analytik Linnestrasse 3 0-70 I0 Leipzig Ger- many; telephone (0)341 23922370; fax (0)34 I 23922625.The Royal Society of Chemistry Annual Chemical Congress April 5-8 1993 University of South- arnpton UK The 1993 Annual Chemical Congress of the Royal Society of Chemistry will take place at the University of Southampton during the period Monday 5 April to Thursday 8 April 1993. The main theme of the Congress is Design Synthesis and Characteriza- tion of New Materials and six plenaryJOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY DECEMBER 1992 VOL. 7 61N lectures associated with this theme will be presented. The Analytical Chemistry Sympo- sium is titled ‘Trace Analysis The Future Limits’. All papers in the Symposium will be by invitation but opportunities will be provided for dis- cussion within the Symposium pro- gramme. Invited speakers in this section include 0.Axner D. Cowan 0. F. X. Donard A. I. Ferguson K. Grob R. F. C . Mantoura H. V. Shur- mer M. Thompson P. C. Uden K. K. Unger C. M. G. van den Berg P. van Zoonen and R. N. Zare. For further information contact Dr. John F. Gibson Secretary (Scientific) The Royal Society of Chemistry Burlington House London UK WlV OBN. XXVIII Colloquium Spectroscopi- cum Internationale (Post-Symposium Graphite Atomizer Techniques in Ana- lytical Spectroscopy) July 4-7 1993 University of Durham Durham UK A first circular on the 1993 CSI Post- Symposium has been produced by the Organizing Committee. The sympo- sium will focus on recent research using graphite electrothermal furnaces in atomic absorption emission fluores- cence and mass spectrometry with an emphasis on achieving accuracy in practical analysis.The topics will include reaction and interference mechanisms; temperature and atom distribution measurements; absolute analysis; coupling with hy- dride generation chromatography and flow injection; laser applications; solid and slurry sampling; metal and other non-graphite surfaces; and all applica- tions in these areas. The meeting will be an excellent forum where scientists both with a great deal of experience in these tech- niques and others new to the field can meet to exchange ideas and views and present their research data. Sessions The Symposium will comprise two and a half days with invited lectures oral presentations and posters.Lec- tures will last 25 minutes with an additional 5 minutes for discussion. The posters will be given equal promi- nence during the whole meeting though the presenters must attend their poster during the dedicated poster session when ample time will be allowed for discussions. Invited speakers include Professor J. A. Holcombe (Austin TX USA); Professor B. V. L’vov (St. Petersburg Russia); Dr. D. Styris (Richland WA USA); Dr. N. J. Miller-Ihli (USDA Beltsville MD USA); Dr. D. Tsalev (Sofia Bulgaria); and Dr. M. Hinds (Ontario Canada). Accom rnoda tion All participants will be accommodated in a University of Durham hall of residence with individual study bed- rooms. As an alternative lists of local hotels and guest houses can be supplied for those who wish to make their own arrangements. Registration fee A f200 registration fee is required to offset expenses incurred in setting up the meeting. However this fee includes the costs for all accommodation meals transportation and social events. As is traditional at UK meetings younger scientists are particularly encouraged to attend the meeting and a number of bursaries will be offered to research students. For further information contact XXVIII Colloquium Spectroscopi- cum Internat ionale (Post-Symposium Graphite Atomizer Techniques in Ana- lytical Spectroscopy) Department of Chemistry (CSI Secretariat) Loughbo- rough University of Technology Loughborough Leicestershire UK LEI 1 3TU.

ISSN:0267-9477    

DOI:10.1039/JA992070060N

出版商:RSC    

年代:1992

数据来源: RSC

摘要:

JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY DECEMBER 1992 VOL. 7 61N Future Issues Will Include- Interferences in Inductively Coupled Plasma Mass Spectrometry A Re- view-E. Hywel Evans and Jeffrey J. Giglio Differentiation Between Organic and Inorganic Chlorine by Electrothermal Vaporization Inductively Coupled Plasma Mass Spectrometry Applica- tion to the Analysis of Polychlorinated Biphenyls in Waste Oils-Peter Rich- ner and Samuel Wunderli Rapid Furnace Programmes for the Slurry Electrothermal Atomic Absorp- tion Spectrometric Determination of Chromium Lead and Copper in Diato- maceous Earth-Ignacio Lopez Garcia Jesus Arroyo Cortez and Manuel Her- nandez Cordoba Use of Thallium as an Internal Correction for the Measurement of Lead Isotopic Ratios by Inductively Coupled Plasma Mass Spectrometry -Andrew J.Walder Philip A. Freed- man and I. Platzner Simple Nitric Acid Dissolution Method for Electrothermal Atomic Ab- sorption Spectrometric Analysis of Atmospheric Aerosol Samples Col- lected by a Berner-type Low-pressure Impactor-Tuomo A. Pakkanen Risto E. Hillamo and Willy Maenhaut Characterization of a Linear-flow Torch for Inductively Coupled Plasma Atomic Emission Spectrometry-Nor- man N. Sesi P. J. Galley and Gary M. Hieftje Feasibility Study for Quantitative Multi-element Determination in Sili- cates by Laser Ablation Inductively Coupled Plasma Mass Spectrometry (LA-ICP-MS)-John G. Williams and Kym E. Jarvis Behaviour of Cadmium Cobalt and Lead in Chlorine Containing Organic Solvents in Electrothermal Atomic Ab- sorption Spectrometry-E. Tserovsky S.Arpadjan and Irina Karadjova Development of an Atomic Fluores- cence Spectrometer for the Hydride Forming Elements-Warren T. Corns Peter B. Stockwell Les Ebdon and Steve J. Hill Analysis of Impurities in Germanium Tetrachloride Germanium Dioxide and High Purity Germanium by Zee- man Graphite Furnace Atomic Ab- sorption Spectrometry-E. Senti- menti G. Mazzetto L. Meregalli and E. Milella Sensitive ‘One Drop’ Flame Atomic Absorptiometric Determination of Cadmium in Botanical Samples Using Direct Nebulization of Chloroform Extract-Isao Kojima and Shinji Kondo Effects of Surfactants in Flame Atomic Absorption Spectrometry With Pneu- matic Nebulization Influence of Hy- drophobic Chain Length-A. I. Ruiz Antonio Canals and Vicente Hernandis62N JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY DECEMBER 1992 VOL.7 Determination of Butyltin Com- pounds in Sediment Samples by Gas Chromatography-Atomic Absorption Spectrometry Following In Situ Deri- vatization With Sodium Tetraethylbo- rate-Yong Cai Spyridon Rapsoman- ikis and Meinrat 0. Andreae Electrothermal Vaporization and U1- trasonic Nebulization for the Determi- nation of Aqueous Sulfur Using a Ulowatt-plus Helium Microwave- induced Plasma-Jorge Alvarado Mingin Wu and Jon W. Carnahan Determination of Scandium Yttrium and Eight Rare Earth Elements in Silicate Rocks and Six New Geological Reference Materials by Simultaneous M ul t i-element Electrothermal Atomic Absorption Spectrometry With Zee- man Background Correction-J. G. Sen Gupta Application of Ultrasonic Nebuliza- tion in the Analysis of Petroleum and Petrochemicals by Inductively Coup- led Plasma Atomic Emission Spectro- metry-Robert I.Botto Figures of Merit for Two-step Furnace Atomization Plasma Emission Spec- trometry-Anders K. E. Ohlsson Ralph E. Sturgeon Scott N. Willie and T. Van Luong Evaluation of a Modified Electrother- mal Vaporization Sample Introduc- tion System for the Analysis of Liquids by Inductively Coupled Plasma Atomic Emission Spectrometry- J. M. Ren and Eric D. Salin Atomic Spectrometry Update Environmental Analysis-Malcolm S. Cresser Janet Armstrong Jennifer Cook John Dean Peter Watkins and Mark Cave JAASbase A unique database of atomic spectrometry reference information for the practising analyst JAASbase is a new PC-based product from the ‘The database consists of listings of published Royal Society of Chemistry designed to meet every atomic spectrometry papers and conference atomic spectroscopist’s need for a comprehensive papers and includes tabulated information relating yet inexpensive source of current analytical atomic to the application of relevant techniques. The spectrometry information.It contains over 20,000 references are easily searched with the database regularly updated references compiled from the manager Idealist which also enables the addition of atomic spectrometry literature. personal data to the database. Subscription Details JAASbase 1993 Updates f99.00/$218.00 JAASbase Backfile (1987-1992) f230.00/$506.00 Idealist Software f210.00/$462.00 Six updates will be issued at regular intervals through 1993. Special Introductory Offer Take out a subscription to JAASbase Updates buy the JAASbase Backfile and receive Idealist absolutely free! Offer available only until July 1993. ROYAL CHEMISTRY SOCIETY OF JAASbase is an invaluable tool for all practising analysts - order your copy today! 6 To order JAASbase and for further information please contact Sales and Promotion Department Royal Society of Chemistry Thomas Graham House Science Park Milton Road Cambridge CB4 4WF United Kingdom. && Tel +44 (0)223 420066. Fax +44 (0)223 423623. Telex 818293 ROYAL. Information Services

ISSN:0267-9477    

DOI:10.1039/JA992070061N

出版商:RSC    

年代:1992

数据来源: RSC

摘要:

JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY DECEMBER 1992 VOL. 7 349R ATOMIC SPECTROMETRY UPDATE-INDUSTRIAL ANALYSIS METALS CHEMICALS AND ADVANCED MATERIALS John Marshall* and John Carroll ICI plc Wilton Research Centre P.O. Box 90 Middlesbrough Cleveland UK TS6 8JE James S. Crighton BP Research Centre Chertsey Road Sunbury on Thames Middlesex UK TW16 7LN Charles L. R. Barnard Department of Physical Sciences Glasgow Polytechnic Cowcaddens Road Glasgow UK G4 OBA Summary of Contents Metals 1 .l. Ferrous Metals and Alloys 1.2. Non-ferrous Metals and Alloys Table 1. Summary of Analyses of Metals Chemicals 2.1. Petroleum and Petroleum Products 2.1.1. Crude oil and fractions 2.1.2. Lubricating oils 2.2. Organic Chemicals and Solvents 2.2.1. Chemicals 2.2.2. Solvents 2.3. Inorganic Chemicals and Acids 2.3.1.Chemicals 2.3.2. Acids 2.4. Nuclear Materials 2.5. Process Analysis and Automation Table 2. Summary of Analyses of Chemicals Advanced Materials 3.1. Polymers and Composites 3.2. Semiconductor Materials 3.3. Glasses Ceramics and Refractories 3.3.1. Glasses 3.3.2. Ceramics refractories and catalysts Table 3. Summary of Analyses of Advanced Materials This Atomic Spectrometry Update is the latest in an annual series appearing under the title of ‘Industrial Analysis’. The structure of the review is the same as that used in previous years. Significant advances have been made during the year under review in the design of GD cells for the analysis of conducting and non-conducting materials. It is evident that the development of r.f. boosted discharges and more practical cell geometries has extended the range of the technique. Applications continue to increase in the multi-layer metals field and there are signs that the semiconductor and materials fields are seeing some of the benefits of this technology such as depth profiling.Techniques involving laser ablation (LA) sampling are also increasing in popularity for the characterization of solids reflecting the requirement for the differentiation of material functionality in situ. Sensitivity is still an issue in many fields as demand for increasingly high purity chemicals and materials grows. Thus preconcentration procedures continue to be reported. The opportunity such methods provide for chemical speciation is evident and chromatography is becoming an essential preparatory tool in the armoury of laboratories involved in inorganic analysis. 1.METALS This section of the review covers the analysis offerrous and undoubtedly the largest number of abstracts refer to nonferrous metals and alloys by analytical atomic spectro- methods based on ICP-AES. Sample treatment method- metry. A summary of the analytical methods reported for ologies such as matrix separation dissolution and direct the analysis of metals in the year under review is given in introduction tended to predominate in the literature. Table 1. Details of these procedures can be found in Table 1. The development of procedures for on-line analysis of molten iron (9211924) and steel (921C3496) has been 1.1. Ferrous Metals and Alloys reported. This was achieved by continuous monitoring of A wide range of analytical techniques have been applied the spectrum from a hot-spot generated by the application to the analysis of ferrous metals in the Past Year but of a stream of oxygen impinging on the surface of the molten metal.This relatively rapid technique (typical *Review Co-ordinator to whom correspondence should be ~ ~ a s u r e m e n t Period 15 S> could be applied to those elements that had a vapour pressure significantly higher addressed.3 50R JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY DECEMBER 1992 VOL. 7 Table 1 Element Ag Ag Ag Al A1 Al Al Al A1 Al A1 As As As SUMMARY OF THE ANALYSES OF METALS Technique; atomization; analyte form* M S; ICP; L Matrix High-purity copper Sample treatmentkomments Sample digested in 50% HNO and mixed with 50 mg of tellurium extracted with HCI reduced and redissolved in HNO,; an LOD of 0.1 1 ppb Ag and precision of 3.8% were reported using isotope dilution Experimental parameters optimized to give sputtering rates of 0.24 mg s-I cm-2 (at 40 mA and 0.15 mbar); LODs of 0.010% and RSDs of 3% were reported Sample mixed with Florisil-CaO heated to 1200 "C when the volatile Ag was transferred into the flame in a stream of purified air An arc-shaped platform was treated with molybdate to reduce matrix effects; RSDs of 1.22-3.38% were reported Acid soluble fraction Magnesium sulfate chemical modifier and pyrolytic graphite tubes were used to avoid interference from iron filtered (0.45 pm); acid soluble Al obtained by alkaline fusion in a 1 + 1 H,BO,-K2C0 mixture ashed at 1000 "C Extraction with C,7-C20 carboxylic acids gave 99% extraction of Al at 60-80 "C Glow discharge cleaning removed surface contamination by C Na F and CI by reaction with H atoms MS and GD-MS Sample is dissolved in HCl-HN0,-H,O (3 + 1 + 2) Computerized interference table described for ICP- Direct sputtering and depth profiling On-line continuous FI manifold for matrix isolation and HG from NIST and BAM reference materials; RSD 1.59/0 ( I0 ppb n = 12) reported Samples dissolved in HNO and HCl and As determined at 193.7 nm.An RSD of 2.8% was reported for 199 ppm of As in pig iron Sample dissolved in HN03 (1 + 1) and As was co-precipitated with MnO and re-dissolved in HN0,-H202. Matrix interferences were removed by addition of 100 ppm of Ba Ca or Ma Samples dissolved in HCIO or H,SO BCS CRM alloy digested in 4% HNO,-48% HF in a microwave oven gave AsV.The system gave an LOD of 0.5 ppb and an RSD of 3.5% at 10 ppb As Samples were extracted into xylene-2-ethyl- 1,3- hexanediol; an LOD of 1.6 ppb was reported Diffusion of B in alloy characterized Dissolution by high-pressure microwave digestion. Isotope dilution LODs of 10 fg g-' were reported; precision was found to be less than 3% Dissolution in acid and generation of methyl borate Samples were dispersed in a B,C-Mo medium; alpha- factor correction gave a 'fairly' linear calibration Particulate Be was boiled in a solution containing 2% HNO Sample was dissolved in concentrated HNO and converted into its hydride Samples were dissolved in 0.1 mol dm- HCI and 0.4 mol dm-' HNO and passed down an AGMP-50 macroporous cation-exchange column which separated analyte from matrix tungsten probe coated with trioctylphosphine oxide then immersed in a 20 ppm Ni solution to remove the excess Samples dissolved in HCI were deposited on a Reference 91/3855 92lC664 9213600 92159 9211 9 18 9211919 9212273 9212952 9213098 9213428 92lC37 56 91lC3632 9113859 9 113864 92/3 187 92lC3663 921248 921 1526 92x3345 9 2 x 3 3 8 2 92/2536 9212990 92/20 10 921249 1 High-purity gold AE;GD;S AA;F;G Copper ore AA;ETA;L Steel Steel Steel AE;spark;L AA; ETA;L Non-alloyed steel AA;F;L Copper- nickel- and zinc-based alloys Aluminium alloy X R F -; - SIMS; -; - Standard solid MS;GD or AA;GD;S AA;ETA FI Hy;L 1CP;S or L Coatings of silicon wafers Copper metal AA;ETA;L Iron and steels Iron copper and nickel AA;ETA;L As Manganese steels As Nickel-based alloy AA;Hy;L AA;FI Hy;L B Steel AE;ICP;L B B Amorphous alloy Steel CRMs SIMS; -; - MS;ICP;L B Be Steel Niobium-beryllium alloys AE;ICP;L EPMA AA;F;L Be Standard beryllium Bi High-nickel alloy AA;Hy F;L Tellurium mercury gold or platinum metals Bi Bi ZAA;ETA;L 921268 1 Copper alloyJOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY DECEMBER 1992 VOL.7 351R Table 1 SUMMARY OF THE ANALYSES OF METALS-continued Technique; atomization; analyte form* AA; F; L SEM;X-ray;S XRF-;S XRFi-iS Element Matrix Ca Iron-nickel alloy Cd Gold-silver alloys Ce Steel c o Iron Sample treatmentlcomments Use of dinitrogen oxide-acetylene flame for improved sensitivity for Ca Detection of Cd in modern solders to distinguish from antique Cd-free solders Measurement of dopant levels e.g.0.001% at the La line Sample was dissolved in acid peroxide mixed with citrate and precipitated from solution at pH 7.0 with 2-nitroso-1 -naphthol. Co was determined at 50 kV 30 mA for a counting time of 40 s ammonium thiocyanate adsorbent supported on naphthalene; Co chelate was stripped from the column with DMF Preconcentration on tetradecyldimethylbenzyl- Dissolved in HCI Reference 9113852 92/27 1 9212937 921294 9213880 92lC3 7 3 5 92150 921C664 92lC72 1 921969 921 1 628 92lC359 1 92lC3670 92K3772 9113773 9113868 921 1 I92 9212937 921 1 397 921 1 848 9212 89 7 92lC3 3 52 921 1809 921 1 924 9212237 c o Aluminium alloys and steel AA;F;L Cr Chrome-phosphate surface c u Aluminium alloys coatings on aluminium AA,AE,XRF;-;- AA;F;L AE;GD;S AA;F;L MS;-;S Electrolytic dissolution into HNO,; repeatability of As for Ag Precipitation of Ag as chloride salt; extraction of Cu Fast atom bombardment and time of flight MS used 4-5% reported from the precipitate to monitor scatter of neutral species.Characterization of the Cu surface Excitation mechanisms and plasma composition investigated and resonance charge transfer between Cu atoms and plasma gas species reported to be main feature Direct analysis of solid samples in a graphite cup introduced into the ICP and time-dependent emission profiles used to separate analyte from matrix cavity described for which 26% of Cu was ablated and transported to the detector system Direct solid analysis by volatilization of sample using a high-voltage spark Metallic Fe is sputtered from the cathode surface and excited with a Nd:YAG pumped tunable UV laser; sub-ppm detection reported Samples were dissolved in 5 mol dm- HNO spiked with a mixture of "Ga and 69Ga (in 1 mol dm-' HNO,).The solution was evaporated to dryness and dissolved in 7 mol dm- HCI then extracted into isopropyl ether and evaporated to dryness and dissolved in 1 .O rnol dm - HNO Redox reactions were used to bind analyte to Cu substrate. Optimization of experimental parameters gave detection at sub-pg levels As for Ce Effect of Li compounds on corrosion of steel LA chamber was characterized and a cylindrical demonstrated that Li ions penetrate the grain boundaries Dissolution in HNO Bulk spectra of the alloy exhibited martensitic transformations that were not observed for Li evaporated on cooled substrates Optimization of sample ablation factors gave usable precision of 1-2% Samples were decomposed in HCI-HNO in a PTFE chamber; Mn was separated from the matrix on a cation-exchange microcolumn with 95% recoveries On-line monitoring of hot-spot generated when oxygen impinges on the Fe offered good correlation between emission intensity and Mn concentration from 0.26 to 1.09% Depth profile analysis revealed that the surface layer was enriched with Mn c u High-purity gold cu Silver nitrate cu Copper cu Copper metal AE;GD;S cu Lead and zinc AE;ICP;S cu Copper metal MS;ICP;S cu Copper alloys Fe Iron MS;ICP;S AF;GD;S Ga Aluminium MS;ICP;L Ir Copper AE;GD;S La Li Steel Steel Li Li Lead-lithium Lithium-magnesium A€; 1CP;L Soft X-ray emission Mg Mn Aluminium metal Nickel and tantalum AE;laser plasma;S AA;ETA;L Mn Molten iron AE;-;L Mn Steel AA;F;L352R JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY DECEMBER 1992 VOL.7 Table 1 SUMMARY OF THE ANALYSES OF METALS-continued Technique; atomization; analyte form* AA;ETA;S Element Matrix Mn Molten steel Sample treatmentlcomments Metal vapour above the molten steel condensed to fine particles and introduced into an electrically heated absorption cell in an argon carrier gas Characterization of diffusion and etching profiles for a GD cell Sample dissolved in acid and extracted as its 5,S-methylene disalicylo hydroxamic acid complex into IBMK; Mo determined as its thiocyanate complex with an LOD of 0.03 ppm determination of N at 149.2 nm giving an LOD of Use of specially coated optics permitted 10 PPm Cathode sputtering atomizer with potential for depth profiling was characterized.An LOD of 24 ppm was reported for a 1 nm thick layer of Mo Most (97.5Oh) Ni was precipitated from solution as its dimethylglyoxime complex and Ni in the filtrate determined with a precision of 0.039% Propane-butane-air flame used with addition of triethanolamine and Sr eliminated depression of Ni signal; an LOD of 0.001% was reported Samples fused in an induction furnace for 2 min then compressed at 200 MPa for 10 s. Analysis time was 15-20 min Low ppm detection of 0 required careful reduction of background Sample solutions with 2-5-fold excess of ammonium molybdate mixed with diantipyrylmethane; indirect method based on Mo detection complex into IBMK has a sensitivity of 0.02 ppm; no interferences were found subjected to an r.f.spark discharge which created a colloidal dispersion which was directly nebulized Sample was dissolved in 7 mol dm-3 HNO,; adjusted to pH >2.0 and mixed with manganese nitrate and permanganate to co-precipitate matrix with MnO,. The filtered precipitate was re-dissolved in 2 mol dm-3 HNO and H,O for detection of Pb Pulsed mode and continuous wave sample sputtering in a hollow cathode atomizer were capable of LODs in the region of 40 ng g-l Discharge conditions were optimized for quantitative analysis so that emission yield was independent of sputter rate calibration was linear to 50 ppm with RSDs in the range 1.19-2.35% Solvent extraction of a phosphantimonyl molybdate Samples were immersed in high-purity water and Samples were determined in HCI-HBF and As for Ir Sample solutions were treated with sodium sulfite to convert any SbV into Sb"' and the stibine swept into a STAT system heated by an air-acetylene flame determination; an LOD of 0.056 ng and RSDs of less than 5% were reported Samples were decomposed in HNO prior to As for As Samples were extracted with dibutyl sulfide in toluene and determined in a double tube furnace arrangement. The LOD was 5 x RSD less than 7% Solvent extraction with potassium xanthates was most efficient at pH < I .5.The method gave a reported RSD of 1.3-1.7% for samples in the range 10-50 pm of Sn g with an Reference 9213867 9211 629 9212487 92lC603 9213606 9 114039 9211927 9212958 92123 14 9212267 921243 1 92lC33 70 9213406 9213607 92x3727 921 164 9211 192 92/3770 9113853 9 llC3632 921 149 Mo Molybdenum metal Mo Steel MS;GD;S AA;F;L N Steel AE;spark;S AF;GD;L Na Molybdenum Ni Ferro-nickel AA;F;L Ni Alloys of aluminium copper and zinc AA;F;L Ni Copper XRF-;S 0 P Alloys Ferro-alloy MS;GD;G AA;F;L P Copper alloys AA;F;L P Copper alloys AE; 1CP;L Pb Zinc AE;ICP;L Pb Copper A€-;S Pb Steel AE; GD;S Titanium alloys AA;F;L Pd Pt Sb Copper base Copper based alloys AE;GD;S AA;F;L Sb Iron and steel AA;ETA;L Se Sn Copper metal Gold AA;ETA FI Hy;L AA;ETA; L Sn Aluminium alloys AE;ICP;L 921302JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY DECEMBER 1992 VOL.7 353R Table 1 SUMMARY OF THE ANALYSES OF METALS-continued Element Matrix Technique; atomization; analyte form* Sample treatmentlcomments Ta Niobium-based alloys AE;ICP;L Analyte separated from matrix by precipitation with tetraphenylarsonium chloride in ammonium hydrogen fluoride and H,SO,; then treated with H,SO,-HNO and dilute H,O Te Copper AA;ETA;L Samples were separated by solvent extraction with IBMK from a 6 mol dm- HCI solution with a linear working range of 0-0.3 ppm extracted into 10% vlv tributyl phosphate in cyclohexane.For 10 g of sample an LOD of 7 pg g-' was reported Th Aluminium MS;ICP;L Samples (dissolved in 10 mol dm- HCI) were As for Th U V Aluminium Ferro-vanadium MS;ICP;L AE;ICP;S V w Steels Nickel-based alloys Various (5) Alloys Various Microalloyed steel Various (7) Alloy Various ( I 5) Zirconium alloys Various (20) Gold Various (10) Ferro-chromium and ferro-manganese Various (1 5) Non-ferrous metals Various Alloys Various (7) Steels Various (8) Iron Various ( 13) Copper Various ( 13) Palladium Various (6) Low-alloy steel AA;ETA;L AA; F; L AE;ICP;L AE;ICP;S AE;ICP;L MS;GD;S AA;F;L Samples were homogenized by melting and diluting with pure Fe in a high-frequency furnace followed by centrifugation.Use of spark ablation for aerosol production gave repeatability of better than 0.4% Complex dissolution-oxidation-extraction procedure using HNO and HC1 K2S208 and KMn04 and IBMK then tributyl phosphate and H,O respectively; the LOD was 0.3 ppm with an RSD for NIST SRM 361 of 3.79/0 (n= 17) 0.5 g of a finely milled sample was dissolved in 1 +4 HF followed by a 3+ 1 mixture of HCI and HNO while heating.The cooled solution was mixed with H,PO and acetone then diluted On-line electro-dissolution in a flow-through cell with FI Comparison of conventional nebulization with spark pre-atomization Rapid two-step microwave decomposition using a mixture of HCl and HNO,; precision of 0.4% was obtained by use of internal standards source gave a reported precision of less than 4% for ten elements and LODs of less than 0.5 ppm for 13 elements permitted determination of elements with LODs in the range 0.002-0.4 ppm with RSDs from 3 to 8% Samples were dissolved in a mixture of phosphoric and sulfuric acids in a PTFE vessel; reported LODs ranged from 12 to 120 ppb Samples were digested with a ternary reaction mixture (HCl H,O MnO,) in a closed thermostated reactor.The method was applicable to determinations in the range 0.0O2-9O0h mlm reported detection range of 10 ppb-I0 ppm with total analytical precision between 1 and 6% relative YAG LA produced fine particles giving detection in the range 0.01-5.6 ppm for 0.18 s integration time Matrix was removed by solvent extraction into IBMK; analysis was carried out by TXRF. Reported LODs were of the order of 100 ng g-I Multi-element preconcentration is achieved by reductive matrix precipitation and LODs of between 0.1 and 5 ppm are achieved for FAAS and 0.01-0.1 ppm for ETAAS; typical RSDs were 3% (n= 12) were in the range 0.6-9.4% Nd:YAG laser and swept into the ICP; analysis of NIST 1767 SRM was reported and RSDs in the range 3-9% were obtained Direct analysis with a gas-jet enhanced sputtering Micro-batch anion-exchange matrix removal FI with on-line electrolytic dissolution gave a AE;ICP;L MS;ICP;S Sample was dissolved in 10% HCI and the RSDs Samples were vaporized with a 500 mJ pulse from a AE;ICP;L AE;ICP;L AE;ICP;L MS;ICP;S XRF-;L AA;F;L Reference 9213504 9212226 92J3596 9213596 921C593 921 1706 921295 1 92157 921249 92lC594 9211 2 12 921201 8 9212405 9212444 9212762 92lC3 568 9213792 9 113882 9213975 9214029 * Hy indicates hydride generation and S L G and SI signify solid liquid gaseous or slurry sample introduction respectively.Other abbreviations are listed elsewhere.354R JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY DECEMBER 1992 VOL. 7 than that of the matrix.In these studies Cr Cu Mn Ni and Pb were detected with an optical fibre connected to a high- resolution monochromator. The use of electrical sparks for pre-atomization of samples continues to find application in metallurgical analysis (9213200). A direct comparison of spark ablation and conventional nebulization ICP-AES indicated that both techniques possessed similar detection and precision characteristics (921249). Thus spark ablation into an ICP has been found to be a reproducible method for the determination of V in steels (92/C593). The determination of low levels of N in steel by spark emission spectrometry has always been difficult owing to sensitivity limitations (= 100 ppm) in the UV region of the spectrum. However the use of magnesium fluoride coated optics coupled with a lithium fluoride entrance lens and a far-UV sensitive phototube has been found to improve the response for N at 174.2 nm (921C3737). It was reported that an improvement in detection limit of two orders of magnitude could be achieved by means of these instrument modifications.A spark source MS technique was described for the determination of H in stainless steels using a pointed metal probe (92/ 1293). The H background level was reduced for the sample in the ion source by vacuum-backing at 323-343 K. The levels of H reported in austenitic steel were in the range 2-4 ppm with an RSD of 20%. Spatial selectivity is not readily available by spark ablation and where this criterion is important the use of laser ablation (LA) is found to be most appropriate (92/ 1252) irrespective of the detector to be selected.The use of ICP-MS continues to gain ground but to a lesser extent than for non-ferrous materials. A report describing the determination of a range of elements in iron materials indicated no significant bias in ICP-MS (92113 16). A typical precision of about 10% relative was achieved for As Co Cr Cu Ga Mo Ni Pb Sb Sn and V. However it was also noted that the determination of Al B Ca C1 F K Na N 0 P S and Si had to be carried out by other means. Spectral interferences arising from the analyte interactions with sample and digestion matrix elements and from plasma gas species have also been the subject of investigation (921C349 1 ). The suppression of ICP-MS analyte ion signals in a steel matrix has also been reported (9212087).A direct sampling approach such as LA can be used to avoid solvent-related interferences in ICP-MS. Thus a Q- switched Nd:YAG laser operated at 15 Hz repetition rate was used to vaporize nanogram amounts of Low-alloy Steel (NIST SRM 1767) prior to the determination of Ag Pb Rb Sr,Th and U by ICP-MS utilizing silicon as an internal standard element (9214029). The reported method gave results in good agreement with certified values with RSDs in the range 3-9%. Studies have also been made using a CW Q-switched Nd:YAG laser focused onto the sample surface (921C3568). It was reported that fine particles of the order of 0.02 pm were generated with a relatively high ablation rate of 22 pg s-I. The accuracy obtained was reported as being ‘acceptable’ with precisions in the range 5-10%.Detection limits were in the range from 0.01 ppm for Nd to 5.6 ppm for Ni using an integration time of 0.18 s. The design and development of GD sources has received attention during the period under review. Glow discharge AES has been applied to the determination of V in steels (921229). A dual cathode lamp was described in which background radiation from the filler gas was eliminated. Using this cell the interference of the argon 437.97 nm line on V at 437.92 nm was avoided. The method was reported to be suitable for the determination of V in steel in the range 0.1-2.5% m1m. A GD source was reported which was a modification of the Grimm design incorporating a floating restrictor (92/ 1 193). The cell was devised in such a way that it could be used directly in place of an ICP source in a conventional ICP-MS instrument. The operation of the GD required that the anode was given a slight positive bias with respect to the earthed skimmerhterface plate of the MS.Secondary ion MS and sputtered neutral MS have both found application in the quantitative analysis of steels (92~572). Two techniques were described for depth profil- ing and surface analysis of zinc-coated steel samples. An apparent bias in the XRF determination of Ti in steels has been reported (9113878). The problem was observed during the analysis of NIST SRMs 1165 and 1264 Low- alloy Steels. It was considered that differences in metallurgical uniformity were the major cause of the bias as discrepancies were not found using other techniques.Electron probe data revealed the existence of Ti inclusions containing varying amounts of Nb Ta and Zr which supported the inhomogeneity hypothesis. 1.2. Non-ferrous Metals and Alloys More than two thirds of the 330 abstracts received concerning metals referred to the analysis of non-ferrous metals and alloys. Most of these papers described the characterization of aluminium- copper- or nickel-based alloys and details are provided for convenience in Table 1. The majority of applications described improvements in the area of sample preparation or presentation. The determination of Cu in aluminium alloys using FI- FAAS has been described (92150). The solid metal samples were dissolved in 0.2-1.0 mol dm-3 HN03 on- line using an electrolytic approach.The effect of electro- lyte composition and electrolysis parameters on the disso- lution of samples was investigated. The repeatability attained for the measurement of Cu in aluminium alloys in the concentration range 0.5-10% was of the order of 5% relative. Microscale electrolytic preconcentration pro- cedures were used for the determination of Cd and Pb in silver (9212769). Anodic dissolution was used to dissolve microgram amounts of the sample and the analytes were simultaneously separated from the silver matrix by elec- trolysis. The determination of Cd and Pb in the electro- lyte was carried out by FAAS. Other reports also describ- ing the use of electrolytic sample dissolution prior to analysis might be of interest (9212762 921C3370 92/C3588).A microbatch anion-exchange method was used for matrix separation in the determination of trace elements in gold (92/2018). This rapid method was developed for the separation of strongly bound metals (e.g. gold palladium bismuth) prior to FAAS detection of 20 trace elements. Detection limits in the range 0.002-0.4 ppm were reported with RSDs in the range 3-8% depending on the analyte of interest. A similar procedure based on microscale ion- exchange separation was described for the measurement of trace amounts of Mn in niobium wire and tantalum powder by ETAAS (9211809). The calibration graph was linear over the range 0.003-0.2 mg of Mn. The recovery obtained for Mn after preconcentration was 95%. The problem of competition between matrix ions and the reducing agent in the HG process may be overcome using FI-AAS in conjunction with on-line matrix isolation (911C3632).The procedure was applied to the determina- tion of Se in Bundesanstalt fur Materialforschung und - priifung (BAM) 36 and NIST SRM 454. These were found to contain 30 and 479 mg kg-l of SeiV respectively. A characteristic concentration of 1 ppb was reported for the method with an RSD of I .5% (1 0 ppb of Se n = 12).JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY. DECEMBER 1992 VOL. 7 355R It has been reported that the use of the graphite cup sample insertion technique can be employed to reduce significantly matrix interferences in the determination of Cu and Fe in lead and zinc metals (92/C359 1). Thus when 20 mg of the metal sample were introduced in a cup into the ICP the matrix was preferentially evaporated on a tempo- ral basis since the analyte elements exhibited higher boiling-points.Time resolved emission profiles allowed the measurement of Cu and Fe with detection limits of 5 and 20 ppb respectively. Spark elutriation can also be used in the reduction of matrix interference effects (92/C337 1). A spark ablation unit was constructed from PTFE with ceramic mounting for the tungsten electrode on one side and the sample on the other side. The sample was subjected to a spark of up to 800 V with frequencies in the range 50-400 Hz in an argon atmosphere. A peristaltic pump was used to remove liquid from the sample surface thence to the ICP. The results indicated that good agreement with the ex- pected results was obtained.Spark ablation sampling for FAAS was used to determine a range of elements in metal alloys (92K775). A spark was applied to the sample under the surface of a solid which resulted in the generation of a lisol-like suspension (i.e. particle size > 1 pm). Matrix effects were found to be minimal when employing this approach and this allowed calibration of response using aqueous standard solutions. One of the perceived limitations of the use of LA for direct sampling of metals by ICP-AES is that of relatively poor repeatability and it has been claimed in a recent report that this has prevented the technique gaining more widespread acceptance (92K3352). Thus a 400 mJ xenon chloride laser with a time gated multi-channel spectrometer was used for the determination of Mg in aluminium.It was demonstrated that the repeatability of the method was 1.3% relative for Mg at the 1% concentration level. A theoretical model has been developed to describe the processes which affect the shape of the transient signal associated with single-shot LA (92IC3353). It was found that a bead packed tube and simulated dispersion produced a response curve which closely matched the spikey profile of the LA-ICP transient signal. Sample entrainment and transport in the ablation of Cu prior to determination by ICP-MS has been the subject of a recent study (92/C3670). It was reported that for a cylindrical chamber 120 mm high and 25 mm in diameter approximately 26% of the ablated Cu would be transported to the detector. However only 44% of the total Cu was accounted for.A hypothesis was put forward suggesting that the remainder could be in the form of small Cu clusters. Ultra-high purity aluminium is used in applications associ- ated with integrated circuit components. There is a require- ment for methods for the determination of Th and U at levels close to 1 ppb (92126 13). Laser ablation ICP-MS has been applied to this problem and detection limits of the order of 0.2 ppb have been achieved. Inductively coupled plasma MS has also been applied to the determination of B at ppm levels in a titanium matrix. Beryllium was used as an internal standard for the determination of B in Commu- nity Bureau of Reference (BCR) 090 SRM and the results obtained agreed with the certificate values. Isotope dilution can be used to achieve good precision in ICP-MS.This feature was used in the determination of Ag in high-purity copper (91/3855) by ICP-MS. The sample was digested in 50% v/v aqueous HN03. Approximately 50 mg of tellurium were added to the solution which was then evaporated to dryness redissolved in HC1 reduced and filtered. The precipitate was redissolved in HN03 and Ag determined by ICP-MS. The detection limit was reported to be 0.11 ppm and typical precision was of the order of 3.8%. A magnetron GD plasma has been applied to the analysis of zinc-based NIST SRMs (92/2058). The device was capable of operating over a wide range of pressures [0.0007-2.5 Torr (1 Torr= 133.322 Pa)]. The operating conditions were optimized for each analyte. Detection limits for Mn and Ni were reported to be 0.006 and 0.0005 5'10 respectively.The performance characteristics of a new cathodic-sputtering atomizer for AAS have been described (91/3806). The ability to control the flow and pressure of argon in the atomizer was claimed to result in a 5-fold improvement in sensitivity compared with a com- mercially available atomizer. A system was described in which two pulsed GD sources were housed within one source (92/2659). Two isolated cathodes were placed parallel to each other to allow simultaneous comparison of an analytical sample and a reference standard. The effect of sample positioning was studied by GDMS using a pair of identical SRM 1262 cathodes. It was found that the optimum arrangement resulted in RSDs in the range 2.2-5.2%. When two different cathodes SRMs 1262 and 1263 were used the error was in the range 0.75-9.1% relative.The potential of a cathodic sputtering cell was investigated for use as an atom cell for ultra trace analysis using laser-induced fluorescence (9 1/3773). The cell which had been designed to be used in AAS was applied to the determination of Fe in brass. Sensitivities in the sub-ppm range were reported with accuracy and precision of the order of 15%. Noise studies indicated that the principal limiting noise arose from laser-induced background signals. Glow discharge MS has been applied to an in-depth analysis of the surface layers of nickel-chromium multi- layer systems (92K3462). It was found that in order to achieve acceptable depth projle data it was necessary to ensure that flat crater profiles were produced during sputtering.This was achieved by careful control of the burning voltage. A penetration rate of 100 nm s-' was established and this was sufficient to complete the analysis in a few minutes. A novel type of combined bipole deflector was developed to reduce the disturbances in MS detection resulting from photo-radiation and neutral particles in an r.f. GD source (92/1062). The deflector consisted of half cylindrical electrodes and diaphragms with eccentric aper- tures. A high S/N was claimed for the device. Glow discharges can be used to clean the surface of samples and the efficacy of this process has been studied using SIMS (92/3098). Contaminants on the surface of an A6063 Aluminium Alloy were found to include C C1 F and Na.The concentrations of these contaminants were effectively reduced using the GD cleaning process in a hydrogen atmosphere. Secondary neutral MS has been applied to the characterization of nickel-chromium multi- layer thin Jilms (92/26). It was reported that quantitative sample composition and absolute depth projling could be achieved by using correction for variations in the time dependency of the sputter rate for all elements if the particle density in the sample was known. The determina- tion of trace amounts of 0 in copper has been carried out using SIMS (92/1562). The analyte could be detected in the negative ion mode at m/z 16 or as the copper oxide polyatomic ion at m/z 79 without the interference of residual gas. The ion intensities were normalized to the copper matrix response and it was found that there was a linear relationship with bulk oxygen concentration in the range 0.5-106 ppm.The application of XRF to the characterization of thin jlms has been the subject of a review (9113821). The report indicated that X-ray absorption enhancement was caused by interelement effects in single-layer systems. The accu- racy of analysis was estimated as 1% for composition and 3% for thickness determination.356R JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY DECEMBER 1992 VOL. 7 2. CHEMICALS 2.1. Petroleum and Petroleum Products Elemental analysis of petroleum related materials has continued to attract significant attention amongst workers in the field of atomic spectrometry reflecting the economic importance of this type of analysis.A summary of papers received during the review period is given in Table 2. In addition a two part review (total 165 references) has been published (92/3070 92/307 1 ) which discussed the occur- rence and significance of trace elements in petroleum and petroleum products and provided a critical comparison of modern instrumental methods of analysis. A more specific review (24 references) covering application of plasma spectrometry in the petroleum industry has also been published (92/3891). 2.1.1. Crude oil and fractions As discussed in last year’s review determination of trace elements in crude oil can provide valuable information that can be used alongside traditional biomarkers such as steranes and triterpanes in assessing the origin and maturity of petroleum for exploration purposes.However perhaps an even more important reason for concern about trace elements in crude oil is that these elements are concentrated in the heavy fractions during distillation and can poison the cracking catalysts used for upgrading. Elements present at relatively high (pg g-l) concentrations (e.g. Fe Ni and V) can be determined using X-ray fluorescence (9213079 92/3 195) but alternative approaches are generally required for lower concentrations. Gonzales and Lynch (92/3073) have discussed direct analysis of crude oils for 18 elements using ICP-AES (kerosene dilution with scandium as inter- nal standard) while Al-Swaidan and Hassan (92/1255) have described a wet ashing procedure for the determination of Al Cd Fe K Li Mn Ni Pt Sn and V using ICP-MS.The latter procedure involved treatment with concentrated H2S04 drying and ashing followed by dissolution in HN03. If only a limited number of elements are to be determined however then this can be accomplished effec- tively using ETAAS with LODs down to sub ng g-’ levels (92/1379 92/ 17 16 92/ 179 1 92/ 1793 92/ 1877). A mi- crowave wet ashing procedure for determination of Cr Cu Fe Ni and V using ETAAS and Na and Zn using FAAS may be of particular interest (92/3 146). Direct analysis of petroleum products using ICP-AES generally requires dilution with an organic solvent. This can cause plasma instability and inferior sensitivity particu- larly if volatile solvents are used. Use of an ultrasonic nebulizer has been reported (92/C33 16 92/C3757) which reduced plasma solvent load and led to markedly improved analytical performance.Organic solvents can cause even more problems with ICP-MS because of blocking of the sampling cone with carbon deposits and carbide molecular ion interferences in the mass spectrum. A novel approach to solving this problem was reported previously at a confer- ence and discussed in last year’s Atomic Spectrometry Update (see J. Anal. At. Spectrom. 1990 5 323R). The method now published (92/ 1242) involves direct nebuliza- tion of the oil sample prepared as a micro-emulsion in water. Accuracy and precision were within 3% but LODs were restricted to 0.1 pg g-*. A similar approach has been reported for AAS analysis of crude oil samples using a mixed solvent system (91/3911). In both cases require- ments for organo-metallic standards were eliminated. Finally a novel approach for elemental analysis of crude oil has been reported that involved decomposition of the sample by flow through oxygen combustion with determi- nation using AAS (921C507).This approach could be particularly useful for the determination of volatile ele- ments which can be subject to selective volatilization problems if sample nebulization is used. It is increasingly being recognized that for many applica- tions it is necessary to know not only the total concentration of elements in a sample but also their chemical form. In last year’s review some preliminary information on chemical speciation of elements in petroleum related material was discussed and it was predicted that many more applications would be reported in future years as suitable instruments became more widely available.This has indeed happened and this year has seen an explosion of papers dealing with chemical speciation mainly utilizing a combination of chroma tograph ic separation techniques with el em en t specific detection using atomic spectrometry. Speciation of metallo- porphyrins can provide valuable information on the origin and maturity of petroleum and shale. Quimby et al. (9 113909) have reported the use of GC-MIP-AES for deter- mination of volatile Ni V and Fe porphyrins. However most porphyrins are not volatile enough for this approach and so the use of reversed-phase HPLC with ICP-MS detection has also been attempted (92/C454 92/C3472 92/C3473).Although relatively successful the method does not have adequate chromatographic resolution to compete with the more conventional approach using normal-phase HPLC (UV detection) after de-metallation of the porphy- rins. A novel approach to characterization of metal species in kerogen and other petrochemical precursors has been re- ported by Uden et al. (92K3469). The method involved pyrolysis GC-MIP-AES with on-line butylation of acidic species using tetrabutylammonium hydroxide added to the pyroprobe. Chemical speciation of elements is even more important in refinery streams and products. This is particularly true for suIfur compounds. As sulfur concentrations in available crude oils rise and environmental legislation limits sulfur concentrations in products (e.g.fuels) the availability and efficient operation of desulfurization processes is becoming ever more critical. A prerequisite for this is knowledge of the chemical forms of sulfur compounds in the extremely complex mixtures that comprise the refinery streams. Quimby et al. (9 1 /C37 19) have described automated software for sulfur specific simulated distillation using GC-MIP-AES while Eckert-Tilotta et al. (921C3723) have reported favourable performance of MIP-AES compared with chemiluminescence for sulfur specific GC detection. Heavier petroleum fractions are not amenable to GC analysis but characterization of sulfur species has been accomplished using X-ray absorption spectroscopy (9 1/3986 92/3856). Speciation of alkyilead compounds continues to attract significant attention in view of the impact of these compounds on the environment.Caruso et al. (9 1 /3907) have applied reversed-phase HPLC-ICP-AES and HPLC-ICP-MS for speciation of inorganic and several trialkyllead compounds. Limits of detection were three orders of magnitude better using ICP-MS detection but gradient elution could not be used owing to plasma instability. For non-ionic alkyllead compounds better chromatographic separation can be achieved using GC. Speciation of organolead compounds using GC-AAS has been reviewed (92/3115) while Caruso et al. have also reported use of GC-ICP-AES (9 1 /C3708). However LODs better by several orders of magnitude can be achieved using capillary GC-ICP-MS (92iC455). Limits of detection using the latter approach were better than 1 ng g-’ for a 1 p1 split injection.The determination of oxygenated compounds in gasoline is of great topical interest. These compounds are added to reformulated gasoline to reduce carbon monoxide emissions and will be mandatory under US legislation by 1995. Goode and Thomas (921C3434 92/C38 13) have shown that GC-MIP-AES is an ideal technique for thisJOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY DECEMBER 1992 VOL. 7 357R Table 2 SUMMARY OF ANALYSES OF CHEMICALS Technique; atomization; Element Matrix analyte form* PETROLEUM AND PETROLEUM PRODUCTS- Sample treatmentlcomments Reference As Feedstocks Ba Lubricating oil AA;ETA; L AA;FL Direct analysis using Zeeman AAS FAAS method using air-C,H flame with sodium dodecyl sulfonate and benzyl trimethyl ammonium chloride mixture as enhancing agent.Results compared well with DIN and IP methods using N,O-air flame 13C:1zC ratios determined for any component of crude oil natural gas or source rock extract using GC interfaced to isotope ratio MS via a combustion unit Speciation of volatile Fe porphyrins using GC-AES (302.1 nm). Detection limits for Fe Ni and V porphyrins were 0.05-5 pg s-I Direct determination of Fe Ni and V in fluidized cracking catalyst (FCC) feedstocks. Error was < 10% even for low concentrations (0.01 pg g-I) Samples treated with H,SO prior to ashing. Co was added as internal standard but corrections applied to compensate for overlap of Fe Ka on Co Kp. Good agreement obtained for NIST reference materials 0.5 p1 sample injected into a hot zone (Pyrojector 11) held at between 0 and 900 "C depending on solvent volatility.Vaporized sample fed straight to ICP torch; LOD=5 pg I-' As for Fe Commercial thermospray-membrane desolvation sample introduction system used with reversed-phase HPLC (C,*) for simultaneous measurement of Ni and V porphyrins in crude oil concentrates As for Fe As for Fe Calibration using aqueous standards; LOD= 3 pg g-' Speciation of porphyrins using HPLC-ICP-MS Determination of oxygenated additives in gasoline using GC-AES. Large variation in detector selectivity found depending on viewing position and support gas composition Collaborative study of standardized IUPAC method for direct determination of P in crude and refined oils and fats ( 1 -100 pg g-I) Speciation of alkyllead compounds using GC-ICP- AES Speciation of inorganic and trialkyllead chlorides using HPLC-ICP-AES or ICP-MS.Reversed- phase step gradient from 10 to 70% methanol used for ICP-AES but 30% MeOH isocratic separation for ICP-MS using AAS with C,H,-air flame at 2 17.0 nm. Suitable for determination of PbEt only; Pb concentration range 0.05-1.0 g I - ' Speciation of alkyllead compounds down to sub- ng g-I levels using capillary GC-ICP-MS Determination of organic lead in solid waste and soil by extracting with xylene; 1% absorbance = 0.20 Samples diluted with aviation fuel and Pb determined g-l Pb Review of GC-AAS methods for speciation of S simulated distillation using GC-AES Determination of sulfidic and thiophenic S contents using S K edge X-ray absorption spectroscopy.Results (after correction for inorganic S) compared well with X-ray photoelectron spectroscopy organolead compounds 921C700 921C3564 C Crude oil MS;-;G 921 1 607 Fe Crude oil Fe Heavy fractions Fe Crude oil and residues AE;MIP;G AA;ETA;L XRF-;L 9 113909 9211877 9213079 921C3489 Hg Light hydrocarbons MS;ICP;G Ni Crude oil Ni Crude oil AE;MIP;G MS; ICP; L 9 113909 921C454 9211877 9213079 9213 195 921C3473 921C3434 and 921C38 13 Ni Ni Ni Ni 0 Heavy fractions Crude oil and residues Crude oil Crude oil Gasoline AA;ETA;L X R F;-;L XRF-;L M S; I C P; L AE;MIP;G P Crude and refined oil AA;ETA;L 9212 54 7 9 1 lC3708 9 1 I3907 Pb Pb Gasoline AE;ICP;G AE or MS;ICP;L Alkyllead chlorides AA;FL Pb Petroleum fuel 9 1 I3934 Pb Alkyllead compounds Pb Alkyllead compounds MS;ICP;L AA;FL 92lC455 9211591 Pb Organolead compounds AA;F;G 9213 1 15 S Diesel fuel S Heavy fractionslasphaltenes A E; M I P;G X-ray absorption; - 9 1 lC37 I 9 9 113986358R JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY DECEMBER 1992 VOL.7 Table 2 SUMMARY OF ANALYSES OF CHEMICALS-continued Technique; atomization; analyte form* AE;MIP;G Element S S V V V V V V V V V V Various Various Various Various Various Various (wear metals) Various (additive and wear metals) Various Various Various Various (wear metals) Various Various Matrix Hydrocarbons Sample treatmentlcomments Comparison of AES and chemiluminescence for S- selective GC detection. LODs for both systems were 6-10 pg. However GC-AES gave better sensitivity and stability for carbon Identification and quantification of S classes e.g.sulfur sulfides thiophenes sulfoxides sulfones sulfinic acids sulfonic acids and sulfate As for Fe As for Ni Reference 92lC3123 9213856 9 113909 92lC454 92lC3472 921 1256 375 116 9211791 921 1877 9213019 9213 195 92lC3413 9 1 lC3157 911391 1 921236 92lC398 92lC502 92lC6 14 92lC65 1 92lC657 92lC706 921 1242 9211255 921 1680 921 1 193 9212719 Petroleum and source rocks X-ray absorption; - Crude oil Crude oil Crude oil AE;MIP;G MS;ICP;L M S; ICP; L Sample diluted with IBMK and V extracted into HNO,. Calibrated using standard additions; recovery 99- 10 1 % Oil sample (10-30 g) ashed at 550 "C then dissolved in 1 + 1 HCI (50 ml). V determined in 20 pl portion at 3 18.4 nm using Ar as carrier gas. LOD was 6.9 ng g-l Direct dissolution in xylene compared with wet and dry ashing procedures.Wet ash procedure (H20,-H,S04) gave low results. Results with xylene dissolution method in agreement with dry ash approach but much more rapid 0.5 ng g-I and RSD 1.06% at 1.10 pg g-' Direct analysis using La chemical modifier. LOD was As for Fe As for Fe As for Ni. LOD = 4 pg g-I As for Ni Use of an ultrasonic nebulizer for determination of Cu Fe Na Ni and V in crude oil after dilution with an organic solvent Trace metals measured using AAS with air-C,H flame. Use of organometallic standards eliminated in both cases Review with 93 refs. LODs below 1 ng g-' for elements free of isobaric and polyatomic ion interferences. 0 added to carrier gas to prevent cone blockage Flowthrough oxygen combustion AAS for determination of trace metals. RSDs better than 9.4Oh and recoveries 80- 103% system for wear metal analysis Samples diluted with mixed solvent or dry ashed.Comparison of ICP-AES and rotrode spark emission Crude and heavy oil AA;ETA;L 921 921 Crude oil AA;ETA;L Fuel oil AA;ETA;L AA;ETA;L XRF-;L XRF;-;L MS;ICP;L MS;ICP;L Heavy fractions Crude oil and residues Crude oil Crude oil Crude oil Crude oil AA;F;L Silicones Diesel fuel XRF;-;- MS;ICP;L Crude oil AA;FL Lubricating oil AE;ICP or spark;L Lubricating oil AE;ICP;L Samples diluted with solvent. Internal standard shown to be essential to eliminate viscosity effects Petroleum samples Crude oil and products MS;ICP;L M S; ICP; L Direct analysis using electrothermal vaporization for sample introduction to ICP-MS Samples introduced into ICP as oil in water emulsions.Accuracy and precision are within about 3% and LODs around 0.1 pg g-I Samples treated with concentrated H,S04 dried and ashed. Residue dissolved in HNO filtered and then made up to volume prior to determination of Al Cd Fe K Li Mn Ni Pt Sn and V Rapid digestion in a closed microwave system. Recoveries for Al Cu Fe Ni and Pb in 300 pg g-l NIST standard oil were 98-103% with standard deviations of 3- 14Oh Determination of Cu Fe K Na Ni and V poisons in fluidized cracking catalyst (FCC) feedstocks Direct analysis of solvent-diluted oil using TXRF for concentrations above 1 p g g-'. Low temperature plasma ashing used for lower concentrations. LODs were in ng g-I range for the latter Crude oil MS;ICP;L Lubricating oil AA;F;L Heavy fractions Oils and greases AA;F;L XRF;-;LJOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY DECEMBER 1992 VOL. 7 359R Table 2 SUMMARY OF ANALYSES OF CHEMICALS-continued Technique; atomization; analyte form* Element Matrix Various Petroleum related materials Reference 9213070 921307 1 9213072 9213073 3213074 9213075 9213076 9213078 9213080 9213 146 9213203 92lC33 16 92lC3469 9213 8 3 9 Sample treat men tlcommen ts Review (38 refs.) of trace metal analysis in petroleum and products Various Various Lubricating oil (wear metals) Various (1 8 ) Crude oil XRF;-;L or AE;ICP;L Comparison of wavelength dispersive XRF and ICP-AES AE;ICP;L Samples diluted in kerosene using Sc as internal Rapid (ten elements per minute) multi-element standard analysis of lubricating oils for up to 24 elements using automated sequential FAAS emission spectrometry.Differences attributed to viscosity and particle size effects Comparison between ICP-AES and rotrode spark Various Lubricating oil (wear metals) (additive and wear elements) (wear metals) (additive elements) Various (1 3) Crude and lubricating oils Various Lubricating oils Various Lubricating oils Various Lubricating oil and additives AA;FL AE;ICP or spark;L AE;spark;L Comparison of three techniques to improve detection and quantification of large wear particles. Ashing rotating disc electrode showed most promise WDXRF methods for determination of Ba Ca C1 Cu Mg P S and Zn. Similar to ASTM D4927 XRF;-;L XRF;-;L AA;F or ETA;L Review ( 15 refs.) of analysis of petroleum and Microwave digestion (1 20 W) using (1 + 3 ) HNO products using EDXRF and H,SO (25-30 min).Cr Cu Fe Mn Ni and V determined using ETAAS and Na and Zn using FAAS. Standard additions used for calibration Samples digested with H,SO for 10-20 min using microwave heating. Cu Fe Mo and Ni determined using AAS and improve performance particularly for volatile hydrocarbons Pyrolysis GC-AES for determination of As C Hg N 0 P S and Se compounds in petroleum precursor sediments. On-line derivatization was discussed with butylation of Se compounds as example Determination of As Hg Sb and Se after microwave digestion under high pressure (82.2 bar) of oily waste solvent extracts. RSDs were 5.4-6.6% and recoveries 89- 105% Ultrasonic nebulizer used to reduce solvent loading Review of AAS analysis of silicones (23 refs.) Various Crude oil Various Lubricating greases AA; F; L Various Petroleum and products AE; ICP ; L Various Kerogen AE;MIP;S Various Oily waste AA;ETA or Hy;L AA;F;L Various Silicones ORGANIC CHEMICALS AND SOLVENTS- Ag Drugs and surfactants 9213924 9212454 AE;ICP;L AA;ETA;S or L Indirect determination of amine hydrochlorides quarternary ammonium chlorides and some reducing agents by precipitation following addition of silver nitrate.Residual Ag measured using ICP-AES containing pharmaceuticals by decomposition in graphite furnace followed by AAS. Concentrations in ng g-I range reported (0.001-0.1 mol dm-,) and surfactants (1-2%). A 10-fold enhancement was observed for oxine or triethanolamine at pH 3 using ion pairing and ion-exchange chromatography with ICP-MS.The As"' AsV and dimethylarsenic species were completely separated within 10 min reversed-phase HPLC-ETAAS. Eluent continuously delivered through fused silica capillary at 0.6 ml min-I. Deposited for 2 s on L'vov platform at 150 "C Direct determination of A1 in alkaline earth Study of enhancement effects of organic reagents Speciation of ng g-I levels of arsenic compounds Speciation of arseno compounds using isocratic A1 Pharmaceuticals 9 113974 9 2lC4 5 8 92lC499 A1 As Organic reagents Dimet h ylarsen ic AA; F; L MS; I CP; L Dimethyl arsinate As AA; ETA; L 92lC739360R JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY DECEMBER 1992 VOL. 7 Table 2 Element Br Br Br Ca Cd Cl c1 CI c1 CI c o c o SUMMARY OF ANALYSES OF CHEMICALS-continued Matrix Halogenated dioxins and furans Sodium diclophenac Volatile halogenated hydrocarbons Fulvic acid Diethylcadmium Halogenated dioxins Non-volatile chlorocarbons and furans 1,3,5-triamino-2,4,6- trinitrobenzene (TABT) Volatile halogenated Pesticides hydrocarbons Cosmetics Pyrrolidin-I-yldithioformate Technique; atomization; analyte form* AE M I P ; L XRFi-i- AE;M I P; L AA;F;L AE;ICP;G AE;MIP;L AE; M1P;L M S; ICP; L AE;MIP;L MS; MI P;L AA;F;L AA;FG Cr Sodium dodecylsulfate AA;FL Cr Organic reagents AA; F L Cr Organometallic compounds MS;ICP;L cu Dimethoxydithiophosphate AA;F;L (DDTP) AA;F;L Sample treatmentlcomments Comparison of AES with electron capture for element specific GC detection. Sensitivity of GC-AED worse and some peak tailing was evident No special pre-treatment required Determination of halogenated C and C hydrocarbons in swimming-pool air by trapping on Tenax cartridges and analysing with GC- MIP- AES using a thermal desorption cold trapping injector Study of complexation of Ca and Fe with fulvic acids at various pH and meta1:fulvic acid ratios Determination of Cd in environmental samples following vapour generation using sodium tetraethylborate(rI1).LOD was below 1 ng ml-l but memory effects were a problem As for Br Use of moving band He MIP interface for element specific HPLC detection using AES. LC eluate deposited on moving polyimide or steel band dried and then flash vaporized into MIP 1 + 1 nitric acid and bomb-digested. Solution diluted to 100 ml and analysed using negative ion mode ICP-MS. Typical C1 concentration 0.3% mlm 0.25 g TABT added to 50 g de-ionized water plus 5 ml As for Br SFC-MIP-MS used to separate and detect mixtures of halogenated compounds and pesticides; LOD 3 pg Samples ashed dissolved in water and analysed using AAS.Recovery was 99.0% RSD 4.loh and LOD 0.1 pg g-1 On-line generation of chelate with pyrrolidin-l- yldithioformate followed by vaporization then atomization in a flame heated silica tube. The LOD was around 0.08 p g Enhancement effect (7.6-fold) when ethanol was used as solvent and sodium dodecylsulfate as carrier stream in FI-AAS determination of Cr As for Al. Cr enhanced 7.6-fold using sodium dodecyl sulfonate and alcohol as carrier for FIA-AAS (0.6 mol dm-3 HCI for Cr solution) SFC-ICP-MS. N,O used as mobile phase to avoid interference at mlz 52 from 40Ar1ZC Indirect determination of pesticide DDTP.Method based on formation of Cu(DDTP) complex extraction into CHCl back extraction with an ammonia buffer (pH 10) and determination of Cu using FI-AAS complexes of Cu and Pb from HN0,-HClO digests of plant material. Precision better and interferences less than when IBMK used foam fractionation using chelating surfactants. Concentrations ng ml-l -pg ml-I in aqueous solution Speciation of Cr organometallic compounds using c u Cyclohexanone Cyclohexanone used for extraction of APDC cu Chelating surfactants AA;F;L Cu concentrated 50-75-fold from aqueous solution by Eu Dimethylsulfoxide (DMSO) or Luminescence; Determination of small amounts of water in DMF dimethylformamide (DMF) laser;L (0.1-1 mol-Yo) and DMSO (0.1-5 mol-%) using luminescence lifetime measurements of Eu11' determination of Fell andlor Fell' pg per 1% absorption RSD (4% and recovery 97.8-99.I% Fe Pharmaceuticals AA;F;L and Comparison of AAS and XRF with other methods for Ge Herbal medicine AA; ETA$ Ni(NO,) used as chemical modifier. Sensitivity was 2 XRFi-i- Reference 9 1 /C3637 9 113889 92lC3433 9 114035 921C647 9 1x3637 9 11C3639 9212640 921C3433 921C3475 9 1/40 14 921C578 9 1/39 17 92lC458 92lC3450 9212678 92lC5 8 5 9211635 9212652 9 1/40 15 921 1 54JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY DECEMBER 1992 VOL. 7 361R Table 2 SUMMARY OF ANALYSES OF CHEMICALS-continued Element Matrix Hg Medicine Hg Methylmercury compounds Hg Chemical waste Hg Methylmercury species I Alkyliodides K Butanol La Butyl acetate Technique; atomization; analyte form* AA;FL AA;quartz furnace;L AE;ICP;G or AA;cold vapour;G AE;ICP;L MS;ICP;L AA or AE;FL A E;I CP; L Mn Bis-2-ethyl hexylphosphoric AA;F;L Ni Pharmaceuticals AA;F;L Pb Cyclohexanone AA;F;L S Organic compounds AE;M I P;L acid s (Ba) Pol ysulfides AA;F;L Se Se Sn Sn Sn Sn Sn Organoselenium compounds AE;ICP;L or AA;ETA;L Alkylselenium compounds AA;ETA;L Organotin compounds AE;CCP;L Butyltin and cyclohexyltin AA;ETA;L compounds Alkyltin compounds AA;ETA;L Organotin compounds Organotin compounds Y Butyl acetate Yb Organic reagents MS;ICP;L MS; I CP; L AE;ICP;L AA;F;L Sample treatmentlcomments followed by 3 + 1 HN0,-HCIO,.Also simulation of stomach leaching with determination of Hg in leachate using cold vapour AAS Speciation of Hg and methylmercury compounds in aqueous samples by GC-AAS after ethylation with NaB(C,H,),. The LOD was 167 pg for CH,HgCl dithiocarbamates prior to extraction and analysis using HPLC.Detection using ICP-AES or AAS after generation of Hg vapour using sodium tetrahydroborate (111) Determination of methylmercury species using capillary GC with axially viewed ICP-AES detection. LOD was 3 pg of Hg capillary GC-ICP-MS AE signals of K (range 20-100 pg ml-I) in air-C,H flame Concentration of La by extraction from aqueous phase using I-phenyl-3-methyl-4-benzylpyrazolone and butyl acetate at pH 5.5. LOD=5.3 ng ml-I in aqueous phase nebulization using Triton X- 100 and excess water Sample decomposed with 1 + I HN0,-H2S0 Species stabilized by complexation with Speciation of alkyliodides at ng g-I levels using Study of enhancement effects of butanol on AA and Kerosene solutions formed into emulsions for direct As for Co.Recovery was 93.6% RSD 1.2% As for Cu Comparison of MIP-AES with flame photometric detection for S specific GC. The AES response was less compound specific and LODs were 100 times better Indirect determination of di- tri- and tetra-sulfides by cleavage of S-S bond with NaBH oxidation to SO,2- using boiling H,O,-HCl treating with excess BaZ+ and measuring residual Ba using FAAS chromatographies were used with ICP-AES or ETAAS detection for speciation of seleno compounds Speciation of dimethylselenium and diethlyselenium using GC-ETAAS with specially constructed interface; concentrations in the range 0.14-20 ng were reported Evaluation of capacitively coupled plasma (CCP) as detector for GC determination of organotin compounds Determination of alkyltin species extracted from marine samples using HPLC-ETAAS (C,* column).Comparison with HPLC-MS and GC-MS after methylation compounds in organic solvent. Greatest enhancement ( I 9. I ) obtained for PdCl,(CH,CN) at 10 pg ml-l Pd; LOD=O.l I ng of Sn Speciation of tetra- and tri-organotin compounds using SFC-ICP-MS. Biphenyl 30 column used with CO with and without modifier (methanol) as mobile phase Speciation of alkyltin compounds using LC-ICP-MS with lauryl sulfate as mobile phase and butyl bonded silica gel as stationary phase. Separation accomplished in 20 min with pg LODs Anionic reversed-phase and ion pairing Study of sensitivity enhancement by organopalladium As for La; LOD=0.28 ng ml-1 in aqueous solution As for Al.Signal for Yb enhanced 50-fold using a mixture of sodium dodecyl sulfonate and salicylic acid in 0.1-0.3 mol dm- HCl Reference 92lC503 92/25 17 92lC3493 9213820 92lC455 92lC528 9212244 921 I 704 9 1/40 I4 9 2 1 0 8 5 92lC3637 9211 12 92/C498 92/24 1 1 9113589 921230 9212164 92lC3474 92lC3 I4 1 9212244 92lC458362R JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY DECEMBER 1992 VOL. 7 Table 2 SUMMARY OF ANALYSES OF CHEMICALS-continued Element Matrix Technique; atomization; analyte form* Sample treatmentlcomments Various Surfactants AA;F;L Various Organometallic compounds Various Various Crude drugs XRF;-;S Various Diethylzinc AE;spark;S Various ( 1 1) Chinese traditional medicine AA or AE;F;L Various (20) Organic compounds MS;ICP;L Various Wine AE;ICP;L Various Deuterated derivatization AE; M I P;L reagents Various Organic reagents AF;I CP ; L Various Methacrylic acid M S; I CP; L Various (1 1) Organic compounds AE;F;L Various Pesticide residues AE;MIP;L Various Organic compounds AE; M I P; L (non- metals) Zn Bis-2-ethylhexylphosphoric AA;F;L As for Mn Various (1 5) Dodecylsulfate surfactants AA;F;L Study of the enhancement effects of dodecylsulfate acid surfactants in FAAS with an air-C,H flame.Also study of interference effects of 19 cations in presence of sodium dodecylsulfate Various Water miscible organic AE;ICP;L On-line concentration onto chelating resin followed by washing with ammonium acetate-H,O and elution into ICP using dilute acid.LODs below ng ml-I for Cd Co Cu Mn Ni V and Zn; 2 ng ml-I for Pb Various Halogenated compounds MS;M I P;L Speciation of halogenated organic compounds using HPLC-MIP-MS with C column 70% methanol as mobile phase and an He plasma operating at between 300 and 350 W surfactants in FAAS determination of organometallic compounds on metals profiles in panax ginseng and platycodon gra ndifIoru rn Sample ashed in a closed system with HN0,-H,SO (5+ 1). Resulting oxides mixed with 5% mlm NaCl and Al Bi Ga Ge Pb Sb and Sn determined using spark emission spectrometry Average recoveries 94- 105% Signal enhancements up to 600% observed for As solvents New model proposed for enhancement effect of Review of recent developments in speciation and Study of effect of vegetational period or parts of plant Au Hg Se and Te in presence of glycerol glucose or methane.No effect for other elements studied ( 1 5). Enhancement linked to ionization energy Samples diluted 1 +4 with water and aspirated into plasma directly using Babbington type nebulizer Simultaneous monitoring of C H D I and S using GC-MIP-AES for determination of impurities in CD derivatized immunoenhancer reducing gases on fluorescence intensities of Ca K Mg and Na Matrix effects caused by methacrylic acid solutions (1-10W mlv) could not be eliminated by optimization or use of internal standards. Standard additions recommended selective GC detection using a dual channel flame photometric detector Comparison of GC-MIP-AES with other element specific GC detectors for determination of 10 pesticides in I2 agricultural commodities. AES used for C CI F P N and S selective analyses specific detection with a microbore packed column SFC.Near-IR lines used for C1 and S and UV-visible lines for C and H. LOD=0.8 ng s-I for S Elemental response factors in GC-MIP-AES found to be independent of molecular structure within about 5% RSD for C N and F and 7 and 9% RSD respectively for C1 and 0 Study of effect of changing methanol concentrations on element response during gradient elution LC-ICP-MS using a direct injection nebulizer. Substantial element specific variations observed Determination of ng g-l levels of impurities in stated semiconductor grade solvent using ETV-ICP-MS Transition metals concentrated on chelation column and eluted with HNO prior to ICP-AES analysis Study of the effect of several organic reagents and Conditional acceptance algorithm for element Moderate power (500 W) MIP-AES for element Various Halogenated hydrocarbons AE;MIP;L (non- metals) Various Organometallic compounds M S;I CP; L Various I -methyl-2-pyrrolidone MS;ICP;L Various Pharmaceutical products AE;ICP;L Reference 921 1 704 9 113598 91x3739 9 113908 9 I I3922 9211 16 921320 921333 921338 921 I 240 92lC 1 946 9212526 9212422 92/26 10 9212658 9212 7 2 8 9212 9 7 2 92lC3432 92lC347 1 92lC3696 92lC3 7 7 3JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY DECEMBER 1992 VOL.7 363R Table 2 SUMMARY OF ANALYSES OF CHEMICALS-conlinued Technique; atomization; Element Matrix analyte form* Sample treatmentlcomments Various Ethanol AE;ICP;L LODs improved 5- 1 0-fold by adding 95% ethanol to (rare earths) "C aqueous solution and desolvating aerosol at 300 Various Organometallic compounds M S; 1CP;L Small volumes (25 pl) of organic solvent injected into flowing stream (2 -4 ml min-I) of 2% nitric acid.Sub-ng ml-' LODs achieved when membrane desolvation device incorporated Various Kerosene AA;ETA;L Various Solvents AE;ICP;L Various Solvents AA;ETA;L Various Quaternary ammonium salts AA;FL Various Organic compounds AE;ICP;L Various Emulsions AA;FL Various Organic solutions AE;ICP;L Study of stability of Cu Fe Ni and Pb in kerosene with different complexation reagents and autosampler vials. Dithizone used for Cu and Ni and APDC-acidified H,O-propanol for Fe and Pb were between 0.5 and 90 ng ml-I for Al Cr Cu Fe Na Ni P Pb Si and Zn in xylene kerosene DIBK white spirit and ethanol toluene and xylene) and chemical form in determination of Cd Co Cu Fe Ni and Pb using ETAAS determination of Ag Cd Fe and Zn after extraction into IBMK or xylene in organic media using ICP-AES atomization processes in FAAS determination of Ca Cu Cr Fe and Pb in emulsified organic solvents solutions using ICP-AES.Includes discussion of formation of volatile chelates solvent extraction methods and use with LC Review (48 refs.) on fundamental aspects of effect of organic solvents on ICP High-efficiency r.f. generator gave improved performance for analysis of volatile solvents. LODs for Cd Cu Mn Ni Pb and Zn in methanol were 0.2-1 1 ng ml-* Study of the role of plasma-solvent interactions in incompletely desolvated droplets in the plasma.Consideration of implications for matrix induced errors in practical analysis placed between heated spray chamber and plasma torch. Comparison of direct nebulization with FI into less volatile carrier stream 0 added to auxiliary gas to aid oxidation. LODs Study of influence of solvent (IBMK butyl acetate Study of influence of quaternary ammonium salts on Review (96 refs.) on direct determination of elements Study of effect of surfactant and solvent on Review (77 refs.) on direct analysis of organic AE;ICP;L AE;ICP;L AE or MS;ICP;L Various Volatile organic solvents AE or MS;ICP;L Novel desolvation system utilizing Peltier cooling Various Solvents Various Volatile solvents Various Solvents INORGANIC CHEMICALS AND ACIDS- Ag Coal XRF;-;S Ag Silver halide emulsion SIMS;-;S microcrystals As Electrolytic copper AF;F;L As As Food grade phosphoric acid AA;ETA;L Yellow phosphorus AFHy;L Reference 9 1/38 I 2 921C393 921C345 1 921C567 921C6 13 921952 921 1436 9211 788 9212227 92/24 14 9212420 921C3628 921C3694 9213822 Coal was ashed prior to analysis; LOD of 0.3 ppm 9 11389 1 Direct analysis 9211 399 reported Sample solution treated with KI-ascorbic acid 921 1 799 solution to mask interference from Cu; AsV was reduced to Asrr1 by treatment with tartaric acid-saturated thiourea in 0.15-0.5 mol dm- H,SO or 0.3-1 mol dm- HCI Pd employed as a chemical modifier 0.1-0.3 g of sample dissolved in 15 ml of HNO and evaporated to fuming with 10 ml of H,SO,; the cooled residue was mixed with urea and diluted; an aliquot of this solution was mixed with a 20% HCI solution containing 5% ascorbic acid and 5% thiourea 921264 1 9213974364R JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY DECEMBER 1992 VOL.7 Table 2 SUMMARY OF ANALYSES OF CHEMICALS-continued Technique; atomization; analyte form* AA;F;L Element Matrix Ba Strontium nitrate Sample treatmenticomments 4 g of dried Sr(NO,) + 0.4 g of KCI were dissolved in 100 ml of H,O; the effects of matrix and flame composition were also reported (RCOCH,COCH,;R=C,H,,) employed for isolation of Be 250 g sample dissolved in 250 ml of H,O and boiled with 10 ml of HNO,( 1.4 g ml-I) and a 200 ml portion treated with 20 ml of I 1.3% diammonium hydrogen citrate 5 ml of 2% ammonium pyrrolidine- 1 -carbodithioate solution and 10 ml of CHCI,; the CHCI extract was then collected in 1 ml of HNO and the extraction was repeated twice with 5 ml of CHCI and finally into H,O Method based on sample decomposition with HCl in PTFE container and the resulting tetrachlorogallium was separated by extraction with diisopropyl ether Trace Cu was electrodeposited on a thin tungsten electrode which was then placed in a graphite cup atomizer single crystal was studied by SIMS; the use of the SIMS signal allowed observation of layer-by-layer film growth Combined /?-diketo liquid exchanger Growth of Co thin films on the (1 00) face of a Cu - Less sensitive Fe line (296.7 nm) employed to avoid contamination problems and dilution of samples; the matrix effects of selenate and sulfate anions were studied Samples introduced into the arc in a 1 + 1 mixture containing 0.15% La 0.3% Bi and 0.1% In as oxides; the Bi line at 278.0 nm was used as an internal standard 10 g of sample mixed with 30 ml of H,O and boiled for 5 min with 4 ml of 22% HCI and 3 ml of 10% NaClO then diluted to 100 ml and a 10 ml portion transferred into an aeration flask and treated with 3 ml of 10% hydroxlammonium chloride solution 60 ml of H,O and 2 ml of SnCI Samples suspended in H,O containing 0.02% sodium hexametaphosphate and Hg generated from HCl media by the addition of sodium tetrahydroborate; good aggreement with dissolution procedure with an LOD of 5 ng g-I Samples collected on cellulose filters; good agreement was obtained with a dissolution method employing detection by AAS Method developed for detection of P at sub-ppb levels in H F optimization of method to reduce molecular interferences As in ref.9212274 Pb separated from the matrix by lanthanum hydroxide coprecipitation. The conditions for separation and detection were studied in detail Pb extracted with APDC and NaDDC into IBMK- cyclohexane Method for the selective extraction of Pd in the presence of Pt using quinolin-8-01 and tributylphosphite in CHCI was reported Non-volatile residues formed from deposition of nanolitre aliquots of solution onto high-purity silicon wafers are analysed using a high- performance CAMECA IMS 4f ion microanalyser; S was determined at ppb levels Chemical generation of S as H,S; method based on the quantatitive reduction of SO,,- ion by NaI-HI-H,PO,; LOD of 3.5 ng ml-I S reported Reference 9113936 92lC795 9212274 9212856 9 113929 9211 555 921 I 160 921101 Be Coal fly ash AA;ETA;L Cd Sodium chloride AA;FL Cd Organogallium compounds AA;ETA;L cu High-purity potassium AA; ETA;S bromide c o Copper single crystal SIMS;-;S Eu Coal fly ash Fe Selenium sulfide IDMS;-;S AA;ETA;L Ga Carbonation products Hg Sodium chloride AE;arc discharge$ 921320 1 AA;Hy;L 9212276 Iron(Ir1) oxide and titanium oxide pigments A A;-;SI 92/26 16 Mn Airborne particulates XRF;-;S 92/70 P High-purity acids MS;ETV 1CP;L 92lC3626 Pb Pb Sodium chloride Lithium and lithium salts AA;F;L AA; H y ; L 921227 5 9212736 Pb Pd Sodium sulfite Copper anode slime AA;F;L AA;-;L 9213053 921C3587 S Semiconductor process solutions (ultrapure HCI) SIMS;-;S 54 67 9213 92lC3 S Gallium phosphide AE; 1 CP; LJOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY DECEMBER 1992 VOL.7 365R Table 2 SUMMARY OF ANALYSES OF CHEMICALS-continued Technique; atomization; analyte form* AA;ETA;L Element Se Se Sn Various (2) Various (6) Various Various (5) Matrix Coal fly ash Sample treatmentlcomments Standard HN0,-HClO digestion CdCI,-PdCl chemical modifier used; LOD of 7 pg ml-l reported precision and accuracy of the method determined for the analysis of NIST SRM 1633a HgC1,-PdCl ( 1 + 1 ) evaluated as chemical modifier; Acorbic acid evaluated as a chemical modifier 0.2 g of sample was dried (120 "C) and digested with one of a series of acid mixtures (tabulated) and the digest evaporated to near dryness; acidic H,O was added and the solution diluted to 100 ml Sample dissolved in HCl; wavelength selection was dependent on spectral interferences and required sensitivity Surface analysis with a Grimm-type glow discharge lamp used to analyse uranyl fluoride layers formed on nickel substrate after exposure to UF,; an in-depth profile of layer composition was obtained LA employed for the direct determination of trace elements in carbonate samples; multi-element synthetic standards were prepared as both pressed powders and fused-glass discs FI employed for sample introduction; both internal standardization and standard additions were used Barium hydroxide octahydrate was analysed for trace element impurities by FAAS ICP-AES differential pulse anodic stripping voltammetry and ion chromatography Method LODs range from 0.1 to 3 pg g-I Direct determination of trace metals in sulfur (1 -5 mg sample size).Calibration using aqueous standard provided a L'vov platform was employed; chemical effects due to sulfur removed by pre-heating the furnace to 120- 150 "C Sample solutions in 0.25 rnol dm- HNO contained I g I-' of sodium as ionization buffer. Interference of REEs was suppressed by addition of 5-sulfosalicylic acid Analytes (Ca Mg) were separated from the WO,*- matrix by adsorption at pH 7.5 by cationic- exchange resin (DOOI-ML) and eluted at pH 8.5 with 0.01 mol dm-I EDTA determination of trace element impurities in a variety of samples; LODs in the range 20-100 pg ml-I have been claimed Direct introduction of solutions of Rh compounds Solvent extraction of analytes with ( 1 -phenyl-3- methyl- 4-benzylpyrazolone-IBMK; recoveries ranged from 94 to 106% Performance of ICP-MS evaluated for trace element determination in a variety of reagents Use of a novel U-shaped d.c plasma source was assessed for the analysis of trace elements in high- purity materials plasma using FI; calibration was achieved using standard slurries of previously analysed samples TXRF has been applied to multi-element Samples suspended in water and introduced into the Reference 921171 I 92lC684 9212488 9211 14 921267 921328 Coal fly ash AA;ETA;L Boric acid Fly ash AA;ETA;L AA;F;L High-purity bismuth oxide AE;ICP;L Nickel substrate A E ; G D; S Carbonates MS;ICP;S 921945 Various (3) Concentrated phosphoric acid MS;ICP;L Various (10) Barium hydroxide AA;F;L or and ammonium nitrate AE;ICP;L 921 1 I97 921 1 820 Various ( 14) Lead-acid battery electrodes AE;ICP;L Various (5) Sulfur AA;ETA;S 9211 857 9212060 921223 1 Various (4) Ores AE;F;L AE;ICP;L Various (2) Sodium tungstate 9212449 Various Ultrapure reagents TXRF;-;L 9212778 Various Rhodium compounds Various (7) Alkali metal salts AE;ICP;L AA;F;L 9212564 9212575 Various Semiconductor-grade Various High-purity acids and reagents solvents M S; IC P; L AE;DCP;L 9212879 921298 1 Various (4) Iron oxide pigments AE;ICP;L 9213599 NUCLEAR MATERIALS- 237Np Uranium solutions M S; ICP; L 237Np extracted in a 1 rnol dm- HNO solution using thenoyltrifluoroacetone (0.5 rnol dm-') in xylene; re-extraction of 237Np in 10 mol dm- HNO and dilution of the aqueous phase to I mol dm- HNO prior to analysis simultaneous multi-element monitoring of solutions eluting from ion-exchange columns Photodiode array detector was employed for real time 92x34 19 237Np Spent fuel dissolver solution AE;ICP;L 9113981366R JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY DECEMBER 1992 VOL.7 Table 2 SUMMARY OF ANALYSES OF CHEMICALS-continued Technique; atomization; Element Matrix analyte form* Pu Uranium and thorium AE;ICP;L 230Th Uranium oxide IDMS;-;L U - AE;ICP;L 230Th Pure uranium compounds U - U Radioactive wastes REE Uranium Various (7) Waters and soils Various Actinide matrices Various Nuclear materials Various Uranium and plutonium Various (9) Uranium oxide Various ( 16) Uranium dioxide MS;ICP;L AE:laser;S MS;ICP;L AE;ICP;L MS; ICP; L MS;ICP;S MS;ICP;S L MS;thermal ionization;S AE;ICP;L AE;ICP;L Sample treatmentlcomments Study of spectral interference of Th and U on trace Pu determination Standard sample of uranium oxide spiked with 230Th; analyte separated from matrix by ion exchange Optical emission spectra from high purity normal isotope abundance U generated with a glovebox enclosed ICP; spectral library of U lines from 197 to 700 nm given Simple anion-exchange separation Study of time-resolved emission from the plasma induced by laser ablation of U samples Development of sample dissolution and analyte separation procedures for several sources of wastewater samples Two step liquid-liquid separation procedure in which analytes were complexed with But phosphate in a CC1 medium; final traces of U were removed from the aqueous phase using tri-n- octylphosphine oxide; recoveries were reported to be in the range 90-103% while LODs varied from 0.1 to 9.5 ng ml-' ultrasonic nebulizer was used for the determination of long-lived radionuclides LA-ICP-MS employed in Q-switched mode for the analysis of a variety of SRMs; analyte sensitivity and relative response factors were calulated for common analytes in each matrix natural impurities in non-irradiated fuels fission products spent fuel and reprocessing solutions Complete sample volatilization while simultaneously integrating the signal for each isotope virtually eliminates effects of isotope fractionation in the evaporation process trialkylrnethylammonium chloride-polytrifluoromonochloroethylene (Kel-F) stationary phase Analytes separated from matrix by extraction on TBP levextrel resin column using 3 mol dm-3 HNO as the eluent; the matrix was retained on the column and the analyte elements determined in the eluent High-resolution ICP-MS system combined with an Methods have been developed for the analysis of Analytes separated from matrix using Reference 9 1 I3948 921 1 169 921 1 86 92lC384 9212784 92lC3740 9211717 9113587 92x347 92x350 921 1 004 921 1 804 9212963 * Hy indicates hydride generation and S L G and SI signify solid liquid gaseous or slurry sample introduction respectively. Other abbreviations are listed elsewhere.application provided that an optimum plasma viewing position and support gases are used. Even when chemical speciation is not specifically required problems can arise if analyte compounds are present in the sample in a volatile form.In these cases selective volatilization during sample nebulization can lead to erroneous results. However injection into a GC type injector causes complete vaporiza- tion of the sample thereby eliminating the problem. Beeren et al. (92/C3489) have used such an approach for determi- nation of organomercury compounds at ng g-' levels in light hydrocarbon matrices using a hot injector connected to an ICP-MS instrument via de-activated fused silica tubing (0.53 mm i.d.). The LOD was approximately 5 ,ug 1-I for a 0.5 p1 injection. Determination of toxic metals in solid and oily waste is an area of increasing concern in terms of environmental impact. Methods have been described for the determination of organolead compounds in solid waste by extraction with xylene and determination by FAAS (92/ 159 1) and for the determination of As Sb and Hg in oily waste using HG or cold vapour techniques following high pressure (> 82.2 bar) microwave digestion (92/3839).A method for the determi- nation of stable carbon isotope ratio analysis on single components in crude oils by direct GC-isotope ratio mass spectrometry (92/1607) may also be of interest. 2.1.2. Lubricating oils Determination of additive elements (Ba Ca C1 Cu Mg P S and Zn) in lubricating oils is routinely carried out in many laboratories throughout the world and standard American Society for Testing and Materials (ASTM) and Institute of Petroleum (IP) methods exist for this type of analysis using XRF ICP-AES and AAS.However readers may be interested in two reviews that have been published detailing methods used in the laboratories of two major oil com-JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY DECEMBER 1992 VOL. 7 367R panies (9213072 92/3078). For smaller blending plants the method of choice is often AAS using an N20-air-C2H2 flame (e.g. IP 308). Xueming (92/C3564) has shown that comparable performance can be achieved for the determi- nation of Ba in lubricating oils with an air-C2H2 flame using a mixture of sodium dodecylsulfonate and benzyltri- methylammonium chloride as enhancing agent. If wear metals are to be determined in addition to additive elements then the most commonly used technique is ICP-AES. Again standard methods (e.g.ASTM) exist for these determinations. However the current ASTM methods are very general and do not specify key experimen- tal parameters dilution factor use of internal standard use of peristaltic pump type of nebulizer etc. Jansen et al. (92/C657) have shown that oil additives particularly viscosity index (VI) improvers can have a large effect on nebulizer efficiency and hence analytical results. It was shown that these effects can largely be eliminated by diluting the sample sufficiently and utilizing an internal standard. It is to be hoped that standard methods will be tightened to ensure that such interference effects are eliminated. These workers also studied the effect of wear metal particle size. With normal engine wear metal particle size was found to be less than 1 pm which is well within the range of the ICP technique (up to 10 pm).However ICP- AES is not suited to off-site use such as is required for many military applications. For these a rotating disc electrode spark emission spectrometer has been shown to be more suitable (92/C6 14 92/C65 1). Unfortunately this latter approach is more prone to viscosity effects necessitating that separate calibrations are established for each grade of oil to be analysed (92K3075). Whereas ICP-AES is limited to normal wear application in which wear metal particle size is at most a few pm spark spectrometers have been shown to be capable of detecting identifying and character- izing wear particles up to 40 pm in size (92/3076) allowing less normal wear processes to be identified and studied.If even larger wear metal particles are of interest then it may be necessary to digest the sample completely. Methods based on microwave digestion have been reported for the determination of wear metals in engine oil (92/1680) and lubricating greases (92/3203) using AAS. Very low concentrations of elements in lubricating oil (down to ng g-l) have been determined using TXRF after ashing the prepared sample reflectors in a low temperature oxygen plasma (92/2779). It will be interesting to see what additional information can be provided about wear pro- cesses from the low concentrations of wear metals that would not normally be detected using conventional ap- proaches (early wear detection wear characterization from minor alloy components etc.).Two reviews have been published on atomic spectro- metry of silicone lubricants (92/3924) and X-ray methods for silicone analysis (92/236) and an application of dynamic SIMS to the study of silicone release coatings has been reported (921 1 400). 2.2. Organic Chemicals and Solvents This section of the review covers the analysis of organic chemicals reagents and solvents. Also included is work in the rapidly growing field of chemical speciation of elements. Methods involving preconcentration by extraction into organic solvents are not specifically included since most are used for the analysis of high-purity inorganic compounds or nuclear materials and so are reported in the appropriate sections of the review. The format is essentially the same as in previous years (see J.Anal. At. Spectrom. 199 l,6,283R). A summary of work during the review period concerned with the analysis of organic compounds and solvents is given in Table 2. 2.2.1. Chemicals As with the analysis of petroleum products by far the most rapidly growing area in the field of organic chemicals analysis is that concerned with elemental speciation. One of the biggest growth areas is in the field of environmental analysis since it is well known that certain elemental forms can be extremely toxic while others are relatively innocu- ous. However elemental speciation is equally important in industrial analysis since the ability of a contaminant to poison a catalytic process can also depend on chemical form and the ability to devise processes to remove undesirable contaminants also requires knowledge of the specific chemi- cal forms present.Recent developments in speciation and determination of organometallic compounds in environ- mental samples have been reviewed by Chau and Wong (92/ 1 1 6). The largest number of papers on elemental speciation have been concerned with GC-MIP-AES reflecting the wider availability of robust commercial instruments (91/C3637). The technique can be used in a synergistic combination with GC-MS the latter technique providing compound confirmation and the former providing elemen- tal ratios to aid interpretation of the mass spectrum (92/C3761). This approach has been used to identify impurities in a CDJ derivatized immuno-enhancer (so- dium dithiocarb-imuthiol) and aid GC-MS interpretation of results (92/2526).A comparison has been made of the performance of helium MIP-AES relative to other element selective GC detectors for the analysis of pesticide residues (9212728). It was reported that MIP-AES was the only detector which was suitable for the determination of C1 F and P containing pesticides in all agricultural commodities studied. Specific advantages of MIP-AES indicated in- cluded good specificity and uniformity of response irrespec- tive of chemical structure. Kovacic and Ramus (921C3432) have reported that for a series of halogenated compounds (aromatic aliphatic and heterocyclic) response factors for C N F C1 and 0 were independent of structure within experimental error (about 5% RSD for the first four elements and 9% RSD for 0).Compound independent calibration could therefore be used when individual stan- dards were unavailable or when a large number of analytes had to be quantified quickly. Applications of the use of GC-MIP-AES have included the determination of volatile halogenated hydrocarbons in a public indoor swimming pool air (921C3433) and quantification of polychlorinated dibenzodioxins and polychlorinated dibenzofurans (92/25 3). Whereas non-polar compounds can be analysed directly polar and ionic compounds generally require derivatization to facilitate GC analysis. Rapsomanikis and Craig (92/25 17) have utilized in situ derivatization with NaB(C,H,) for the determination of ionic methylmercury compounds using GC with a quartz furnace AAS detector. A problem which can arise if MIP-AES is used for GC detection of organometallic compounds is that these materials can deposit on the discharge tube walls and later be displaced by hydrocarbon species giving rise to spurious peaks in the element specific chromatograms.One approach to eliminating this problem is the use of a CCP in place of the MIP. Huang and Blades (92/3589) have utilized such a plasma for speciation of orgunotin compounds with LODs of around 0.1 ng s-l. For organometallic compounds and heavy halogens the ICP can also be utilized for element specific GC detection. Kato et al. (9213820) have reported the determination of methylmercury species by capillary column GC with axially viewed ICP-AES detection. The LOD was calculated to be 3 pg as Hg. However approxi- mately two orders of magnitude better sensitivity can be achieved by utilizing ICP-MS as a capillary GC detector (92/C455).In the latter work a novel heated torch was used368R JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY DECEMBER 1992 VOL. 7 to prevent condensation of higher boiling compounds in the ICP torch injector. Good recovery was obtained for compounds with boiling-points in excess of 320 "C. Other novel approaches reported for element specific GC were combination with ETAAS (92124 1 1); injection of organic vapours into a running hollow cathode discharge (9 1/38 10); and use of a dual-channel flame photometric detector with a conditional access algorithm (92/2658). Non-volatile compounds such as most inorganic and ionic forms are generally not amenable to speciation using GC.In these cases some form of liquid chromatography is therefore required. Several forms of liquid chromatography can be used; normal phase; reversed phase; ion chromato- graphy; size exclusion; supercritical fluid etc. A compre- hensive review has been published covering metal specia- tion using various types of liquid chromatography with atomic spectroscopic and other forms of detection (9212599). Atomic emission spectrometers utilizing plasma sources have been extensively used over the years as element specific HPLC detectors. However this approach may have reached maturity since this year has seen fewer reports of applications of this type. Two notable exceptions were the speciation of Hg in chemical waste using HPLC-ICP-AES (92/C3493) and the determination of As- and Se-containing compounds using HPLC with an alter- nating current plasma (ACP) detector (91K3638).In the former application species were stabilized before extrac- tion by complexation with dithiocarbamates. In both cases analytes were introduced into the plasma using post- column vapour generation with sodium tetrahydrobor- ate(II1). Although sensitivity for elements that can be introduced into the plasma in vapour form is generally adequate for most applications sensitivity can be limited if the analyte must be introduced using solution nebulization. In these cases use of ICP-MS rather than ICP-AES can be beneficial. Fischer and Boender (921C499) have reported speciation of As and Se using ion chromatography with ICP-MS detection. Thus A P AsV and dimethylarsenic acid were completely separated in 10 min with LODs ranging from 1 to 5 pg 1-l.Application of LC-ICP-MS (butyl bonded silica gel-lauryl sulfate) has also been reported for speciation of six organotin compounds with LODs in the picogram region (921C3741). For LC-ICP-MS sensitivity and peak dispersion can be improved using a low dead volume direct injection nebulizer. However Houk et al. (92/C3471) have shown that although this system tolerated volatile solvents such as methanol or acetonitrile analyte sensitivity varied substantially from element to element when solvent gradients were used. This might limit applications of this approach to cases when mild solvent gradients can be used. An alternative approach to improv- ing sensitivity is to use ETAAS as an element specific detection system for HPLC.Such an approach has been used for quantification of butyltin species in marine samples (921230) and for speciation of As compounds (92K739). However the duty cycle of the furnace is typically about 40 s which restricts the speed at which data points can be acquired. For speciation of non-metals the ICP is not a suitable plasma source in view of the inability of argon plasmas to ionize elements with higher ionization potentials efficiently. For these elements the helium MIP is generally preferred. Caruso et a/. (9 113908) have used a 500 W helium MIP-MS with reversed-phase HPLC (70% methanol mobile phase) for speciation of halogenated organic compounds. Detection limits were reported to be 50 1 and 10 ng respectively for Br I and C1.Supprrriticalfluid chromatography has attracted increas- ing interest over recent years in view of its ability to allow speciation of non-volatile and thermally labile compounds often with greater speed and resolution than HPLC. Caruso and co-workers have reported application of SFC-MIP-MS for characterization of Cr compounds (92/C3490) organo- tin species (921C3474) and pesticide mixtures (921C3475). The coupling of a microbore packed column SFC with a moderate power (500 W) MIP-AES system has also been described (9212972). Lines in the UV1VIS region of the spectrum were used for C and H but near-IR lines were used for C1 and S. It was found that molecular band interference was a problem in the UV/VIS region with both COz and N20 mobile phases but the near-IR region was affected only As in previous years studies of sensitivity enhancement caused by organic compounds and surfactants in atomic spectrometry has received considerable attention over the review period.Wei et al. (921C458) have reported enhance- ment factors of 10 7.5 and 50.7 respectively for the determination of Al Cr and Yb using FAAS with a C2Hz flame Reagents used were oxine (Al); alcohol + sodium dodecyl sulfate as carrier for FI (Cr) (9 1/39 17); and salicylic acid + sodium dodecyl sulfate (Yb). The influence of different cations on the enhancement effects of dodecyl sulfate surfactants in the determination of 15 elements by FAAS has been studied by Pharr et al. (9113598) and a novel surfactant enhancement mechanism has been pro- posed (9 113922).Organic compounds and surfactants have also been shown to have a significant effect in ICP spectrometry (921 1240 9212422 92/26 10 921C377 1). In particular it has been shown that signal enhancements of up to 600% can be observed for the determination of As Au Hg Se and Te in the presence of glycerol glucose or methane (92/1240) using ICP-MS. No effects were ob- served however for most other elements. The effect appeared to be linked to ionization energy and was most pronounced between 9 and 11 eV. Such problems have led Marshall and Franks (9212610) to recommend use of standard additions to avoid calibration problems in the analysis of methacrylic acid solutions by ICP-MS. Two novel sensitivity enhancement systems have been reported based on vapour generation techniques.Mir et al. (921C578) have reported a detection limit of 0.08 pg for the determination of Co by AAS (flame heated silica tube atomizer) using on-line generation of its chelate with pyrrolidin-1-yldithioformate while Manzoori et al. (921C647) have reported the determination of Cd by ICP- AES. Several indirect methods have been reported for the determination of organic chemicals and other molecular compounds using atomic spectrometry. The pesticide dime- thoxydithiophosphate (DDTP) has been determined using FI-AAS with liquid-liquid back extraction (9212678). The method was based on the formation of the CU(DDTP)~ complex extraction into chloroform and back-extraction using an ammonia solution buffer (pH 10). Flame AAS has also been used for the determination of di- tri- and tetra- sulfides following cleavage of the s-S bonds using NaBH with AlC1 and NH4C1 catalysts oxidation of the produced thiols to and treatment with excess of Ba2+ (921112).The unconsumed Ba was determined using FAAS with an N,O-C2H2 flame. Indirect methods for the determination of some chloride containing drugs and surfactants using ICP-AES have also been discussed (9212454). The methods which are based on precipitation of silver chloride are claimed to exhibit superior accuracy and precision than titrimetric or FAAS methods. by N2O. 2.2.2. Solvents As in previous years most of the work over the review period has concentrated on the effect of organic solvents on ICP sources for AES and/or MS. Three review articles have been published (9211 788 9212414 9212420) that deal with fundamental effects of solvents on ICP discharges optimi-JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY DECEMBER 1992 VOL.7 369R zation analytical characteristics and applications (includ- ing extractions and coupled HPLC). Fundamental studies have been carried out on the effect of solvent and solvent load on the ICP discharge both macroscopically and around incompletely desolvated droplets (9213396 9213694). It was noted that the magnitude and direction of matrix effect errors can be affected by plasma-solvent interactions in these latter regions of the plasma. Analysis of volatile organic solvents is particularly difficult using ICP techniques since the high solvent load produced normally leads to thermal quenching of the plasma.Tyler et al. (921C3628) have shown that this problem can be reduced by using a high-eflciency r.f generator. These workers claimed LODs for methanol that were an order of magnitude better than other published data. Nevertheless band interference from molecules such as C2 and CN can still be a problem and so addition of oxygen to the auxiliary gas flow to aid combustion of organic species is still beneficial (921C6 13). However in view of the matrix effects that can arise from incompletely desolvated aerosol dro- plets and problems that can occur with polyatomic ion interferences in ICP-MS it is generally better to remove as much solvent as possible from the aerosol prior to introduc- tion into the plasma. Ebdon and co-workers (921C393 921C345 1 9213822) have described two desolvation de- vices for the analysis of particularly volatile solvents using ICP-AES or ICP-MS.The first of the devices was based on a heated spray chamber and Peltier cooled condenser while the second made use of a membrane separator for desolva- tion. In both cases improved results were obtained by FI of 25-50 p1 of the volatile sample into a less volatile carrier stream (2-ethoxyethanol or dilute HNO,). This approach was used for analysis of reactive organometallic species such as trimethylgallium and methyllithium. An alternative approach for water miscible volatile organic solvents has been described in which transition metals are removed from the solvent (on-line) onto a chelating resin washed with ammonium acetate solution and then eluted into the plasma with dilute HN03 (9 lK3739).A particularly interesting application of ICP-MS with organic solvents has been described in which solvent (octanol) filled dialysis sacs were placed in water or sediments for extraction of organometallic pollutants (921C3494). The effect of organic solvents on ETAAS has also received some attention over the review period. Unlike FAAS in which the effect of organic solvents can be advantageous owing to improved nebulization efficiency with ETAAS the effect is usually detrimental. Tserovsky and Arpadjan (921952) have studied the behaviour of Cd Co Cu Fe Ni and Pb in various organic solvents (those commonly used in extraction methods) during analysis by ETAAS. The influ- ence of the nature of the solvent complexing agent atomizer type chemical form and amount of modifier were studied and optimum conditions established.With analysis by ETAAS the relatively long analysis times usually necessitate use of an autosampler if large numbers of samples are to be analysed. However for organic samples problems may arise due to adsorption of metals on the vessel walls. Curtius et al. (921C567) studied the stability of metals in kerosene as functions of ligands and vial material. For Cu and Ni the complexes with dithizone were stable for at least 40 min using polyethylene vessels whereas for Fe and Pb the best stability (3 h) was obtained by mixing the organic solution containing the ammonium pyrrolidin- 1-yldithioformate complexes of the metals with acidified water and adding enough propan- 1-01 to make a one-phase solution.Vessels made of PTFE were best for Fe and quartz vessels for Pb. Sensitivity enhancement of 19-fold were reported for the determination of alkyltin compounds in organic solvent by ETAAS using 10 pg ml-' of Pd added as PdCl,(CH,CN) (9212764). Of the solvent extraction methods used for sensitivity enhancement Radecka and Radecki (921C585) have shown that cyclohexanone gives superior performance to IBMK for the extraction of Cu and Pb as their APDC complexes while Chen et al. (9212244) have reported enhancement factors of 3.6 and 11.9 for the determination of La and Y respectively by ICP-AES and extraction with PMBP ( 1 -phenyl-3-methyl-4-benzylpyrazolone)-acetate at pH 5.5. A novel preconcentration technique has been reported by Garip and Thompson (9211635) in which transition metal cations could be concentrated from aqueous solution by foam fractionation using chelating surfactants. A 50-75- fold increase in concentration was reproducibly achieved for solutions containing Cu in the ng ml-1 to pg ml-1 range with determination by FAAS.2.3. Inorganic Chemicals and Acids 2.3.1. Chemicals As with previous ASU reviews a significant number of abstracts were received concerning the application of atomic spectrometric techniques to the analysis of samples containing high dissolved solids. In the chlor-alkali industry the transition from traditional mercury cells to new membrane cell technology for the electrolysis of brine has placed more stringent demands on the required purity of brine feed stocks.Trace level impurities can quickly cause blockage of cell membranes which leads to reduced cell efficiency and ultimately to costly replacement of mem- branes. High solids analysis has traditionally been a problem when using ICP-AES. Despite improvements in nebulizer designs to address this problem at very high salt concentrations these nebulizers may still suffer from block- ages. An evaluation of the performance of several nebulizer designs applied to the analysis of high dissolved solids has recently been presented (921C3764). Concentric C-type and Babington V-groove set-ups were examined and the effect of sample bore size and nebulizer geometry assessed. A standard high precision concentric nebulizer in series with a high solids accessory was also employed in combination with a multi-channel polychromator for simultaneous multi-element analysis of concentrated salt solutions.The high solids accessory allowed a continuous flow of rinse solution to the nebulizer and spray chamber. The sample was introduced in 100 pl slugs to this rinse system. This enabled the sample introduction system to be continuously flushed preventing blockages. In contrast another applica- tion reported that the use of a wide bore injector tube combined with the use of humidified argon allowed saturated brine solutions to be nebulized in a stable manner for hours without the need of a high solids nebulizer (911C3741). Detection limits in the low ppb range were claimed using this procedure. Other applications to brine analysis received in this review period included the deter- mination of iodide and iodate by helium MIP (91/3971) and the analysis of heavy metal impurities by FAAS following an extraction procedure (92/40 16).Direct analysis of sea-water using electrothermal vapori- zation into an ICP has also been reported (921C3293). The transport efficiencies of elements of interest were deter- mined by collection of the aerosol exiting the injector tube on a series of stacked depth and membrane filters. Analyte transport efficiencies were typically greater than 50%. Attempts were also made to correlate matrix effects with variabilities in sample transport morphological differences in the aerosols and excitation potentials of the analytical lines of interest. The use of ETAAS combined with chelation ion exchange has also been applied to the analysis of sea-water (921C3704).Preconcentration and matrix elimination was achieved by the use of a Dionex chelating resin (Metpac-CC1) in an off-line mode. A series of papers370R JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY DECEMBER 1992 VOL. 7 detailing methodology for the analysis of sodium chloride by FAAS have been published by the British Standards Institution. Methods for Cd (92/2274) Hg (92/2276) and Pb (92/2275) have been described. In each case trace metals were separated from the salt matrix by solvent extraction. The analysis of lithium salts has also received attention. Lead was determined in lithium and lithium salts by HG- AAS following a lanthanum hydroxide co-precipitation separation procedure (92/2736).In addition Ca and Mg were determined by FAAS following extraction from the matrix by PMBP-IBMK at pH 7.2. The requirement to provide high-purity chemicals and reagents for a wide variety of industries has resulted in an increased demand for trace level determinations in these materials. This is evident in the present review by the increased number of abstracts received relating to the analysis of high-purity chemicals. Thus FAAS ETAAS and ICP-AES have been applied to the determination of impurities in vanadium disilicate and vanadium pentoxide (9212485). The matrix was removed by ion-exchange separation after converting the vanadium into an anionic Vv peroxide complex. An ETAAS method has been reported for the determination of Fe in selenium sulfide; magnesium and nickel were employed as chemical modifiers.Trace amounts of Re have been measured in copper sulfide samples by ICP-AES (92/2935). Two differ- ent methods of sample decomposition were employed oxidative alkali fusion and acid dissolution. A combination of ICP-AES differential anodic stripping voltammetry and ion chomatography were employed for trace element analysis of barium hydroxide (92/ 1820). The analytical procedures employed were discussed with respect to matrix interference effects. The rapid determination of trace metal impurities in high-purity bismuth oxide by ICP-AES has also been reported (92/267). Other applications published in the year under review included the determination of Ca and Mg in sodium tungstate by ICP-AES (92/2449) Cu and Ni in pure barium nitrate (92/2737) Cu in highly pure potassium bromide by ETAAS (92/3929) and Ba in stron- tium nitrate by FAAS (9113053).Ultra-pure chemicals such as mineral acids ammonia solution hydrogen peroxide and organic solvents are applied in different process steps in the semiconductor industry (see also section 3.2 of this review). The higher the integration density of the chip production the more the chip yield is limited by extremely low trace element contamina- tion of the applied process solutions. Suppliers of electronic grade chemicals must guarantee maximum trace levels of up to 40 elements in the lower ng g-l range. Considerable effort has been expended to develop methods of analysis to meet these exacting requirements. A review of the perform- ance of ICP-MS applied to the direct analysis of semicon- ductor-grade reagents has been published (9213064).Micro- volume SIMS has been applied to the determination of non- volatile S residues in semiconductor process solutions (92/3 1 54). Residues formed from the deposition of nano- litres of samples were analysed by dynamic SIMS which offered the capability to detect and quantify S in ultrapure HCl solutions used in gallium arsenide wafer fabrication. High-purity corrosive gases used in semiconductor manu- facturing present problems not only in production storage and handling but also with regard to sampling and trace element analysis. A method has been described for the sampling and analysis of hydrogen chloride for trace metal impurities (92K3389).A method for the determination of Si in ultra-pure acids using ETAAS has been reported (92/C375 1). Problems due to contamination were controlled by operating with clean rooms (class 10000) and clean bench (class 10) facilities. Under these conditions it was shown to be possible to determine Si in aqueous solutions free from environmental contamination. In some cases the LODs available with state-of-the-art techniques are not sufficient for some semiconductor applications. In such cases some form of preconcentration or enrichment step is required prior to analysis. A new closed apparatus for the evaporation of samples for preconcentration of sample solutions used primarily in semiconductor production has been described (92/36 15). The principle is comparable to sub-boiling distillation.The sample was heated from above using an IR heater and the vapour produced condensed at a cold finger and the condensate collected in a U-shaped glass tube. The system has been used for the evaporation of ultrapure water HC1 HN03 H,SO and ammonia solution samples. Using this apparatus ETAAS detection limits of 0.05 ng g-1 were reported even for ubiquitous elements such as Ca Fe and Na. Atomic spectrometric techniques continue to be widely applied in the electroplating industry for the analysis of electrode materials plating bath solutions and waste pro- cess streams. Thus FAAS has been applied to the determi- nation of heavy metals present at high concentrations in electroplating waste sludges (9212576). The use of ICP-AES for the determination of 14 trace element impurities in Pb-acid electrodes has also been reported (921 1857).Impurities in carbon anodes employed for the electrolysis of aluminium have been determined by AES (9212263). Other reported applications included the determination of Pd in copper anode slime (92/C3578) major and minor trace elements in plating solutions by FAAS and chrome in chrome-acid plating solutions by flame emission spectro- metry (9213790) and Mn in airborne particulates in a dry- cell battery factory by XRF (92/70). A significant increase in the number of abstracts relating to the analysis of coals and fly ash was observed compared with previous reviews. This undoubtedly reflects increased environmental awareness and more stringent controls on power station emissions.A rapid and accurate method for the determination of major and minor elements in coal by ICP-AES with slurry sample introduction was described (92/305). Optimization of slurry preparations such as optimum coal and surfactant concentrations and sample grinding regimes were reported. Also ETAAS was em- ployed for the determination of Se in coal fly ash (92/C684). A mixed mercury-palladium modifier was employed and the validity of the method assessed by analysis of NIST SRM 1633A Coal Fly Ash. In an alternative method Se was determined in coal fly ash by ETAAS employing a conven- tional HN03-HC104 sample dissolution. A cadmium-pal- ladium modifier was employed in this case. Using this procedure no spectral interferences were reported from iron or chlorine and an LOD of 7 pg 1 - I was achieved (92/17 1 1).In another application SIMS X-ray microanalysis and SEM were used to investigate the surface characteristics and depth profiles of coal fly ash (92/1561). Coal fly ash particles were size fractionated magnetically separated and mounted in a 6 mm diameter holder. Large particles (100 pm) were then analysed. Other applications reported were mineral speciation of Cu and Zn in fly ash using FAAS (92/114) determination of Be in fly ash by ETAAS following a liquid chelating extraction procedure (92/C795) and the determination of trace amounts of Eu in coal by isotope dilution-MS (921 1 160). Laser ablation ICP-MS has been applied to the analysis of carbonate materials (92/945). Multi-element synthetic stan- dards were prepared as both pressed powders and fused discs.The elements Ba Mg Mn Pb and Sr were added to the pressed powder standards and these elements together with U were added to the fused discs. Calibration graphs for both synthetic standard types were linear over three orders of magnitude but the fused disc standards gave more precise results. The accuracy of the technique was assessedJOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY DECEMBER 1992 VOL. 7 371R by the analysis of SRMs. Other articles of interest received during the period under consideration included a review of inorganic MS in agriculture (92135); determination of trace elements in phosphate fertilizers and animal feeds by ICP- MS (9113667); the determination of Cu Cr Mn and Zn in iron oxide pigments using FAAS with FI slurry sample introduction (9 113599); and a cold vapour atomic absorp- tion method for the determination of Hg in iron(I1) oxide and titanium oxide pigments employing slurry sample introduction (92/26 16).A review examining future trends in the application of XRF in the cement industry was also published (9211 930) 2.3.2. Acids There have been fewer abstracts received relating to the analysis of acids in the year under review (although there is a degree of overlap with abstracts relating to the analysis of semiconductors) Total reflection X-ray spectrometry has been applied to the analysis of a number of ultrapure acids (9212778). This technique would seem to be ideal for this type of application in that it offers a rapid and sensitive method of analysis with minimum sample preparation.Thus a 100 pl volume of sample was sufficient for complete multi-element coverage. Detection limits in the range 20- 100 pg ml-I have been obtained. Using preconcentra- tion procedures LODs below 5 pg ml-l have been claimed. The reliability of the sample preparation procedures and the accuracy of the technique were assessed by independent analysis of duplicate samples using ICP-MS. An ETV-ICP- AES method for the determination of P in HF has been reported (921C3626). Data were presented on the optimiza- tion of the method to reduce polyatomic interferences and an LOD of 1 pg 1-l was claimed. The determination of Ge Pd and Pt in highly concentrated solutions of H3P04 and NH4N03 by ICP-MS using FI sample introduction has been reported (92/ 1 179).It was reported that selection of sample and skimmer sets together with the use of two isotopes per element for measurement minimized interference effects. Both internal standardization and the method of additions were used. The use of a U-shaped d.c. arc plasma source in the determination of trace elements in high-purity acids and solvents by AES has been described. The technique has been compared with ICP-AES (921298 1). The determina- tion of As in food-grade H3PO4 by ETAAS using Pd as a chemical modifier was reported. (92/264 1). 2.4. Nuclear Materials Analysis using atomic spectrometry continues to play a vital role in all aspects of the nuclear industry from nuclear fuel fabrication to monitoring and quantifying waste products prior to disposal.The ability to provide both elemental and isotopic information at trace levels makes ICP-MS an invaluable tool in the nuclear field and the growing number of reported applications provide evidence of its acceptance within this industry. However the methodologies employed for the analysis of nuclear ma- terials must take into account the different and in many cases unknown isotopic abundances compared with those encountered in naturally occurring samples. Consequently most determinations must reflect isotopic rather than elemental determinations. Methods for the analysis of natural element impurities in non-irradiated fuels for fission products actinides in spent fuel and for actinide impurities in reprocessing solutions of Pu and U by ICP- MS have been reported (921C350).The requirement to monitor long-lived radionuclides in the environment is of considerable importance in ascertaining long term radia- tion effects on humans and the demand for such measure- ments has dramatically increased in the ‘post Chernobyl era’. Conventional ICP-MS is limited in its application in this area due to the effect of molecular interferences below m/z 80 and because of insufficient sensitivity to determine some radionuclides directly in environmental samples. To address this need a high-resolution ICP-MS system employ- ing an ultrasonic nebulizer has been applied to the measurement of long-lived radionuclides (9 1/3587). A ten- fold gain in sensitivity using the ultrasonic nebulizer was reported. At low concentrations more accurate isotopic information was obtained by employing the high-resolution instrument compared with a conventional quadrupole system by virtue of the improved counting statistics resulting from the greater efficiency of ion transmission in the high-resolution instrument.The ICP-MS method has also been applied to the analysis of radioactive wastes in ground waters surface waters and other forms of aqueous wastes (92/C3740). Developments in methodology for sample dissolution and chemical separation in addition to instrumental optimization for the analysis of both total uranium and its isotopes were described. The determina- tion of traces amounts of 237Np in enriched uranium solutions by ICP-MS has also been reported (921C34 19). In this procedure the 237Np was extracted by 0.5 mol dme3 thenoyltrifluoroacetone in xylene and re-extracted in 10 mol dm-3 HNO and finally diluting to 1 mol dmw3 HN03 prior to ICP-MS analysis.A commercial LA system has been modified for hot cell operation (921C7 10) and applied to the direct analysis of a number of radioactive materials using ICP-MS. Inductively coupled plasma AES continues to enjoy widespread use in the nuclear industry. However the complex nature of the spectra produced from such ma- terials means that in the majority of cases some form of extraction1separation is required prior to analysis. The separation of some REE from a uranium matrix by a two step liquid-liquid extraction procedure and analysis by ICP- AES has been described (92/17 17). The first stage involved the separation of the REE by complexing with tributyl phosphate in carbon tetrachloride.The second stage in- volved the use of tri-n-octylphosphine oxide for the removal of the residual traces of uranium from the aqueous phase. Recoveries of REE obtained using this method were in the range 90-103°/o while the LODs achieved by ICP- AES ranged between 0.2 and 9.5 ng ml-l. Reversed-phase partition chromatography has been employed for the pre- separation of the uranium matrix prior to analysis of trace elements by ICP-AES (92/4030). A paper detailing an ICP spectral atlas for uranium has been published (92/186). Optical emission spectra from high-purity normal abun- dance uranium were generated using a glovebox enclosed ICP. Spectra covering the range 197-700 nm were docu- mented and a general commentary on uranium ICP spectroscopy was presented. A number of abstracts have been received concerning the application of XRF in the nuclear industry.The determination of Fe and Ti in uranium by EDXRF was described (9213903). Combined gamma and passive XRF measurements have been employed for the measurement of 23sU enrichment and total U concentrations (92/3902). A review has been published detailing the present status of radionuclide determination in coals using XRF (9 114028). 2.5. Process Analysis and Automation The main emphasis in abstracts received relating to laboratory automation were concerned with automation of front-end sample introduction and sample preparation. An inexpensive automated system capable of multi-component standard preparation was described (9 1 /3670).This proto- type system was constructed from commercially available372R JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY DECEMBER 1992 VOL. 7 inert valves which were controlled from a PC. The system also performed automated sample spiking and could be used in conjunction with a laboratory robot. Similarly the analytical performance of an automated samplehtandard preparation system for AAS has been described (921C3701). An apparatus for automatically introducing organometallic samples to an ICP has been reported (9213 12 1 ). The liquid sample stream was continually injected into a heated stream of argon gas which was introduced continuously into the plasma. A fuIIy automated fusion system for rapid sample preparation of fused beads for XRF analysis has also been described (9213725).The system was capable of high-temperature borate-type or low-temperature peroxide fusions. An automated system for the dissolution of titanium oxide employing a microwave oven and a labora- tory robot has been reported. The system weighed out samples added acid carried out microwave digestion diluted the solutions transferred the solutions into breakers and cleaned the digestion vessels. The system was able to process 60 samples in 16.5 h (921600). A robotic system for the preparation of Ta powder for trace analysis was also reported (921225). 3. ADVANCED MATERIALS Developments made in analytical techniques and methodo- logy for the analysis of advanced materials are reviewed in this section of the Update.The key areas in which progress has been reported in the past year are highlighted in the text. A comprehensive summary of reported analytical methods of relevance to the characterization of advanced materials is provided in Table 3. 3.1. Polymers and Composites The materials encountered in the pIastics industry are enormously varied in terms of chemical composition. Base polymers which themselves can be extremely pure in respect of trace element content may be formulated with selected compounds from a vast range of additives (e.g. pigments fillers fibres and flame retardents) in order to achieve particular physical properties. The requirements for analysis range from highly accurate precise and rapid bulk quantification at the per centage level to spatially resolved lateral and depth profiling for trace constituents.Consequently no single analytical technique is likely to be suitable for all applications in this field. The diversity of the approaches which can be employed is evident from the literature. The major disadvantage of using ICP- or flame-based instrumentation for the analysis of plastics is the time required for sample preparation. Some materials containing polymers are soluble in aqueous solution (92/2207) but most sample preparation regimes rely on aggressive ap- proaches involving acid digestion and often employing oxidants such as hydrogen peroxide which can be used for the digestion of poly(viny1 chloride) (9212604 921C3653). Wet oxidation is the method of choice for the determina- tion of P as it prevents the losses of volatile species but conventional hot-plate acid digestion procedures can be relatively slow.This is particularly true for high-perform- ance polymers which have characteristics of high strength and modulus and are resistant to the effects of elevated temperature. A method for the determination of P (present as polyphosphoric acid) in poly(p-phenylenebenzobisoxya- zole) a rigid rod aromatic heterocyclic polymer was described in which microwave technology was used to speed up the digestion process (921C3355). The film was decomposed in H2S04 and HN03 and the resulting solution analysed by ICP-AES; and the method was validated using spiking and an independent standard. A spectral interfer- ence from sulfur (due to the acid) was identified at the 178.290 nm P line but this could be avoided by use of alternative wavelengths at 213.620 and 214.914 nm.The use of hot corrosive acids in sample preparation procedures often presents a safety hazard and for this reason automa- tion of such methods can be desirable. A system based on a labovatory robot has been developed for the determination of trace metals on the surface of epoxy laminates used in the manufacture of printed circuit boards (92/224). The method involved the immersion of the circuit board in a mixture of hot HN03 and HCl followed by detection of metals in the resulting solution by plasma AES. Some of the system hardware was modified to perform in a corrosive environment and it was reported that the potential for acid spillage and related accidents was much reduced.The system also provided a shorter analysis time for quality assurance testing. Polymers are now increasingly used in preconcentration methods and a number of papers on this topic have been published in the past year. These included the synthesis and use of chelating and polymeric resins such as phospho- ramidate for Ga and In (921409); tercopolymeric resins involving 8-hydroxyquinoline and resorcinol-hydroqui- none for Cd and Zn (921423); macroporous poly(viny1 amidine thiocyanate-thiourea) for Be Cr Cu La Ti V and Y (921 1693); poly(dithi0carbamate) for platinum group metals (921C3387); polyacrylonitrile for Co Mn and Ni (9211633); and polyurethane for Au Pd and Pt (92/58 921 1 66). Other abstracts concerning polymers which are indirectly associated with AS procedures included the investigation of blanks for S arising from synthetic tubing used in argon supply lines for ICP-AES (92/2625) and the use of PTFE slurry to prevent the formation of carbides in the determination of refractory elements by ETV-ICP-AES (91/3590). X-ray methods remain popular for direct analysis.Solid and relatively inexpensive energy dispersive XRF instru- ments are finding increasing application in quality control of engineering plastics (921C3714) and in screening of paints for Pb for example (91lC3733). Wavelength disper- sive instruments employing multi-layer crystals are increas- ingly being used to detect elements of low atomic number and analytical performance data have been published for the determination of F in fluoro-polymers (921 199).Total reflection XRF is now a well established branch of the technique and a review of applications including polymers has been published (9114037). An overview of the applica- tions of PIXE to quantitative trace element determination including an examination of polymer insulation for high- voltage cables may be of interest (9 113955). The characteri- zation of polyaniline thin films on stainless-steel and titanium alloy substrates has been carried out using low energy electron induced X-ray spectrometry XRF and GD- AES (921C667). The growth of the films via an electrodepo- sition route was monitored by examining the degree of incorporation of sulfate anions. Since polyanilines are conducting polymers this facilitated the application of GD- AES which was used for depth profiling.Surface analysis continues to be an important topic in the materials field and reviews on the application of SIMS (92/ 1305) electron- and ion-beam analysis (9211210) and RIMS (92/1578) have been published. The use of charge compensation in imaging of insulator materials by time-of-flight SIMS has been described (921956). The system was applied to the examination of PTFE-glass fibre and silicone-contami- nated polypropylene fibre electrical insulators. Lateral imaging and depth profiling SIMS studies have also been carried out on spatially modified polymers (92/24). ItJOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY DECEMBER 1992 VOL. 7 373R Table 3 SUMMARY OF ANALYSES OF ADVANCED MATERIALS Technique; atomization; analyte form* Element Matrix POLYMERS AND COMPOSITES- Sample treatmentlcomments Reference 9211855 921331 92lC365 3 9213 I50 9 1 I3964 9213205 9212207 921 I99 921 I83 92lC3 35 5 921 1855 91x3733 92123 1 92lC667 9213 150 9213 106 92lC3646 92lC3646 9211678 92lC3646 921 1678 9 llC3734 Ba Cd Cd C1 Cr Cr c u F N P Pb Pb S S S Sb Sb Si Ti Ti Zn Acrylate-styrene copolymers Leather X-ray absorption Preparation and characterization of metal diacrylate containing polymer for X-ray protection Samples were treated with sulfuric acid and H,O for the determination of Cd at levels of 2 ppm and above; recoveries were in the range 97- 100% with addition of H,O,; analysis using tungsten coil atomizer indirect determination at 338.29 nm Ag line with LOD of 5 ppm HN0,-H2S0 at 45 “C for 1 h and diluted with water and CaCI solution Dissolution of sample in 2 h using HN03-H2S0 Recovery of chloride by precipitation with Ag and Sample was ground digested in concentrated Review article with 31 ref.Dissolution of polymer complex in water and analysis using an air-C,H flame; no interference found from 400-fold excess of polymer for detection of Cu in range 0.5-3 ppm proportional counter and a multilayer AX06 crystal; detection in the range 120 ppm to per cent. levels Study of interaction between N-containing excited species in the plasma and surface interactions with polymer Microwave digestion using H,SO and HNO,; spectral interference from sulfur avoided by using 2 14.9 14 nm P line Measurement of Ka line for 30 s using a flow As for Ba Samples were ground to 200 mesh to remove homogeneity errors and analyte detected in the range 0.06-2.2% mlm by energy dispersive instrumentation employing a Io9Cd radioisotope source Wet digestion of sample in open vessel Measurement of sulfate incorporation in films and levels of dopant; correlation with GD-AES depth profiling Sample prepared using ammonia solution and calibrated using 1% vlv matrix matched standards; detection using 182.04 nm S line Dissolution of antimony-based finishing paint coating AA;F using slotted tube;L PVC AA;ETA;S Polymers AE;ICP;L Leather AA;F;L Leather Polymer metallo-complexes AAi-i- AA;F;L Fluoropolymers XRF;-;S Polypropylene AE or MS;corona disc ha rge;- Poly(p-phen ylene benzobisoxyazole) AE;ICP;L Acrylate-styrene copolymers Paint X-ray absorption XRF;-;S Wool Polyaniline thin films AE;plasma;L XRF;-;S Polymers AE; I CP; L Dried paint Rubber Si-containing polymers Dried paints Plastics Dried paints AA or AE;F or 1CP;L AE;spark;S AE;spark;S AA or AE;F or 1CP;L AE;spark;S AA or AE;F or 1CP;L XRF-;S Direct analysis using novel ‘sliding spark’ excitation Direct analysis using novel ‘sliding spark’ excitation Dissolution of dried paint sample source source Direct analysis using novel ‘sliding spark’ excitation As for Ti source Various (4) Paint on steel Measurement of paint thickness using Compton X-ray scatter from the painted steel sheet and intensity corrections for presence of C Fe Mo and Ti preferred to aqueous measurement dissolution in hot HCI and HNO using robotic protocol Study of adhesion of sputter cleaned polyimide to metal surfaces by detection of Cr Ti and Zr Dissolution of dried paint sample and detection of Cr Fe Ti and Zn Detection of Ba Cd P and Zn in organic media Quantitative measurement of trace metals by Various (4) Vinyl stabilisers Various Epoxy laminates AE;ICP;L AE;plasma;L 9212 I9 921224 Various (3) Metal-polyimide interfaces SIMS 9211414 92t 1676 Various (4) Dried paints AA or AE;F or 1CP;L374R JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY DECEMBER 1992 VOL.7 Table 3 SUMMARY OF ANALYSES OF ADVANCED MATERIALS-continued Technique; atomization; analyte form* AA or AE;F or 1CP;L AA;F;L Sample treatmentlcomments Analysis of dirt resistant paints for Cu Sn and Zn using a dissolution method Comparison of dissolution using H2S0,-H,O,-NH,OH-EDTA procedure and H,SO,-H,O,-HNO method Direct analysis of metals in polymers in the range 10 ppb-% mlm levels; precision values of 5% RSD reported Direct solid sampling for the detection of Cr Cu Co Fe Mn and Ni; water extraction for Na; comparative data from NAA and synchrotron radiation XRF fundamental parameter method used in estimation of concentration with single standard for up to five inorganic fillers Sample presented in disk or pellet form and Reference 9211679 9212604 921C3454 92lC354 1 921C37 14 9212 1 72 921388 1 921 1 326 9212353 9213063 92/C47 1 921 1 326 9211 337 921 1 340 9212296 9212353 921C3609 Element Matrix Various (3) Dry paint Various (4) PVC Various Polymers MS;LA and 1CP;S Various (7) Polycarbonate AA;ETA;S or L Various (5) Thermoplastic compounds XRF;-;S SEMICONDUCTORS- A1 Al As As As B B B B B B B Be Be C C C Ca cu Silicon substrates Germanium and silicon SIMS MS; ETA;S Study of re-distribution of ion implanted A1 Samples were evaporated electrothermally in vacuo and atoms were excited using laser radiation prior to detection by time of flight MS; LODs of 0.1-0.2 ppb were reported Study of effect on primary beam parameters were investigated to optimize detection in shallow junctions Quantitative depth profiling Silicon SIMS Molybdenum silicide- Silicon silicon layers SlMS AA;ETA;L Depth profiling by chemical etching; the use of Direct determination As for As Quantitative analysis for B in a silicide sample; error Quantitative detection of B impurity Study of matrix effects on accuracy of quantitaitve As for As platforms and chemical modifiers was studied correction in dopant profile analysis MS;spark;S SIMS SIMS SIMS SIMS Silicon Silicon Semiconductor Silicon dioxide-silicon layer Silicon Molybdenum silicide- silicon layers Silica and silicon SIMS AE;ETV-1CP;L Analyte was extracted with ethyl violet into toluene and vaporized at 1400 "C in a reducing hydrogen atmosphere to improve sensitivity LOD of 1 ppb reported Depth profiling of Be doped structures grown by molecular beam epitaxy Depth profiling of Be as dopant Novel discharge cell accommodating flat samples was used for determination of C at sub-ppm levels Detection of the SbC polyatomic ion was found to improve sensitivity 3-fold Use of load line calibration technique to achieve reproducibility of 4.5% in quantitative determinations Pre-volatilization used to remove gallium up to 0.3% mlv in an HNO medium to avoid interference on Ca; LOD of 0.057 ppm Ca reported Sample masses up to 20 mg analysed directly by ET volatilization into flame and response calibrated using aqueous standards; LOD of 0.1 ppb reported by mechanochemical polishing Quantitative analysis for Cu introduced into silicon Quantification of F levels on HF-treated surface Sample was diluted 7-20-fold with 2-ethoxyethyl acetate and introduced directly into ICP-MS system using oxygen gas to remove C deposition on cone; LOD was 1 ppb 921967 Galium arsenide layered structures Aluminium gallium arsenide Silicon wafers RIMS RIMS MS;GD;S 9211421 921C339 Indium antimonide SIMS 921975 Silicon SIMS 9212340 Gallium AA;ETA and ETA-F;L 921C769 High-purity germanium LE1;ET and F S and L 92lC5 86 c u Silicon SIMS and XPS 921 1278 F Silica-silicon substrates Fe Photoresist SlMS and XPS MS;lCP;L 921 1 244 9211 163JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY DECEMBER 1992 VOL.7 375R Table 3 Element Fe Fe Fe Ga Ga H H In SUMMARY OF ANALYSES OF ADVANCED MATERIALS-continued Technique; atomization; analyte form* SIMS Matrix Indium phosphide Sample treatmentlcomments Spatial investigation of Fe concentrations in doped ingot Measurement of Fe contamination in non-uniform highly luminescent regions of sample on the micrometre scale Pre-treatment by ashing or dilution 7-10-fold with organic solvent; LOD of 0.2 ppb reported Films were dissolved in aqua regia evaporated and mixed with internal RMs As for As Methods of overcoming gaseous residual contaminants to achieve low LODs Quantitative analysis in good agreement with NAA method Sample masses up to 20 mg analysed directly by ET volatilization into flame and response calibrated using aqueous standards; LOD of 0.001 ppb reported Sputter coating of platform with sample addition of dilute HNO in situ and direct atomization in ETA; detection of In at a concentration of 600 PPm Sputtered neutral volatilization combined with resonance ionization MS used to eliminate isobaric interferences; LOD of 0.3 ppb reported Comparison of methods for determination of In- based compounds As for Ga Study of Li depth profile in sample aged over a six As for Fe As for Fe Non-destructive method for quantification of Ni; As for C Improved method for quantitative distribution of 0; year period accuracy confirmed by FAAS repeatability 2 4 % relative and accuracy of within 1Ooh reported Quantitative determination of 0 using the load line calibration method; reproducibility of I-2% reported Quantitative determination of intersitially dissolved oxygen with a repeatability of 3% relative As for B Indirect method based on formation of bismuth phosphomolybdate complex and extraction into IBMK; detection of Bi at 223.06 nm line Quantification of S in thin films Reference 921 1280 92/C 1449 9 2 x 3 5 38 921294 1 92/3063 92/ 1 608 92/280 1 92/C586 92/C778 9211 325 921 I8 10 921294 I 921966 9211 163 92lC3538 9212804 92/C339 92/23 16 9212344 9212796 92lC47 1 9212452 921994 9 113856 92lC 1449 921 1245 9 llC368 1 91lC3681 921334 9 2 x 5 3 2 92lC696 Indium phosphide SIMS Photoresist MS;ETV-ICP;L Gold films contacts AE;-;S Silicon Semiconductors AA; ETA; L SIMS Silicon-germanium alloys SIMS Cadmium mercury telluride LE1;ET and F;S and L In Cadmium telluride single crystals AA;ETA;S Silicon RIMS;-;S In In Semiconductors Gold film contacts Cadmium mercury telluride Photoresist Photoresist Silicon wafers XRF or AA or AE;FS or L AE;-;S SIMS In Li Na Na Ni MS;ICP;L MS;ETV-ICP;L XRF;-;S 0 0 Silicon wafers Czochralski-silicon MS;GD;S SIMS 0 Silicon SIMS 0 Czochralski-silicon SIMS P P Silicon High-purity silicon MS;spark;S AA;-;L S Si Cadmium telluride-cadmium sulfide films Semiconductors Electron probe MS;ICP;L Si was volatilized from acid dissolution mixture as tetrafluoride complexed to form molybdosilicic acid prior to indirect determination of Si as molybdenum As for Fe Study of doping of Sn in indium phosphide grown by Application of tungsten coil vaporization for molecular beam epitaxy introducing microlitre samples; detection down to 0.01 ppb for a I g sample As for Th Preconcentration of trace impurities by chelation with hexamethylene ammonium hexamethylene dithiocarbamate extraction chromatography platforms and Ni Mg and Pd nitrates as chemical modifiers to remove interference effects Separation of In from impurity elements by Layer by layer chemical etching of substrates; use of Si Sn Indium phosphide Indium phosphide SIMS SIMS MS;ICP; L Th Semiconductors U Various Semiconductors Silicon and germanium tetrachlorides MS; ICP; L AA;ETA;L Various Indium and indium phosphide Semiconductors AE;ICP;L Various ( 13) AA; ETA;L376R JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY DECEMBER 1992 VOL.7 Table 3 SUMMARY OF ANALYSES OF ADVANCED MATERIALS-continued Element Various ( 4 ) Various (4) Various (4) Various (3) Various (6) Various ( 3 ) Various ( 3 ) Various ( 3 ) Various (8) Various (6) Various (7) Various ( 4 ) Various ( 3 ) Matrix Microelectronic devices Aluminium gallium arsenide Indium phosphide Semiconductors Silicon wafers Silicon wafers Silicon Gallium phosphide Cadmium stannate-zinc sulfide substrates Silicon wafer Silica-silicon substrates Silicon wafers Amorphous silicon solar cell Various ( 1 1) Silicon nitride films on gallium arsenide Various ( 10) Bismuth germanate Various ( 5 ) Indium phosphide Various (4) Silicon wafers Various ( 14) Semiconductors Various ( 3 ) Gallium arsenide GLASSES- Al Silicate glasses B Borop hosphosilicate glass films Technique; atomization; analyte form* SIMS SIMS SIMS MS;GD;S SIMS XRF;-;S RIMS SIMS SIMS SIMS SIMS SIMS SIMS SIMS AE;-;- AA;ETA;L XRF;-;S MS;spark;S SIMS XRF;-;S XRF;-;S B Borophosphosilicate glass Electron microprobe B Borophosphosil icate glass XRF;-;S B Quartz MS;ICP;L Sample treatmentlcomments oxide and nitride layers and detect traces of CI and F from processing Caesium ion bombardment for quantitative detection of Al As and Ga and depth profiling of Zn dopant Quantitative analysis for C H N and 0 using caesium ion bombardment and negative secondary ion collection Detection of C N and 0 using gallium as a sample binder Impurities such as C CI F H N and 0 were encapsulated in the interface made by wafer bonding and detected by depth profiling Implanted Co Cr and Ni detected using instrument with total reflection geometry; accuracy checked by FAS A 30 keV gallium ion beam used to identify thin Detection of Al Be and Co as impurities Use of background subtraction method to improve detection limits for C N and 0 by an order of magnitude detection; depth profiles of Cd H Mn Na 0 S Sn and Zn were measured Quantitation of surface contamination of Al B Ca K Mg and Na as a function of wafer storage time A 5.5 keV molecular oxygen ion bombardment was used to examine behaviour of CI Co Cu K Na Ni and Ti at the material interface quantitatively Al Cr Cu and Fe as contaminants nitrogen used to overcome interference from hydrogen in detection of B C and N Caesium and oxygen primary ion beams used for the measurement of As C Ca Cr Fe H Mg Mn 0 S and Zn impurities preconcentrate Cd Co Cr Cu Ga In Mn Ni V and Zn present as impurities HNO heated and then dissolved in 5 mol dm- HNO,; trace amounts of Al Cd Cu Cr and Ni were detected Total reflection instrument used to detect Fe Ni and Zn following vapour phase decomposition of the surface; measurement of Cu problematic due to losses Detection of trace elements in Cd and Te and related compounds Quantitative determination of C H and 0 Caesium and oxygen ion beams were used in Time-of-flight instrument used to detect Gas spraying method using carbon dioxide or Autoclave decomposition of samples to Samples were treated with a mixture of HCl and Reference 92/97 1 921 1003 9211331 9211341 921 1 546 921 1999 9212028 9212 163 9212 9212 9212 70 77 81 9212331 9212332 9212 35 6 9212447 9212509 9212777 92/28 17 9213 174 Samples were prepared by r.f.sputtering and the 9213954 composition of the films produced were examined using a high resolution dual crystal wavelength dispersive instrument spectrometry with conventional wavelength dispersive measurement Study of lateral uniformity of composition and film thickness; quantitative analysis demonstrated Direct determination using wavelength dispersive instrument suppress volatilization of B during HF acid decomposition Comparison of low energy electron induced X-ray 9 2 x 4 7 9 921 1 749 921 1904 92lC3739 Investigation of use of mannitol and dulcitol toJOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY DECEMBER 1992 VOL.7 377R Table 3 SUMMARY OF ANALYSES OF ADVANCED MATERIALS-continued Element c o Fe Na P Pb Si Various Various Various (9) Various (60) Various Various (4) Various (7) Matrix Zirconium fluoride Zirconium fluoride Float glass Borophosphosilicate glass films Borosilicate and Glass mineral glasses Aluminium fluoride Fluorophosphate glasses Sheet glass fragments NIST SRM 6 10 Glass NIST Mineral Glass K-411 Lithium and aluminium Optical glass precursors fluorides CERAMICS AND REFRACTORIES- Technique; atomization; analyte form* AA;ETA;L AA;ETA;L Electron microprobe or AA;-;L XRF-$3 AA or AE;F or 1CP;L AE;ICP;L AEi-i- AE or MS; laser- ICP or 1CP;S or L XRF or AE; 1CP:S or L Ion microprobe Electron AA;ETA;S microprobe AA;F or ETA;L Sample treatmentlcomments Use of Zeeman-effect background correction and Pd(NO,) and HNO as chemical modifiers to overcome interference from fluoride; recovery 100- 105% achieved Use of Zeeman-effect background correction and Pd(NO,) and HNO as chemical modifiers to overcome interference from fluoride; recovery 97-105% achieved Distribution of sodium oxide in surface layers was investigated using an etching process Use of wavelength dispersive instrument for quantitative analysis using fused phosphorus standards; agreement obtained with independent ICP-AES data Sample was crushed melted and taken into solution and a variety of detection techniques compared Comparison of sodium tetraborate-sodium carbonate fusion method and decomposition with HF in a sealed vessel impurity elements at ppb level direct solid sampling using LA Technique described for the determination of Comparison of wet chemical ICP based methods and Comparison of techniques for identification and quantification of elements present for forensic purposes Investigation of the suitablity of the ion microprobe as a technique for standardless quantitative analysis Use of calculation method in improving quantitative electron microprobe analysis Slurry deposition onto pyrolytic platforms for determination of Cu Fe Ni and Pb at ppm levels Preconcentration of Ag Bi Co Cu Ni Pb and Zn impurities in metal fluorides by extraction of diethyldithiocarbamate complexes into iso- propanol; flame detection only used for Ag and Zn Al Aluminium oxide dusts AA;-;L Al Silicon carbide B Silicon dioxide AE;ICP;L AE;DCP;L C Superconductor SIMS Ca Silicon carbide AE;ICP;L c o Lanthanum and yttrium AA;ETA;S oxides Fe Silicon nitride AE; 1CP;S H Ni 0 Fusion with potassium pyrosulfate preferred to direct acid decomposition method - Decomposition of sample with HF-HNO in the presence of mannitol in a closed vessel and subsequent evaporation of silicon dioxide Minor isotope in situ ion implantation used to provide quantification in a sputtered thin film sample Cation exchange on AG 50W-X4 column to remove Na; then elution with 200 ml of 0.2 mol dm-3 HNO Coprecipitation with APDC from HNO solution; recoveries in range 100-103% and RSDs 1.9-3.0% for direct analysis of precipitate Sample (0.05-0.5 g) dispersed in 100 ml of 0.5Oh sodium hexa(metaph0sphate) solution as dispersant; this was agitated ultrasonically and the slurry aspirated into the ICP Measurement by detection of protonated metal ion; SIMS was used for near-surface detection and laser MS for bulk determination Coprecipitation with APDC from HNO solution; recoveries in range 95- I001 and RSDs 3.9-4.1 O/o for direct analysis of precipitate Superconductor SIMS or laser MS Lanthanum and yttrium AA; ETA;S oxides Superconductor SIMS As for C Reference 92/12 921 12 9211915 921300 I 921 1 84 92lC3625 9 113904 92IC590 921946 9211 253 921 1 748 9212206 9213065 921 I 763 9213044 92156 9212362 9213044 921272 1 92lC3 5 36 9212927 921212 1 9212362378R JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY DECEMBER 1992 VOL.7 Table 3 SUMMARY OF ANALYSES OF ADVANCED MATERIALS-continued Technique; atomization analyte form* AE:ICP or F L Element S Zr REE REE REE REE (14) REE (14) REE (14) REE REE ( 1 5) Various ( 10) Various (23) Various (2 1 ) Various (7) Various (20) Various (8) Various (5) Various (3) Various (4) Various ( 1 2) Matrix Superconductors Sample treatmenticomments Indirect determination by flame using precipitation as barium sulfate; matrix interference was removed by pre-separation using a strong acid cation- exchange column; ICP detection of S at 182.043 nm compatible with determination of N by titration quantitative analysis; LODs reported in the range 0.02-0.2 ppm in the solid 1 ppm reported layer pelleting technique and critical thickness studies; LODs in the range 20-100 ppm Orthogonal experimental design used to optimize conditions for detection of Ce Dy Er Eu Gd Ho La Lu Nd Pr Tb Tm Y and Yb Use of correction factors to compensate for interferences without the use of matrix matching of standards Optimization of parameters using orthogonal experimental design; LODs 5- 100 ppm Impurities were separated in 10 mim by HLPC using a silica-octadecyl column and gradient elution with 2-hydroxyisobutyric acid Fusion with 1 + 1 lithium borate-lithium tetraborate with iodine pentoxide added as a fusion agent; RSDs in the range 0.75-3.59% reported Lanthanum hydroxide was used to coprecipitate Co Cr Cu Fe Mn NI Ti V Zn and Zr to separate from the matrix graphite and 5% sodium fluoride and evaporated from crater of graphite anode columns; simultaneous recovery of elements after separation from matrix at pH 4 with 9 mol dm-3 HNO as eluant gave recoveries in the range 96- 102Oh by choice of background correction line selection and matrix matching methods; agreement reported with XRF method Reduction in blank levels by use of sealed double PTFE vessel for acid purification for the detection of Al Ca Cu Fe Mg Mn Na and Ti metaphosphate containing I OW lithium carbonate) for detection of Bi Ca Cu Pb and Sr Solution of tungsten oxide mixed with 1-(2- pyridylazo)-2-naphthol to precipitate Co Cu and Ni and were separated using ammonium chloride- ammonia solution pH 10 buffer Detection of Cr Mn Nb Ni and V qualitatively using XRF and quantitatively by ICP Powdered samples were mixed 1 + 1 with graphite powder and analysed for Al Co Cr Fe Mg Mn Mo Ni Pb Si Sn and V as impurities; LODs reported at ppm levels Sample shaken with solvent mixture of 5+ 1 gallium oxide-potassium chloride; for niobium oxide graphite powder also added detection of Ag Al Ca Fe Mg Mn Nb Si Sn and Ti at 3-300 ppm Ashing followed by fusion with borate-carbonate mixture and extracted with 1 + 1 HCI; LOD reported in range 1-93 ppb in the solid Comparsion of several acid digestion procedures Use of chemically prepared standards to achieve Sample is spiked before separation by HPLC; LOD of Use of small sample (400 mg) by means of double- Powdered samples mixed with 10% powdered Use of iminodiacetate chelating resins on mini- Acid dissolution for Al B Fe Mn Mo Si and Ti Determination of 15 REE and Al Ca Fe Pb and Si Fusion of sample with 19-fold excess of flux (lithium Reference 92/28 13 92lC3548 92/32 921C467 921 1 860 9211933 92127 16 9212739 9213045 9213943 9 113795 9 1/38 17 9113858 9113995 9 113938 92154 921151 921 165 92lC5 9 7 921 I299 9211357 921 192 1 Zirconium nitride Yttrium oxide A E; I CP; L SIMS High-purity yttrium oxide Rare earth oxides ( 1 5) Isotope dilution MS XRF;-:S Samarium oxide AE;-;S Yttrium oxide AE;ICP;L Dysprosium oxide Terbium oxide AE;d.c. arc;S AE;ICP;L Rare earth oxide mixtures XRF;-:S Molybdenum oxide A E; ICP; L Mangesium oxide ceramic AE;d.c.arc$ Silicon nitride and silicon carbide AE;ICP;L Ceramic electrodes Rare earth oxide mixtures AE;ICP;L AE;ICP;L High-purity silica AA or AE;F or 1CP;L XRF;-;S Superconductors Tungsten oxide AA F L Titanium dioxide Superconductors XRF or AE;ICP; AE;a.c.arc;S S or L Various ( 1 0) Tantalum and niobium AE;d.c. arc$ oxides Various (16) Graphite AE;ICP;LJOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY DECEMBER 1992 VOL. 7 379R Table 3 SUMMARY OF ANALYSES OF ADVANCED MATERIALS-continued Technique; atomization; analyte form* XRF;-;L Reference 921 I925 9212059 9212084 9212202 9212204 921222 I 9212222 9212507 9212624 9212976 9212989 92lC3386 92x355 1 92lC3 5 5 8 Element Various (4) Various (1 6) Various (3) Various (7) Various (4) Various ( 1 1) Various (8) Various Various (8) Various (4) Various (4) Various ( 1 7) Various ( 1 0) Various (6) Matrix Superconductors Sample treatmentlcomments Microdroplet analysis combined with fundamental parameter method for standardless determination of Ba Ca Cu and TI as oxides Sample heated in platinum crucible with HF and H,SO and evaporated; residue heated with HF and H,PO until fluid became transparent Radionuclide source used to achieve detection of Ba Cu and Y with precision 3% or better; accuracy confirmed by ICP-AES Samples fused 1 + 19 with lithium metaphosphate at 850 "C for 50 min in a CO-C02 atmosphere; detection of Ba Bi Ca Cu Sr T1 and Y using a LiF(200) crystal Samples dissolved in dilute HCI or HNO and Ba Cu La and Y determined using Mn as internal standard Sodium chloride was used as carrier and indium as the internal standard; LODs in the range 1-5 ppm for B Bi Co Cr Mn Ni Pb Sb Sn V and Zn LODs for Ca Dy Er Ho La Tb Tm and Yb in the range 0.48-5.9 ppm; spike recoveries of 90-1 10%; RSDs <4% Comparison of sample preparation and direct insertion techniques Direct determination of Co Cr Cu Fe Mn Ni Pb and Zn reported; LODs in the range 0.07-0.3 ppm by FAAS Slurry nebulization of powdered sample for detection of Al Ca Fe and Mg; reported atomization efficiencies of 77- 1 OOYo for these elements Sample was dissolved in HNO and interference free lines were selected for the determination of Ce Nd Pr and Sm at ng ml-I levels digestion decomposition with ammonium sulfate and fusion with lithium tetraborate Sample dissolved in HF and HNO,; dissolved Si and remaining HF were removed by fuming with Use of dervative spectrometry to overcome spectral interferences in the determination of Al Ce Cu La Sm and Pb Comparison of three methods involving acid H2SO4 High-purity alumina A E ; I CP; L Superconductor films XRF;-;S Superconductors XRF;-;S Superconductors AE;ICP;L Terbium oxide AE;d.c.arc$ Yttrium oxide AR;ICP;L High-purity alumina Europium oxide AE;ICP;S or L AA;F and ETA;L Silicon nitride A E; I C P ; S Lanthanum oxide AE;ICP;L Lead zirconate-titanate ceramics AE;ICP;L Molybdenum disilicide AE;ICP;L Yttrium oxide AE;ICP;L CATALYSTS- Ir Pd Pt Pt Pt Pt Rh Rh Various ( 6 ) Catalysts and alumina Extraction with potassium xanthate by heating in a Dissolution of 0.2 g of sample in up to 10 ml of water bath for 25 min various acids or alternatively bomb digestion with HCl and H,O Sample mixued with conductive host matrix material; internal standardization employed to compensate for sputtering rate differences between samples Comparison with UV-visible spectrometry AES and AAS methods High-pressure decomposition (Knapp 1984); interferences due to Al Ca Fe P Pb S Si and Sn studied dithiocarbamate in the pH range 5.2-6.2; no inteference was found from 12 other elements Solvent extraction with potassium u-butyl As for Pt 921 1429 9214057 AE;ICP;L AA;FL Aluminium-based catalyst 9219 Alumina-based automotive catalysts AA;G D;S Catalysts 9212074 9212 12 1 XRF;-;S AA;ETA;L AE;ICP;L Catalysts Catalysts 9213047 Alumina-based automotive Catalysts catalysts AA;GD;S AE;ICP;L 9219 921286 Extraction with potassium hexyl xanthate by heating in a water bath for 15 min; RSD of t2% reported for 10 runs Fusion with lithium metaborate-tetraborate flux; good agreement obtained in round robin tests Zeolite-based fluid cracking catalysts XRF;-;S 9 l/C3657380R JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY DECEMBER 1992 VOL.7 Table 3 SUMMARY OF ANALYSES OF ADVANCED MATERIALS-continued Element Various (5) Various (3) Various (3) Various (3) Various (8) Technique; atomization; Matrix analyte form* Automotive catalysts XRF or MS;ICP;L Alumina-based catalysts XRF;-:S Zeolites XRF-;S Reforming catalyst XRF-;S Alumina-silica base catalysts AA;F;L Sample treatmentlcomments Reference 9214 1 5 Comparison of microwave digestion procedures and ICP-MS detection with wavelength dispersive XRF method for Ba Cd Fe Ni and Pd Comparison of XRF method with established procedures based on UV-visible spectrometry ETAAS and ICP-AES for CI Pt and Re Fusion of 1 g of calcined sample with 1.6 g of lithium borate 4.8 g of lithium tetraborate and 0.1 g of potassium iodide; detection of Al Na and Si Wavelength dispersive instrument used to achieve reproducibility of 1 O/o or better for determination of Ir Pt and Re of HNO nitric and fluoroboric acids 921425 9212418 9213077 Microwave oven slurry preparation using a mixture 92lC3655 * Hy indicates hydride generation and S L G and SI signify solid liquid gaseous and slurry sample introduction respectively.Other abbreviations are listed elsewhere. was reported that surface derivatized polymers metal doped conductive polymer films and patterned polymeric materials or fibres were mapped in two or three dimensions.The adhesion of metals such as Cr Ti and Zr to sputter- cleaned polyimide has also been investigated using SIMS (92/ 14 14). The application of LA to the analysis of polymeric materials was reported in two papers at the 1992 Plasma Winter Conference. Lord and Nelson (92/C3454) decribed the determination of trace elements in polymers by ICP-MS using single spot multiple spot and raster LA. It was reported that elements could be detected quantitatively in the range 10 ppb to per centage levels using a combination of pulse and analogue counting detector modes and that under optimum conditions RSDs of 5% could be achieved. The application of laser-induced AES for industrial on-line analysis has been described (92/C335 1).A high-power laser was used to ablate and excite the constituents of rubber slabs made during the early stages of tyre production. The emitted light was collected using an optical fibre connected to a spectrometer equipped with a multichannel analyser with high time resolution. The focused laser beam could be scanned across the the plane surface of the slabs to monitor spatial element distributions of compound constituents. A new technique known as sliding spark excitation has been described which allows the direct examination of non- conducting polymers by AES (92/C3646). The system allowed the generation of AE on the surface of the solid material although the abstract gives no details of how this was achieved. The excitation source was coupled via optical fibres to a spectrometer. Examples of applications cited included silicon-containing polymers antimony-containing rubbers or plastics incorporating different concentrations of titanium dioxide.3.2. Semiconductor Materials Over 150 abstracts were received in the year under review concerned with surface analysis techniques (primarily SIMS) for the characterization of semiconductor materials. Most of these abstracts are associated with SIMS 7 and the proceedings of this international conference on SIMS has now been published (e.g. see 92/2862). However only a small proportion of these papers was concerned with quantitative analysis. Where sufficient detail has been given in the abstract an entry has been made in the relevant section of Table 3. A few of the more pertinent papers are highlighted in the following section.One of the main difficulties encountered in the examina- tion of solids with a heterogeneous structure involves the calibration of instrument response. This is problematic because of the lack of availability of suitable reference standards. Since many of the materials under investigation have novel structures it is unlikely that external calibra- tion methods for surface analysis techniques such as SIMS will provide a complete solution to this problem. The use of relative sensitivity factors (RSFs) in SIMS for analytes in a particular matrix has been the subject of much investiga- tion. In one paper the RSFs for up to 74 elements implanted into 23 materials were studied over an 8 year period (9211020).It was found that the reproducibility of the RSFs was around 60% using several Cameca magnetic sector instruments with particular reference to silicon gallium arsenide and cadmium mercury telluride matrices. Plots of log RSF versus ionization potential of the sput- tered impurity elements were observed to have linear trends. The trends were similar for a variety of materials including semiconductors metals and insulators. The same workers observed similar trends in a more detailed study of silicon and silica (92/ 10 19). Relative sensitivity factors for 43 elements in silicon were measured using a Cameca IMS-3F system (9212298). Both caesium and oxygen ion bombardment were employed and secondary ions of the opposite polarity were detected. The influence of factors such as sample holder design (e.g.flatness or mask window type crater position) and spectrometer parameters (e.g. energy bandpass peak shape) on the reproducibility of RSFs in SIMS has been studied (92/2862). It was found that there is a relatively large spread in RSF values for repeat measurements of a single reference sample which would give rise to a commensurate uncertainty in the estimation of concentration. A number of SIMS round robin exercises have been conducted to aid in the process of making RSF values transferable between instruments and establish the accu- racy of quantitative methods (92/3223). The analysis of NIST prepared calibration standards for silicon and silica was carried out by five magnetic sector SIMS instruments and two quadrupole systems in seven laboratories (92/2861).The samples were implanted with Al C Cr Cu Fe and Na. Data on implanted high dose Cr Cu and Fe were also reported using Rutherford backscattering andJOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY DECEMBER 1992 VOL. 7 381R NAA. A Japanese round robin on the analysis of gallium arsenide was conducted in collaboration with 16 SIMS participants and 1 8 chemical analysis laboratories (92/22 18). The purpose of the trial was to obtain validated gallium arsenide standard materials for SIMS analysis and as a by-product acquire secondary-ion yield data. The statistics produced by the study were discussed in detail. Gallium arsenide was also the subject of two other SIMS round-robin trials (92/2338). Interlaboratory differences in the quantitative data were reduced to around 10% by the use of common calibration standards.The alternative approach recommended for quantitative analysis was that instrument dependent databases could be used to achieve an accuracy of approximately 50%. Several reviews have been published on the application of SIMS to the anal-vsis of semiconductor materials. These include the application of SIMS to the mapping of dopant distribution in silicon (92/1067 92/2803) and to quantita- tive depth profiling (92/ 1056. 92/2339). Sputtered neutral MS is increasingly finding a role in the characterization of bulk silicides and thin films (921963 9211069). This technique relies as the name implies on the detection of neutral species sputtered from the sample but the sampling process can be used in conjunction with RIMS.Systems of this type have been decribed for the determination of Fe and 0 s in silicon (92/1567) Mg in silicon (92/2315) and depth profiling of silica-indium phosphide materials (92/ 1325). Finally reviews comparing surface analysis and other techniques for the characterization of semiconductors may also be of interest (9211051 92/1058 92/1066 921 1068). Owing to the sensitivity requirements for the analysis of semiconductors techniques based on mass spectrometry tend to dominate the literature. Solids can be directly sampled using laser ablation and this procedure has been adopted in an investigation of dopant lateral diffusion in cobalt and tantalum silicides (92/1574). It was claimed that the LAMMA system used could achieve 1-3 pm resolution which was adequate for studying device lines in these materials.The LAMMA technique was used for the analysis of inorganic solutions by deposition on the porous layers of the surface of a silicon wafer anodically oxidized in HF (92/2821). It was indicated that this procedure resulted in preconcentration of impurities which were completely absorbed. The use of an ETV device for sample volatiliza- tion prior to laser ionization MS was described (92/388 1). Using this approach the sample was evaporated by means of a graphite ETA operated at 1700 "C in vacuo. The system was applied to the determination of A1 in germanium and silicon. Detection limits for A1 were reported to be 0.1 and 2 ng g-' respectively in these matrices. Spark source MS has found application in the the analysis of cadmium mercury telluride (92/2 19 1 92/28 17) and in the detection of P and B in silicon and semiquantitative analysis of gallium arsenide (92/C47 1).Glow discharge MS would appear to offer many of the advantages of spark source MS (92/ 134 I) including providing the depth profiling capability of the surface analysis techniques referred to above and two articles providing an overview of the technique have been pub- lished (921988 9211267). The main development in this field reported this year involved the construction of a new discharge cell that can accommodate flat samples (92/C399 92K3610). The geometry of the cell allowed the direct analysis of silicon wafers. It was reported that C and 0 could be detected at sub-ppm levels using a magnetic sector mass spectrometer.The relative merits of GDMS SIMS NAA and ICP-MS have been assessed for the analysis of refractory metals and their silicides used in low resistivity gates interconnections and ohmic contacts in minimum integrated circuit geomet- ries (92K3404). It was concluded that ICP-MS was the most suited to this application exceeding the sensitivity of the other techniques for the bulk characterization qf refractory metals. Certainly it would appear that ICP-MS is increasingly being employed in this field. Extremely high sensitivity can be achieved by the use of ETV sample introduction for ICP-MS. A system of this type has been applied to the determination of impurities in photoresist for very large scale integrated circuits (92K3538). It was found that a very small amount of sample could be used which resulted in less contamination of the spectrometer.The photoresist was diluted 10-fold with ethoxy ethyl acetate and an aliquot injected into the graphite tube. A decrease in spectral interferences from C and 0 polyatom- ics was observed in comparison with conventional nebuli- zation. Detection limits for Fe and Na in photoresist were 0.2 and 0.06 ppb respectively. The ETV-ICP-MS technique has also been used for the determination of Th and U in electronic materials (9 1/C368 1). Alpha particle emissions from these elements present at ppb levels can result in errors in the devices. Samples were prepared chemically in small volumes and a 10 pl aliquot was deposited to dry on a tungsten coil rod.The analytes were vaporized into the ICP-MS system and it was found to be possible to determine down to 0.01 ppb using this approach. The detection of Fe down to about 0.02 ppb has also been achieved using ETV-ICP-MS (92K3595). However per- haps the most effective method for improving sensitivity and/or reducing spectral interferences is to use a high- resolution MS detection system (92K3622). The determi- nation of P and S in aqueous and organic solutions has been demonstrated using such an instrument. Perhaps as a consequence of the success of ICP-MS in this field there were relatively few novel developments in the application of ICP-AES to the analysis of electronic materials. Those methods which have appeared are sum- marized in Table 3.However AAS would still appear to have something new to offer in this field. A new method of solid sampling has been described based on argon sputter- ing the sample and forming a layer on a graphite platform which is then placed in the graphite furnace of an atomic absorption spectrometer (92K778). It was found that for different materials the sputtered layer gave different responses on atomization. However if 20 pl of HN03 were deposited on top of the platform the sample appeared to be taken into solution and this removed the matrix effects thus allowing the use of aqueous calibration. Measurements indicated that when cadmium telluride ( 1 1 ) single crystals were used as the sputter target a film was formed with a stoichiometry of Te:Cd of 1.09:l on the platform.The method was applied to the determination of the impurities such as In present at a concentration of 600 ppm in cadmium telluride. A study has been made of the volatiliza- tion of Ca in a gallium matrix using ETAAS molecular absorption spectrometry and ETA-FAAS (92K769). It was found that gallium was evaporated at 900-1 100 "C when applied at the 10 ng level corresponding to the evolution of gallium oxide elucidated by MS studies. However when gallium was present as the matrix element at 10 pg the major fraction was found to vaporize as metal between 1120-2300 "C. Since Ca at the 1 ng level vaporizes above 1520 "C the use of a pre-volatilization temperature step to remove the matrix was found to allow the interference free determination of Ca up to a gallium concentration of 0.3% m/v in a nitric acid medium. A detection limit of 0.057 ppm was reported for the determination of Ca in gallium.Conventional X-ray jluorescence spectrometry does not offer the sensitivity required for the detection of trace dopants in semiconductor materials. However the tech- nique can be applied to the characterization of major components in films and to thickness measurement and progress in this area has been the subject of a review382R JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY DECEMBER 1992 VOL. 7 (92/222). The development of total reflection XRF has revitalized the use of the technique and a number of methods for the analysis of silicon wafers have now been published. These include the detection of Cu Fe Ni and Zn as impurities (92/2777 92/3274) and the measurement of ion-implanted Cr Co and Ni.In both cases the sample was dissolved using HF and silicon was volatilized as the fluoride prior to determination of analyte concentrations in solution by TXRF. Further improvements in sensitivity were claimed for a more advanced TXRF system which utilized monochromatic source radiation (92/3274 92/3905). The conventional X-ray tube was removed from the instrument and replaced with a rotating anode and a monochromator was added to improve the S/B ratio. An improvement factor of 1-2 orders of magnitude in terms of detection limit was reported. The application of the system to the determination of impurities on silicon wafers was described. The analysis of gallium arsenide by TXRF using two different commercial instruments has also been de- scribed (9211 895). 3.3.Glasses Ceramics and Refractories 3.3.1. Glasses There were fewer abstracts received in the year under review pertaining to the analysis ~f gfasses and related materials. A summary of analytical methods is provided in the relevant section of Table 3. Some methods for the analysis of glasses by ICP-AES involve dissolution with acid mixtures including HF. It is known that analytes can be lost as volatile fluorides using such procedures and the range of applications is therefore limited. However there is some evidence to suggest that if the decomposition is carried out in a sealed vessel Si may be retained (92/C3625). A microwave digestion procedure of this type was evaluated for the determination of Si in NIST SRMs by ICP-AES.It was reported that the method was found to be faster and as accurate as procedures based on fusion with sodium tetraborate-sodium carbonate. The determination of B in high-purity quartz may also be subject to error if an HF dissolution is employed (92K3739). It was found that the addition of mannitol or dulcitol in 1000-fold molar excess provided a means of achieving 100% recovery for B in an HF dissolution. However these organic compounds were found to reduce the ICP-MS signals for B as a result of carbon deposition on the sampling cone. This effect was overcome by the use of beryllium as an internal standard. The application of LA-ICP-AES and ICP-MS to the direct analysis of fluorophosphate glasses has been dis- cussed but no details were given in the abstract (921C590).An r.J planar magnetron GD source has been employed for the direct determination of elements in glass samples by AES (92K3647). The dependence of the analytical atomic and ionic line emission intensities on argon pressure (0.5-20 Pa) and r.f. power (50-200 W) was studied. A comparison has been made between the use of ICP- AES XRF and refractive index for the forensic characteri- zation of sheet glassfragments (92/946). The concentrations of nine elements were determined by ICP-AES and preci- sions in the range 1-10% were obtained. The X-ray intensities of five elements were determined by EDXRF and precisions in the range 1-25% were reported. It was concluded that the ICP-AES method while slower and destructive provided quantitative data which allowed improved discrimination with respect to the source of the material.However XRF methods are attractive in this type of application because they are non-destructive. Matrix interferences can be compensated for by use of correction factors based on mass absorption coefficients (91/3797). Limitations in terms of range of analyte coverage are being overcome as a result of recent developments in instrumen- tation which permit the detection of light elements such as B (92/1904). A method has been described for the determi- nation of P in borophosphosilicate and phosphosilicate glasses using WDXRF (9213001). The glasses were coated on a silicon wafer. Secondary spectral line intensities from the wafer were monitored and compared with those from an uncoated wafer and a fused P standard.The results were converted into P content and film thickness by relating the spectral line intensities for P and silicon. Good correlation was achieved with independent ICP-AES analysis of the glass films for P. In another study low energy electron loss induced X-ray spectrometry (LEEIXS) was applied to the quantitative determination of B in borophosphosilicate glass films (92K479). The instrumentation used was a WDXRF system equipped with a high-performance gas discharge tube as an electron source. Layered synthetic microstructures were used for dispersion which improved sensitivity for light elements. Unfortunately the abstract does not provide any information about the detection limit of the method. The application of ion microprobe analysis to the detec- tion of over 60 elements in NBS (now NIST) Glass SRM 610 has been described (92/1253).The variation of ion yield with atomic number was found to give a relatively smooth pattern which might allow a move towards stan- dardless analysis using the technique. However it was noted that Si which was a candidate element for normaliza- tion was most susceptible to variations in analytical conditions. The electron microprobe was applied to the measurement of elemental constituents in NIST SRM K411 Mineral Glass again for the purposes of calibration of response (92/1748). However it was noted that the study emphasized methodology and concept rather than the pursuit of numerical precision! The electron microprobe was also utilized in the non-destructive characterization of borophosphosilicate glass coatings (92/ 1 749).An accuracy of about 3.6% was achieved for the determination of B in glass films. It was considered that the electron microprobe method could be employed as a reference method to support production control methods based on XRF. 3.3.2. Ceramics refractories and catalysts The analysis of REE oxides continues be a focus for research effort. Secondary-ion MS has been used to deter- mine the concentration of REE in yttrium oxide (92/32). A Cameca IMS-3F system with a duoplasmatron primary-ion source was employed. Charring effects at the sample surface were eliminated by mixing the sample with graphite powder. Spectral interferences from polyatomic ions were suppressed using an energy filtering technique.The levels of REE were quantified using a calibration graph derived from chemically prepared synthetic standards. It was reported that detection limits were obtained in the range 0.02-0.2 ppm using this technique. Spectral inte!fevences are also a significant problem when ICP-AES is used to determine trace elements in yttrium oxide (92K3558). Intense yttrium lines were found to be adjacent to the lines for Ce I1 at 4 18.660 nm La I1 at 379.083 nm and Sm I1 at 359.262 nm. The determination of these elements was further compli- cated by sloped or curved background interferences. Spec- tral line overlaps were also observed in the analysis of Al Cu and Pb in this matrix. A numerical derivative technique was applied to correct for such spectral interferences.It was reported that all background-related interferences were eliminated using this approach and that the analytical lines for Al Cu and Pb were resolved from the interfering lines. As a result of the enhanced spectral resolution achieved using the derivative procedure detection limits were improved by 7- 1 10-fold. A high-resolution sequential spectrometer has been applied to the determination of traceJOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY DECEMBER 1992 VOL. 7 383R elements in REE mixtures (92lC3808). The system incor- porated an automatic exit and entrance slit mechanism that permitted the optimization of resolution sample through- put and detection for seqential measurement which related to the spectral complexity around the analyte line.It is possible to eliminate spectral interferences by using a separation procedure prior to analysis. The determination of REE in terbium and terbium oxide has been carried out using an interfaced HPLC-ICP-AES system (9213045). The rare earth impurities were separated from the sample matrix by gradient elution from a silica-octadecyl column with 2-hydroxyisobutyric acid. The mutual separation of impurities could be carried out satisfactorily within 10 min. The rapid elution resulted in sharp peaks and sensitive detection. Up to 30 pl of a 1% m/v solution of terbium could be injected onto the column. The use of a power setting of 800 W was found to give a 5-fold improvement in SIB compared with operation at the usual setting of 1300 W. Recoveries of REE from the terbium oxide matrix were in the range 85- 100% and it was found unnecessary to use matrix matched calibration standards. The characterization of catalysts remains a major chal- lenge in the field of trace inorganic analysis.Fluid cracking catalysts are intensively used in the petroleum industry. These catalysts are supported on zeolites (crystalline or amorphous silica-alumina structures) which can be impreg- nated with REE to alter their functionality. The determina- tion of the si1ica:alumina ratio is an important parameter in the characterization of zeolites and several methods have been published in the last year based on SIMS (92/1605) PIXE XRF and NAA (91/4013) and fusion followed by XRF (92/2478). The detection of poisons such as Ni and V which derive from the processing of petroleum oils is extremely important and highly sensitive methods are required.Fusion-based XRF procedures (9 1/C3657 92/C595) have a role to play in such applications but rapid dissolution methods based on microwave slurry sample preparation for FAAS or ICP-AES may provide a viable alternative (92K3655). However since catalysts tend to be contaminated on the surface of the support SIMS can be used advantageously and two overview articles on the application of the technique to the characterization of petroleum cracking catal-vsts may be of interest (92/ 1490). Precious meta/ catalysts supported on alumina are widely used in the petrochemical industry as the means of altering hydrocarbon structures. Such ‘reforming’ catalysts tend to be based on the use of platinum although other elements such as iridium (92/1429) and palladium (92/4057) can be used in specific applications. In the year under review a number of methods have been published for the determina- tion of Pt in catalysts based on XRF (92/2074 92/3077) ICP-AES (92/286,92/3047) and ETAAS (92/2 12 1).Perhaps the most interesting application described involved the determination of C1 Pt and Re on alumina-based bimetallic reforming catalysts by XRF (921425). Chlorine is not an element which is easily determined by most atomic spectro- metry methods and a UV/VIS spectrometry procedure was adopted as a comparative method to assess accuracy. The XRF method developed was also compared with reference methods involving ICP-AES ETAAS and ED-SEM.Statis- tical evaluation of the data indicated that the proposed XRF method gave no significant bias. Automotive catalysts also make use of the properties of platinum group metals on alumina substrates. Two rapid microwave digestion procedures were described in which dissolution of such catalysts could be achieved in 2-3 h (921415). In the first the dried sample was digested in a mixture of HCI and HF acids in a microwave perfluro- alkoxy (PFA)-PTFE sealed vessel followed by treatment with HClO and aqua regia in an evaporating dish on a hot- plate. In the second method a mixture of HF HN03 and HCl was used in an initial microwave digestion step. The sample was cooled and neutralized with H3B03 the vessel was recapped and heated further in the microwave oven. In both cases the final solutions were diluted and analysed by ICP-MS.It was noted that the ICP-MS method compared favourably with existing ashing methods in terms of speed and WDXRF. In a relatively novel approach the determi- nation of Pt and Rh in automotive catalysts was carried out by GDAAS (92/9). The alumina-based catalyst was mixed with a conducting host matrix material and analysed directly thus avoiding time-consuming sample preparation steps. It was found that differences in sputtering efficiencies between samples could be compensated for by use of an internal standard. It was reported that the technique provided accurate results with relative errors of 2-3%. Relatively few papers have been published in compari- son with previous years on the analysis of alumina or other oxide-based ceramic materials.Work has continued on solid sampling methods for the ICP including the introduc- tion of ceramic powder in the form of a slurry (92/2494) by ETV (92/280) and by direct sample insertion (92/280 9212507). Chemical methods for sample preparation have also been described (92/ 1763 92/2059). The analysis of perovskite ceramics has received some attention in the year under review. Acid dissolution and fusion-based sample preparation procedures have been developed for the analy- sis of lead zirconate-titanate (92/C3385 92/C3386) and manganite and cobaltite perovskite electroceramics (92/2285) by ICP-AES. The application of GDAES to these materials was also discussed (92lC648). Samples were pressed and analysed following 1 0-fold dilution in a copper conducting host matrix.Analytical performance was as- sessed by comparison with an ICP-AES method. Lan- thanum and strontium manganite and cobaltite perovskite ceramics have also been characterized in the solid phase by LA-ICP-AES and ICP-MS (921C3374). A Q-switched ruby laser with an output energy of 0.1 J was employed for ICP- AES studies. Lanthanum was used as the internal standard. In the case of ICP-MS the samples were prepared as pressed pellets and ablated using a Nd:YAG laser with an output energy of 0.1-0.3 J. Strontium was used as an internal standard and calibration was achieved using external solid standards. Results obtained with the two methods were compared with ICP-AES analyses using a dissolution procedure.Papers continue to be published concerning the charac- terization of high-temperature superconductors. The great majority of these were concerned with the analysis of Y-Ba-Cu-0 type ceramics. Most of the wet chemical sample preparation methods reported for ICP-AES and AAS determinations were similar to those already in the literature. However in a novel approach AAS has been used as an in situ diagnostic tool to study the sputtering of high-temperature superconductors (92/3206). Hollow cath- ode lamps were employed as oxide targets using a Kaufman ion gun. The ground state Ba and Cu atoms ejected from the composite target during argon and oxygen-ion bombard- ment were studied as a function of sputtering parameters. The composition of high-temperature superconducting films and single crystals has been examined by ETAAS (92/2201).The central portion of the graphite furnace was lined with tantalum foil which was found to improve the sensitivity stability and reproducibility of the analytical method. It was reported that small amounts of sample (0.00 1-0.000 1 g) could be analysed using this procedure. X-ray .fluorescence remains a popular technique for the analysis of high-temperature superconductors using various types of instrumentation. X-ray excitation using a radionu- clide source (92/2084) a tungsten target tube (92/2202) and a synchrotron (92/3008) have a\\ been evaluated in this type of determination. In the last case a total reflection geometry384R JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY DECEMBER 1992 VOL.7 was adopted to minimize background radiation from the film substrate. A fundamental parameter XRF method was applied to the characterization of a TI-Ba-Ca-Cu-0 superconductor to avoid the need for standards containing TI which is poisonous (9211 925). It might be expected that LA-MS techniques may offer some utility in the characterization of superconductors. However the study of laser-sample interactions appears to be dominating this field at present (92/1246 92/1417 92/153 1 92/3258). This is because LA may provide a route to the preparation of high-quality superconducting thin films (92/1576 92/2 148,92/3 153). The application of SIMS to the analysis of these materials has received further attention. Quantitative methods for the determination of C and 0 (9212362) and H (92/2927) in Y-Ba-Cu-0 type superconductors have been published.Relative sensitivity factors for SIMS (92/ 1053) and Auger electron spectroscopy (92/1055) have also been determined in this matrix. Image depth profiling studies using SIMS have also been carried out (92/974 92/2 187). Finally a number of papers have been published or pre- sented on the analysis of non-oxide ceramics. As with other developing fields of materials science the application of SIMS is well represented. The coating of Nicalon fibres with silicon carbide has been studied by SIMS (92/ 152 1). It was found that there was no change in the fibre structure as a result of the coating process indicating that the fibre should retain its properties. A SIMS depth profiling technique has been used to examine fibre-matrix interfaces in silicon carbide fibre reinforced composites (92/15 1 1).The use of a conductive metal coating and electron bombardment during sputtering compensated for sample charging allowing the analysis of insulating ceramic materials. Lateral resolution of ion images was reported to be about 1 pm but depth resolution was claimed to be as low as 5-10 nm. The use of electron bombardment and self-compensation for reduction of surface charging of samples has also been applied to the characterization of silicon nitride (92/968) and oxide nitride and organic thin films (92/2873). A Cameca IMS-3F SIMS instrument utilizing a 200 nA 14.5 kV oxygen primary beam has been used to monitor B diffusion in silicon carbide films formed by chemical vapour deposition (92/2 189).The detection of positive ions allowed quantitative digital imaging for B. A SIMS method for the detection of N Ti and Si in the interface between silicon nitride and titanium metal was described (92/1161). The specific ions of titanium silicide and titanium nitride were selected for measurement. It was found that the method produced data which were in good agreement with XPS and Auger studies of the metal- ceramic interface. The application of SIMS to the quantita- tive analysis of titanium boride and titanium carbide wear protection coatings has also been reported (92/2868). It was commented that the signals from the metalloid species could be used to measure the extent of wear and to help explain wear resistance (e.g. as a result of oxidation).Ceramic materials are increasingly produced in fine powders and this provides opportunities for direct analysis by ICP-AES using the slurry procedure (921276). This approach has been adopted for the determination of Al Ca Fe and Mg in silicon nitride powder (92/2976) and for the determination of Fe in silicon nitride (92/C3536). In the latter case the sample (0.05-0.5 g) was diluted to 100 ml by the addition of 0.5% m/v aqueous sodium hexametaphos- phate (Graham's salt) as dispersant and slurried by ultra- sonic agitation. The sample was introduced directly into the ICP and the suspension was maintained by magnetic stirring. When samples have to be ground or pulverized prior to slurry preparation or to help speed up sample dissolution there is always the possibility of contamination by the equipment used.This has been the subject of study in the development of a method for the determination of impurities in sintered silicon carbide (92K3535). It was found that the use of a vibrating mill with pots made of iron tungsten carbide and zirconia caused contamination of the sample. In the case of zirconia this was found to be as much as 5% with 30 min of pulverization. Attempts were made to remove iron contamination by extraction with hydrochloric acid but this was found to extract other impurities from the sample. It was found that the best method to minimize the problem involved the dissolution of a small amount of sample (0.15 g) in an HF-HN03-H2S04 mixture in a PTFE vessel by heating for 24-48 h at 230 "C. The direct analysis of high-purity ceramics by LA-ICP-MS has been reported in conference presentations in recent years (see J.Anal. At. Spectrom. 1991 6 318R and references therein). Some of this important work is now being published in the primary literature. The technique has been applied to the analysis of silicon nitride powders (92/ 125 1 ) and to the trace analysis of cerium oxide silicon nitride and silicon carbide (92/1361). Two other papers also indicated application of LA-ICP-MS to the analysis of ceramics but no details were available in the abstracts (92/15 10 92/1579). The advantages of LA-ICP-MS cited included high sensitivity (sub-ppm) rapid analysis low background and minimal spectral interference and little or no sample preparation. A review of the analysis of ceramics by LA-FTMS may be of interest in the above context (92/ 1428). A number of conference papers have appeared in the last year describing the use of GD techniques for the characteri- zation of ceramic materials.Few analytical details are provided in these abstracts but the development of r,f powered GD sources has opened up real possibilities for application to the direct anal-vsis of ceramic insulators. Examples have included the use of r.f. GD sources for AES (9 1/3608 911C3723 92/C559 92/C3526) and MS (9 l/C3724 92/C3526). The move towards cell geometries accommodating flat samples instead of the older pin type configurations represents a significant step forward in a move towards the practical application of the technique in the ceramics field (911C3724 91/C3731).JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY DECEMBER 1992 VOL.7 385R LOCATION OF REFERENCES The full list of references cited in this Update have been published as follows 9113585-9114050 J. Anal. At. Spectrorn. 1991 6(8) 323R-340R. 9211-921425 J. Anal. At. Spectrom. 1992 7( I) 53R-66R. 92lC426-9211447 J. Anal. At. Spectrom. 1992 7(3) 1 19R-154R. 9211448-9212589 J. Anal. At. Spectrorn. 1992 7(4) 173R-2 13R. 9212590-92lC3494 J Anal. At. Spectrom. 1992 7( 5) 247R-277R. 92lC3495-9214073 J. Anal. At. Spectrom. 1992 7(7) 329R-348R. Abbreviated forms of the literature references quoted (excluding those to Conference Proceedings) are given on the following pages for the convenience of the readers. The full references names and addresses of the authors and details of the Conference presentations can be found in the appropriate issues of JAAS cited above.Abbreviated List of References Cited in Update 9113053. Zavod. Lab. 1990 56(4) 40. 9113587. J. Anal. At. Spectrom. 1991 6 205. 9113589. J. Anal. At. Spectrom. 1991 6 2 15. 9113590. J. Anal. At. Spectrom. 1991 6 22 1. 9113598. Analyst 1991 116 51 1. 9113599. Analyst 1991 116 5 17. 9113608. Spectrochim. Acta Part B 199 1,46,483. 9113773. J. Anal. At. Spectrom. 1991 6 261. 9113795. Fresenius J Anal. 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ISSN:0267-9477    

DOI:10.1039/JA992070349R

出版商:RSC    

年代:1992

数据来源: RSC

摘要:

388R JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY DECEMBER 1992 VOL. 7 Glossary of Abbreviations Whenever suitable elements may be referred to by their chemical symbols and compounds by their formulae. The following abbreviations are used extensively in the Atomic Spectrometry Updates. a.c. AA AAS AE AES AF AFS AOAC APDC ASV CCP CMP CRM cw d.c. DCP DDDC DMF DNA EDL EDTA EDXRF EIE EPMA ETA ETAAS ETV EXAFS FAAS FAB FAES FAFS FI FPD Fr FTMS GC GD GDL GDMS Ge(Li) HCL h.f. HG HPGe HPLC IAEA IBMK ICP ICP-MS IR alternating current atomic absorption atomic absorption spectrometry atomic emission atomic emission spectrometry atomic fluorescence atomic fluorescence spectrometry Association of Official Analytical Chemists ammonium pyrrolidinedithiocarbamate anodic-stripping voltammetry capacitively coupled plasma capacitively coupled microwave plasma certified reference material continuous wave direct current d.c.plasma diammonium diethyldithiocarbamate N,N-dimethylformamide deoxyribonucleic acid electrodeless discharge lamp ethylenediaminetetraacetic acid energy dispersive X-ray fluorescence easily ionizable element electron probe microanalysis electrothermal atomization electrothermal atomic absorption electrothermal vaporization extended X-ray absorption fine structure flame AAS fast atom bombardment flame AES flame AFS flow injection flame photometric detector Fourier transform Fourier transform mass spectrometry gas chromatography glow discharge glow discharge lamp glow discharge mass spectrometry lithium-drifted germanium hollow cathode lamp high frequency hydride generation high-purity germanium high-performance liquid chromatography International Atomic Energy Agency isobutyl methyl ketone (4-methylopentan-2- inductively coupled plasma inductively coupled plasma mass infrared (ammonium pyrrolidin-1-yl dithioformate) spectrometry spectroscopy one) spectrometry IUPAC LA LC LEAFS LEI LMMS LOD LTE MECA MIP MS NAA NaDDC NIES NIST NTA OES PICE PIXE PMT PPb PPm PTFE QC r.f.REE(s) RIMS RM RSD SIB SEC SEM SFC Si(Li) SIMAAC SIMS SIN SR SRM SSMS STPF TCA TIMS TLC TOP0 TXRF u.h.f. uv VDU vuv WDXRF XRF International Union of Pure and Applied Chemistry Laser ablation liquid chromatography laser-excited atomic fluorescence laser-enhanced ionization laser-microprobe mass spectrometry limit of detection local thermal equilibrium molecular emission cavity analysis microwave-induced plasma mass spectrometry neutron activation analysis sodium diethyldithiocarbamate National Institute for Environmental National Institute of Standards and nitrilotriacetic acid optical emission spectrometry particle-induced gamma-ray emission particle-induced X-ray emission photomultiplier tube parts per billion parts per million polytetrafluoroethylene quality control radio frequency rare earth element(s) resonance ionization mass spectrometry reference material relative standard deviation signal to background ratio size-exclusion chromatography scanning electron microscopy supercritical fluid chromatography lithium-drifted silicon simultaneous multi-element analysis with a continuum source secondary ion mass spectrometry signal to noise ratio synchrotron radiation Standard Reference Material spark source mass spectrometry stabilized temperature platform furnace trichloroacetic acid thermal ionization mass spectrometry thin-layer chromatography trioctylphosphine oxide total reflection X-ray fluorescence ultra-high frequency ultraviolet visual display unit vacuum ultraviolet wavelength dispersive X-ray fluorescence X-ray fluorescence spectrometry Studies Technology

ISSN:0267-9477    

DOI:10.1039/JA992070388R

出版商:RSC    

年代:1992

数据来源: RSC

摘要:

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Paudyn A Determination of Pb Hg Sn As and Se using atomic spectrometry detectors (e.g. ICP-MS) for gas chromato- graphy. (Res. Centre Anal. and Testing N.E. Normal Univ. Changchun Jilin China). 92/C4128. Huang M. Jiang Z.-c. Zeng Y. Study on vaporizer for ETV-ICP-AES. (Dept. Chem. Wuhan Univ. 430072 Wuhan China). 92K4129. Ye Y.-c. Fluctuation of analytical signal in ICP-AES I. Effect of the carrier gas flow rate. (Dept. Chem. Central Iron & Steel Res. Inst. 100081 Beijing China). 92/C4 130.Chen Z.-n. Computational algorithm of improvingJOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY DECEMBER 1992 VOL. 7 391R matrix effect in ICP-AES. (Dept. Appl. Chem. Harbin Inst. Technol. 150006 Harbin China). 92/C4131.Qiu D. Lin B. Ouyang S. Hydride generation 92/C4 92/C4 92/C4 92/C4 92/C4 92IC4 92lC4 sequence of hydride-forming elements in hydrogenation reaction. (Chem. Dept. Fudan Univ. 200433 Shanghai China). 32. Liu K . 4 Preliminary investigation of a new-type solid sampling system of ICP. (Inst. Chem. Metall. Acad. Sin. Beijing 100080 China). 33. Nygaard D. D. New concept in wavelength scanning mechanisms for sequential ICP spectrometers. (Baird Corp. 125 Middlesex Turnpike Bedford MA 0 1730 USA). 34.Chen P. Luo YA Bai M. Shen L.-s. Research in ICP-AES intelligent database system.(Univ. Sci. Tech- nol. China). 35.Zhuo Z. Xue Z.-g. Huang Y.-x. Zhang X.-d. Qu R.-q. Application of derivative transformation and orthogonal function transformation in ICP-AES. (Anal. Centre East China Normal Univ. 200062 Shanghai China). 36.Zhang Z.-y. Piao Z.-x. Zeng X.-j. Application of factor analysis to correction of spectral overlap inter- ference in ICP-AES. (Changchun Inst. Appl. Chem. Chinese Acad. Sci. 130022 Changchun China). 37. Zhang D.4 Marked B. Natural background content of rare earth elements in a forest ecosystem and transfer factors of rare earth elements from soil to plant. (Henan Central Lab. Minist. Geol. Mineral Resour. 450053 Zhengzhou China). 38.Xia0 J. Li Q.-y. Qian H.-w. Li W.-c. Zhang Z.-x. Matrix effect of easily ionized elements of the spatial distribution of electron number density in ICP dis- charge using optical fibre probe diagnostic.(Dept. Chem. Zhongshan Univ. 5 10275 Guangzhou China). 92fC4139. Zhang J.-h. Ye D.-m. Zhang H.-q. Yu A.-m. Duan Y.-x. Jin Q.-h. Study on determination of phosphorus by MIP-AES. (Dept. Chem. Jilin Univ. 130023 Changchun China). 92fC4140. Liu M.-z. Shi W. Chen H.-j. Chen Z.-x. Xu X.-z. Guo X.-w. Jin Q.-h. Study on atomic fluorescence spectrometry system with pulse-operated hollow cath- ode and microwave plasma torch. (Beijing Haiguan Instrum. P.O. Box 8054 100083 Beijing China). 92lC414 1. L’vov B. V. Polzik L. K. Romanova N. P. Formation of soot during the decomposition of gaseous carbides in ETAAS. (Dept. Anal. Chem. Leningrad State Tech.Univ. Leningrad 19525 1 Russia). 92lC4142. Ni Z.-m. Yan X.-p. Determination of lead by hydride generation atomic absorption spectrometry with in situ concentration in a zirconium coated graphite tube. (Res. Centre Eco-Environ. Sci. Acad. Sin. P.O. Box 934 Beijing China). 92IC4143. Yan X.-p. Ni Z.-m. Determination of kinetic para- meters for the formation of gaseous analyte atoms from the absorbance signal in electrothermal atomic absorp- tion spectrometry a computer simulation study. (Res. Centre Eco-Environ. Sci. Acad. Sin. P.O. Box 934 Beijing China). 92fC4144. Willie S. N. Sturgeon R. E. Luong V. T. Berman S. S. Furnace atomization plasma emission spectrometry. (Inst. Environ. Chem. Natl. Res. Council Canada Montreal Road Ottawa Ontario K1 A OR9 Canada).92/C4145.Fang Z.-l. Is flow-injection creating a new era of progress for atomic absorption spectrometry?. (Flow- injection Anal. Res. Centre Inst. Appl. Ecol. Acad. Sin. 110015 Shenyang China). 92K4 146. Liu W.-y. Li J.-x. Application of ultrasonic slurry sampling (USS) in atomic spectral analysis. (Inst. Rock Miner. Anal. Minist. Geol. Miner. Resour. Beijing 100037 China). 92K4 147. Bojovic V. Jeremic M. Antie-Jovanovic A. Lalib M. Study of some interferences in the atomic absorption spectrometry of magnesium. (Dept. Phys. Chem. Fac. Sci. Univ. Belgrade Studentski trg 16 1 1000 Belgrade Yugoslavia). 92/C4 148. Ma Y.-z. Comparison of calculated and experimental 92lC4 92lC4 92/C4 92/C4 92/C4 9 2/C4 92/C4 values of characteristic mass for cadmium in ETAAS. (Inst.Anal. Measure. Chinese Res. Acad.. Environ. Sci. 1000 1 2 Beijing China). 49. Ma Y.z. Studies of the determination of chromium in different atomizers in view of absolute analysis in ETAAS. (Inst. Anal. Measure. Chinese Res. Acad. Environ. Sci. 10001 2 Beijing China). 50. Yasuda K. Hirokawa K. Measurement of effective temperature in a graphite furnace and its application in atomic absorption. (Naka Wks. Hitachi Katsuta Ibaraki 3 12 Japan). 51.Gucer S. ozdemir Y. Some speciation studies of Cd and Cu in Turkish teas. (Inonu Univ. Fac. Sci. Arts Dept. Chem. 44069 Malatya Turkey). 52.Zeng X.-b. Zhong Y.4 Liang S.-c. Modification of aluminium atomization in graphite furnace atomic absorption spectrometry. (Inst. Chem. Acad. Sin. 100080 Beijing China). 53.He J.4 Study on the bioaccumulation of several metals in a strain of algae (anabaena) by AAS.(Centre Anal. Testing Wuhan Univ. 430072 Wuhan China). 54.Hou S. Chang C. Lin S A Studies on absolute analysis for probe atomization in graphite furnace atomic absorption spectrometry. (China Univ. Geosci. 430074 Wuhan China). 55. Xu. S.-k. Sperling M. We15 B. Determination of cadmium nickel and cobalt in biological samples by flow injection flame atomic absorption spectrometry combined with on-line coprecipitation preconcentration without filtration. (Flow Injection Anal. Res. Centre Inst. Appl. Ecol. Acad. Sin. Shenyang 110015 China). 92/C4156.Deng B. Liu Q. Studies on the atomization mecha- nism of elements on the graphite probe surface in the graphite furnace atomization mechanism of strontium nitrate.(Dept. Chem. Tsinghua Univ. 100084 Beijing China). 92/C4157.Lin W.-y. He Y.-z. Luo J.-h. Lin K. Huang L.-j. Huang W.-q. Wu K.-g. Mo C.-z. Determination of silicon in blood by optical temperature control Zeeman flameless atomic absorption spectrometry. (Instrum. Anal. Res. Centre Guangxi 530022 Nanning China). 92/C4158.Lin S.-q. Chen S.-y. Bi M.-h. Huang Y.4 Qi W.-q. Effect of metal-coated tubes on determination of arsenic by ETAAS. (Structure Res. Lab. Univ. Sci. Technol. China Hefei 230026 Anhui China). 92/C4159. Feng X.-j. Jiang Y.-c. Fu B. Determination of trace amounts of arsenic antimony selenium and tellurium in nickel metal by hydride atomic fluorescence spectro- metry. (Dept. Anal. Chem. Beijing Central Res. Inst. Mining Metal. 100044 Beijing China).92/C4 160. Duan Y.-x. Zhang H.-q. Lu H. Hou M.-g. Du Z.-h. Jin Q.-h. Determination of some elements by micro- wave-induced plasma atomic absorption spectrometry with ultrasonic nebulization sample introduction sys- tem. (Dept. Chem. Jilin Univ. 130023 Changchun China). 92/C4 16 1. Lang H.-y. Xie Z.-h. Lei Z.-h. Application of atomic absorption spectrometry to organic analysis (1)- Indirect determination of nicotine in tobacco. (Dept. Chem. Northwest Univ. 7 10069 Xian China). 9 2 x 4 162. Hou C.-f. Wang H.-q. Qiao G.-x. Zhao N. Jiang Y. Yang H.-l. Study on the in-line chelate resin concen- trate and AAS method for the determination of Cd Co Cr Cu Mn Ni Pb and Zn in water. (Liaoning392R JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY DECEMBER 1992 VOL.7 Provincial Environ. Monit. Centre 1 1003 1 Shenyang China). 92/C4 163. Li C.4 Vertical atomization system for AAS. (Instrum. Anal. Res. Centre Guangdong Inst. Technol. 510090 Guangzhou. China). 92/C4164. Bao C.4 Zhang F.-j. Liu C.-h. Determination of trace germanium in plants by graphite furnace atomic absorption spectrometry with MIBM-DMF extraction. (Changchun Univ. Earth Sci. 130026 Changchun China). 92/C4165.Xu Z.-g. Xiong Y.-f. Xu D.-g. Study on slotted tube atom trapping technique. (Centre Anal. Testing Zhejiang Univ. 3 10027 Hangzhou China). 92/C4 166. Qi W.-q. Chen Y.4 Cao J.-s. Chang M.-s. Determi- nation of beryllium in environmental samples by matrix modifier and coated graphite furnace atomic absorption spectrometry. (China Nat. Environ. Monit.Centre 1000 12 Beijing China). 92/C4167.Liu Q. Deng B. Studies on the atomization mecha- nism of elements on the graphite probe surface in the graphite furnace-IX The atomization mechanism of antimony chloride. (Dept. Appl. Chem. Taiyuan Univ. Technol. 030024 Taiyuan China). 92/C4 168. Hu F. Three-dimensional study on atomization mecha- nisms of IIA elements in air-acetylene flame. (Qinghai Inst. Salt Lakes Acad. Sin. 810008 Xining China). 92/C4 1 69. Gohshi Y.-c. Synchrotron radiation X-ray fluorescence analysis. (Dept. Indust. Chem. Fac. Engin. Univ. Tokyo Tokyo Japan). 92/C4 170. Wang B. Shi G.-z. Liang F. New method of directly determining zinc in human hair by X-ray fluorescence spectrometry. (Centre Anal. Testing Wuhan Univ. Wuhan 430072 Hubei China).92/C4 17 1. Xiao Y. Chao Z.-y. Wu Y.-g. SR microprobe analysis of the poisoning situation of catalytic processor. (Syn- chrotron Radiat. Lab. Inst. High Energy Phys. Acad. Sin. 100039 Beijing China). 92/C4 172. Nishino M. Tanaka T. Okashita H. XRF analysis of carbon in organic compounds. (Kyoto Anal. Appl. Centre Shimadzu Corp. 1 Nishinokyo-Kuwabaracho Nakagyo-ku Kyoto 604 Japan). 92/C4173. Nakagawa Y. Kohara K. Komi H. Niwa N. Monte Carlo approach to quantitative analysis of thin films with EPMA. (Kyoto Anal. Appl. Centre Shimadzu Corp. 1 Nishinokyo-Kuwabaracho Nakagyo-ku Kyoto 604 Japan). 92/C4 174. Ji A. Wu M.-m. Tao G.-y. Quantitative determina- tion of the bridging and non-bridging oxygen abundance in glasses by X-ray fluorescence spectrometry. (Shanghai Inst.Ceram. Acad. Sin. 200050 Shanghai China). 92/C4175. Li G.-h. Bu W. Fan S-z. Rapid determination of multi-elements in the animal sample by X-ray fluores- cence spectrometry Inst. Geophys. Geochem. Explor. Minis. Geol. Miner. Resour. 102849 Langfang China). 92/C4176. An Q.-x. Zhan X.-c. Chao Z.-y. Wu Y.-r. Xiao Y.-n. Study of geological standard reference for SR X-ray microanalysis. (Inst. Rock Miner. Anal. 100037 Beij- ing China). 92K4177. Wang Y.-m. Bai Y.-z. Li G.-I. Li J. Software for radioisotope source exciting proportional counter mea- suring EDXRF system. (China Build. Mater. Acad. C h ina). 92/C4178. Wu Y.-r. Chao Z.-y. Hong R. Xiao Y.-n. Huang Y.-x. Li Q.-j. Observation on trace elemental change in hair of pregnant women. (SR Lab. Inst. High Energy Phys.Acad. Sin. China). 92/C4 179. Huang Y.-c. Wang Q.-g. Xie G.-g. Determination of multi-elements in mussel by X-ray fluorescence spec- troscopy. (Res. Centre Eco-environ. Sci. Acad. Sin. P.O. Box 934 100083 Beijing China). Papers 92/C4 180-92K4205 were presented at ICP-a source for the ' ~ O S Macquarie University 24-27 November 199 1. 92/C4180. Stux R. A new solid state spectrographic detector offering continuous wavelength coverage for qualitative and quantitative analysis. (Thermo Jarrell Ash 8E Forge Pkwy. Franklin MA 02038 USA). 92/C418 1. Cassagne P. C. Fry R. C. Gower G. H. A new approach in ICP-AES. (Fisons Instruments Applied Research Laboratories En Vallaire 1024 Ecublens Switzerland). 92/C4 182. Holmes K. The use of and recent developments with official fibres in ICP spectrometry.(Spectro Analytical Instruments 4 190 Kleve Germany). 92/C4183. Cassagne P. C. Eastgate A. E. Dahlquist R. L. Fry R. C. Developments in sample introduction in ICP spectrometry. (Fisons Instruments Applied Research Laboratories En Vallaire 1024 Ecublens Switzerland). 92/C4 184. Nham T. T. Sub-ppb measurements using inductively coupled plasma atomic emission spectrometry with an ultrasonic nebulizer. (Varian Australia Pty. Ltd. 679 Springvale Rd. Mulgrave Victoria 3 17 1 Australia). 92/C4 185. Bishop J. G. Analysis of samples with high dis- solved salts and particulate matter by ICP-OES. (GBC Scientific Equipment Pty. Ltd. 23 Brooklyn Ave. Dandenong Victoria 3 175 Australia. 92/C4 186. Zborowski M. Advances in ICP-AES optics and sources.(Precision Equipment Co. Pty. Ltd. Australia). 92/C4 187. Dale L. S. Farrell 0. P. Implications of isotope ratio measurements using ICP-MS for environmental and biomedical research. (CSIRO Div. Coal and Energy Technol. Lucas Heights Res. Lab. PMB7 Menai New South Wales 2234 Australia). 92/C4 188. Louie H. Driving your dollar further with ICP-MS. (Trace Elements Section Australian Government Anal. Lab. 1 Suakin St. New South Wales 2073 Australia). 92/C4 189. Hutton R. C. McCurdy E. J. The PQe-a new routine ICP-MS for the 90s. (VG Elemental Ion Path Road Three Winsford Cheshire UK CW7 3BX). 92/C4190. Dale L. S. Farrell 0. P. Lyall C. S. The determina- tion of heavy metals in environmental samples by ICP- MS. (CSIRO Div. Coal and Energy Technol. Lucas Heights Res.Lab. PMB7 Menai New South Wales 2234 Australia). 92/C4 19 1. Finlayson R. Spectroscopic tricks for ICP-AES analy- sis. (Univ. New South Wales POB 1 Kensington New South Wales 2033 Australia). 92/C4192. Hutton R. C. McCurdy E. J. Recent developments in ICP-MS. (VG Elemental Ion Path Road Three Wins- ford Cheshire UK CW7 3BX). 92/C4193. Jordan P. A quality control concept for ICP emission and ICP mass spectrometry. (Perkin Elmer Pty. Ltd. 30 Miles St. Mulgrave Victoria 3 170 Australia). 92K4194. Dale L. S. ICP-photons or ions? (CSIRO Div. Coal and Energy Technol Lucas Heights Res. Lab. PMB7 Menai New South Wales 2234 Australia). 92/C4195. Kimber G. M. Krieger B. L. Selby M. Petty J. D. Sweatman D. R. Potential for discontinuous flow analysis with inductively coupled plasma sources.(Centre for Anal. Sci. QUT GPO Box 2434 Brisbane Queensland 400 1 Australia). 92/C4196. Byrne J. P. Gregoire D. C. Lamoureux M. Chakra- barti C. L. ETV-ICP-MS and its relation to solution nebulization ICP-MS and graphite furnace AAS. (Dept. Chem. Univ. Technol. Sydney P.O. Box 123 Broad- way New South Wales 2007 Australia) 9 2 x 4 197. Matousek J. P. Control and enhancement of electro- thermal vaporization for inductively coupled plasma spectrometry. (Dept. Anal. Chem. Univ. New South Wales P.O. Box 1 Kensington New South Wales 2033 Australia).JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY DECEMBER 1992 VOL. 7 393R 92/C4 198. Stux R. A novel method for the analysis of gold in ores using solid sampling ICAP following a fire assay preconcentration. (Thermo Jarrell Ash 8E Forge Pkwy.Franklin MA 02038 USA). 92/C4 199. Abdullah M. Horlick G. Karanassios V. Haraguchi H. Direct analysis of liquids and solids in ICP-AES utilizing a graphic cup direct insertion device instru- mentation and applications. (Water Board Scientific Services Trace Anal. Sect. 51 Hermitage Rd. West Ryde New South Wales Australia). 92K4200. Holmes K. Simultaneous spectrochemical analysis of water soils and sewage sludges. (Spectro Analytical Instruments 4 190 Kleve Germany). 92/C4201.Nham T. T. Application of a high resolution ICP emission spectrometer for the analysis of geological samples. (Varian Australian Pty. Ltd. 679 Springvale Rd. Mulgrave Victoria 3 17 1 Australia). 92/C4202.Riley K. W. Dotter L. E. Godbeer W. C. Forty samples for forty elements in sixty minutes by ICP- AES-sample preparation the weak link. (CSIRO Div.of Coal and Energy Technol. P.O. Box 136 North Ryde 2 1 1 3 New South Wales Australia). 92/C4203. Atherton A. J. Kimber G. M. Selby M. Kaiser J. E. A comparison of torch designs-the all glass demount- able versus fixed versus Teflon base demountable. (Centre for Anal. Sci. QUT P.O. Box 2434 Brisbane Queensland 400 1 Australia). 92/C4204. Palmer L. T. Warner I. M. Parouchais C. Mode of internal standardizationkalibration for routine analysis by inductively coupled plasma mass spectrometry (ICP- MS). (South Australian Department of Agriculture State Chemistry Laboratories (SCL) Australia). 92/C4205.Eames J. C. Craven S. J. Whitford D. J. The determination of rare earth elements in geological materials by isotope dilution ICP-MS.(CSIRO Division of Exploration Geoscience Canberra Australia). Papers 92X4207-92fC4258 were presented at the Ffth Italo- Hungarian Symposium on Spectrochemistry Quality Control and Assurance in Life Sciences Pisa Italy 9- 1 3 September 199 1. 92/C4206. Biancifiori M. A. Del Monte Tamba M. G. Standardi- zation and reference materials a survey of the Italian situation. (ENEA CRE Casaccia Via Anguillarese 30 1 00060-Rome Italy). 92K4207.Del Monte Tambe M. G. Biancifiori M. A. CNMR the new Italian organization for reference materials. (Centro Sviluppo Materiali Via di Caste1 Romano 1001 102 00 1 29-Rome Italy) 92X4208. Griepink B. How to detect and avoid analytical errors. (Commun. Bur. Ref. Commission Eur.Commun. Rue de la Loi 200 B-1049 Brussels Belgium). 92K4209. Watters R. L. Jr. Use of standard reference materials 92/C42 92/C42 92/C42 92/C42 92/C42 in spectrometric analysis quality assurance pro- grammes. (Natl. Inst. Stand. Technol. Gaithersburg MD 20899 USA). 0. Heltai Gy. Fuleky Gy. Soil analysis and the nutrition capacity. (Univ. Agricul. Sci. Godollo H-2 103 Hun- l.Allegrini I. De Santis F. Febo A. Metrology of atmospheric pollution. (Inst. Atmos. Pollut. CNR Via Salaria km 27.300 CP 10 0001 6-Monterotondo Sta- zione Rome Italy). 2.Bezur W. Varga J. Pungor E. Evaluation of metal- contaminated waste using the cup-flame AAS method. (Inst. Gen. Anal. Chem. Tech. Univ. Budapest XI 152 1 Budapest Hungary). 3.Cervelli S. Di Giovanni F. Use of quadrupole mass spectrometers in environmental studies determination of I5N abundances.(Inst. Soil Chem. CNR Via Corri- doni 78 27 100-Pisa Italy). 4.Kantor T. Zaray Gy. ICP-AES analysis of pure gary). substances using halogenation-volat ilization techniques. (Inst. Inorg. Anal. Chem. Eotvos Lorand Univ. P.O. Box 32 Budapest-I 12 H-1518 Hungary). 92/C42 1 5. Marabini M. A. Passariello B. Barbaro M. Induc- tively coupled plasma mass spectrometry capabilities and applications. (Inst. Treatment of Miner. CNR Via Bolognola 7 00 1 38-Rome Italy). 92/C42 16. Posta J. Berndt H. Improvement of the analytical performance of the FAAS method by hydraulic high pressure sample introduction. (Inst. Inorg. Anal. Chem. Kossuth Lajos Univ. P.O. Box 21 Debrecen H-4010 H u n gary ) . 92K4217. Wegscheider W.Neubiick R. Otto M. Schierle C. Automated qualitative analysis by ICP-OES with fuzzy logic and neural network support. (Inst. Anal. Chem. Microchem. Radiochem. Graz Univ. Technol. Tech- niker Str. 4 A-80 10 Graz Austria). 92/C42 1 8. Demeny D. Radziuk B. Investigation on the practical applications of FANES. (Dept. Inorg. Anal. Chem. Kossuth Lajos Univ. P.O. Box 2 1 Debrecen H-40 10 Hungary). 92/C42 19. Pap T. Inczedy J. Fitting equations to spectroscopic signals. (Inst. Anal. Chem. Univ. Veszprem P.O. Box 158 Veszprem H-8201 Hungary). 92K4220. Lakatos J. Lakatos I. Distribution of atoms in air-acetylene flames the effect of flow and gas expan- sion on atom distribution. (Res. Lab. Mining Chem. Hungarian Acad. Sci. P.O. Box 2 Miskolc-Egyetem- varos Hungary).92/C422 1. Colinet E. Quality assurance in the field of biomedical analyses the role and the contribution of the BCR programme of the European communities. (Commis- sion Eur. Commun. Commun. Bur. Ref. (BCR) 200 Rue de la Loi B-1049 Brussels Belgium). 92/C4222. Moriai G. Patriarca M. Menditto A. Organization of interlaboratorial quality assurance programmes for the analysis of trace elements in blood evaluation of procedures and analysis of data. (1st. Superiore di Sanita Viale Regina Elena 299 00 16 1 -Rome Italy). 92K4223. Patriarca M. Menditto A Morisi G. Performance of Italian laboratories in determination of trace elements in blood. (1st. Superiore di Sanita Viale Regina Elena 299 00 16 1 -Rome Italy). 92/C4224. Bozsai G. Quality control and assurance in hair analysis.(Natl. Inst. Hyg. Gyali lit 2-6 Budapest H-1966 Hungary). 92/C4225.Zaray Gy. Kultsar E. Varga I. Kantor T. Quality control of ceramic powder production by ICP-AES methods. (Inst. Inorg. Anal. Chem. Eotvos Lorand Univ. P.O. Box 32 Budapest 112 H-1518 Hungary). 92/C4226. Orvini E. Nuclear methods fortraceelementsdetermina- tion in fossil fuels. (Nucl. Chem. Sect. Dept. Gen. Chem. Univ. Pavia Via Taramelli 12 27 1 00-Pavia Italy). 92K4227. Paksy L. Use of mathematical-statistical methods in spectrochemical quality control. (Metalcontrol Kft. P.O. Box 557 Miskolc H-3510 Hungary). 92K4228. Hlavay J. Analysis of respirable dust. (Dept. Anal. Chem. Univ. Veszprem P.O. Box 158 Veszprem H-820 1 Hungary). 92K4229. Tittarelli P. Biffi C. Applications of slurry analysis by ETAAS in environmental quality control. (Stazione Sperimentale per i Combustibili 20097-San Donato Milanese (Mi) Italy). 92/C4230.Halmos P.Borszeki J. Use of ICP-OES method in ion-exchange chromatography. (Dept. Anal. Chem. Univ. Veszprem P.O. Box 158 Veszprem H-8201 H u nga ry ) . 92/C423 1. Fodor P. Atomic spectroscopy quality control of food industry in Hungary. (Chem. Dept. Univ. Hortic. Food Ind. Villanyi lit 3 I Budapest H- 1052 Hungary).394R JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY DECEMBER 1992 VOL. 7 921C4232. Sabbioni E. Metallotoxicology research at the JRC- ISPRA present trends and perspectives for the future. (CEC Life Sci. Unit Environ. Inst. JRC Ispra Estab- lishment 2 1020-Ispra (Va) Italy). 92K4233. Caroli S. Accuracy syndrome in trace element analysis of biological samples.(1st. Superiore di Sanita Viale Regina Elena 299 00 16 1 -Rome Italy). 92/C4234.Boniforti R. Data quality as an essential need for marine environment studies. (ENEA Res. Center Energy Environ. Forte di Santa Teresa 19100-La Spezia Italy). 921C4235. Brondi M. Torcini S. Determination of T I in natural waters by means of graphite furnace atomic absorption spectrometry. (ENEA CRE Casaccia Via Anguillarese 30 1 00060-Rome Italy). 921C4236. Buzaisi-Gyiirfi A. Herceghalmi-Pankotai M. Pankotai- Gilinger M. Spectrochemical determination of metals content in pesticides and treated vegetables. (Inst. Mater. Testing Qual. Control P.O. Box 114 Budapest H-175 1 Hungary). 921C4237. Caroli S. Mura G. Fornarelli L. Caimi S.Pilot study on the content of some trace elements in Artemia Salina L. (1st. Superiore di Sanita Viale Regina Elena 299 00 1 6 1 -Rome Italy). 921C4238. Cerjan-Stefanovit s. Kasteian-Macan M. Spectro- photometric observations of solar cells elution in waters. (Dept. Anal. Chem. Fac. Technol. Univ. Zagreb MaruliCev trg 20 41 000 Zagreb Yugoslavia). 92/C4239.Costantini S. Giordano R. Beccaloni E. Perani C. Grego S. Experimental approach to aluminium phyto- toxicity. (1st. Superiore di Sanita Viale Regina Elena 299 001 6 1 -Rome Italy). 921C4240. Fagioli F. Landi S. hcatelli C. Caiias De Moreno F. 921C424 1 Magarini R. Element determination in organic ma- trices (flying ashes coals and resins) by atomic spectro- scopic techniques with sampling of carbonaceous slurry. (Dept.Chem. Univ. Ferrara Via Luigi Borsari 46 44 I 00-Ferrara Italy). Horvath Zs. Lisztity A. Varga I. Role of spectro- chemical analysis in the study of the composition of atmospheric precipitation and aerosol samples in re- mote environments. (Inst. Inorg. Anal. Chem. Eotvos Lorand Univ. P.O. Box 32 Budapest 112 H-1518 Hungary). 921C4242. Karpati P. Wegscheider W. Borszeki J. Contribu- tions to the analysis of bauxites by inductively coupled plasma optical emission spectrometry using the Kalman filter technique. (Dept. Anal. Chem. Univ. Veszprem P.O. Box 158 Veszprem H-8201 Hungary). 92/C4243. Racz L. Papp L. Racz J. Study of element migration in soil-mushroom systems by atomic spectroscopic methods. (K. Eszterhazy Teacher’s Training Coll. Eger Hungary ). 921C4244. Santarsiero A.Ottaviani M. Heavy metals in residues from hospital solid waste incineration. (1st. Superiore di Sanita Viale Regina Elena 299 001 61-Rome Italy). 92/C4245.Alimonti A. Fornarelli L. Coni E. Caroli S. Bolis G. B. Cristallini E. Assessment oftrace metal concentra- tions in human lungs of urban subjects. (1st. Superiore di Sanith Viale Regina Elena 299 00 16 1 -Rome Italy). 92/C4246.Bortoli A. Gerotto M. Marchiori M. Palonta R. Troncon A. Accuracy of ICP-MS measurements and early detection of previously unsuspected elements. (Presidio Multizonale di Prevenzione ULSS 36 Via Campo della Lana 60 1 30 125-Mestre Italy). 92/C4247. Caroli S. Fornarelli L. Delle Femmine P. Falconieri P. Assessment of reference values for trace elements in human milk.(1st. Superiore di Sanita Viale Regina Elena 299 00 16 1-Rome Italy. 921C4248. Caroli S. Violante N. Quaglia M. G. Lopez A. Trace elements as potential markers for identifying the geo- graphical origin of addictive drugs. (1st. Superiore di Sanith Viale Regina Elena 299 00 16 1 -Rome Italy). 92/C4249.Caroli S. Senofonte O. Violante N. Fornarelli L. Power A. Assessment of reference values for elements in hair of normal urban subjects. (1st. Superiore di Sanita Viale Regina Elena 299 00 1 6 1 -Rome Italy). 92/C4250. D’Ulivo A. Lampugnani L Zamboni R. Atomic fluorescence spectrometry for trace element determina- tion in biological matrices of environmental interest. (ICAS-CNR Dept. Chem. Univ. Pisa Via Risorgi- mento 35 56 126-Pisa Italy). 921C425 1. Giordano R. Costantini S.Vernillo I. Moramarco A. Rasi V. Giustolisi R. Balacco-Gabrieli C. Calcium potassium zinc and copper determination in catarac- tous human lenses. (1st Superiore di Sanita Viale Regina Elena 299 00 1 6 1 -Rome Italy). 92/C4252. Ikrenyi K. AAS and ICP determination of As Hg and Se. (Hungarian Geol. Inst. P.O. Box 106 Budapest H- 1443 Hungary). 92/C42 5 3. Kastelan-Macan M. Diirrigl A. Cerjan-StefanoviC S. AAS detection of biologically active organometallic compounds. (Dept. Anal. Chem. Fac. Technol. Maruli- Cev trg 20 41000 Zagreb Yugoslavia). 921C4254. Naray M. Experiences with determination of toxic substances in biologicals in external quality control assessment. (Natl. Inst. Occup. Health Nagyvarad tCr 2 Budapest H- 1450 Hungary). 92/C4255. Szilvassy-Vamos Zs.Lbar J. Horvath M. Pozna A. Study of interfering effects of calcium in the analysis of selenium traces in human hair by a hollow cathode AES spectrographic method. (Dept. Radiochem. Phys. Univ. Veszprem P.O. Box 158 Veszprem H-8201 Hungary). 92/C4256. Michaelis M. Knapp G. Design of a modular off-line sample preparation system for elemental trace analysis using the TraceCon preconcentration system. (Knapp Logistik Automation GmbH Knapp-Strasse 5-7 A-8042 Graz Austria). 92/C4257.Violante N. Petrucci F. Delle Femmine P. Caroli S. Comments on the determination of A1 in biological fluids by ICP-AES. (1st. Superiore di Sanita Viale Regina Elena 299 00 16 1 -Rome Italy). 92/C4258.&nicki W. Spectroscopic study of argon MIP dis- 9214259. 9214260. 921426 1.9214262. 9214263. charge used for analysis of solutions. (Inst. Inorg. Chem. Metall. Rare Elements Tech. Univ. Wroclaw Wybrzeze St. Wyspianskiego 27 50-370 Wroclaw Poland). Eissa N. A. Sallam H. A. Salah N. El Enany N. 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Spectrosc. 1991 12 87. (Chem. Dept. Hebei Univ. Baoding 07 1002 China).412R JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY DECEMBER 1992 VOL. 7 Ramon M. Barnes Editor Department of Chemistry LGRC Towers University of Massachusetts Amherst MA 01 003-0035 Telephone (413) 545-2294 fax 545-4490 0 bjective The ICP INFORMATION NEWSLETTER is a monthly journal published by the Plasma Research Group at the University of Massachusetts and is devoted exclusively to the rapid and impartial dissemination of news and literature information re- lated to the development and applications of plasma sources for spectrochemical analysis.Background ICP stands for inductively coupled plasma discharge which duringthe 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 atso are included in the scope of the ICP IN- FOR MA TI0 N N€ WSL E T TER. Scope As the only authoritative monthly journal of its type the ICP INFORMATION NEWSLETTER is read in more than $0 coun- tries by scientists actively applying or planning to use the ICP or other types of plasma spectroscopy. For the novice in the field the ICP INFORMATION NEWSLETTER provides a concise and systematic sourm of information and background material needed for the selection of instrumentation or the development of methodology. For the experienced scientist it offers a sin- gle-source reference to current developments and literature. Editorial The ICP INFORMATION NEWSLETTER is edited by Dr.Ramon M. Barnes Professor of Chemistry University of Mas- sachusetts at Amherst with the assistance of a 20-member Board of National Correspondents composed of leading plasma spectroscopists. The Board members from around the world report news viewpoints and developments. Dr. Barnes has been conducting plasma research on ICP and other dis- charges since 1968. He also serves as chairman of the Winter Conference on Plasma Spectrochemistry sponsored by the ICP INFORMA TlO N NEWSLETTER. R eg ul a r 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. 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ISSN:0267-9477    

DOI:10.1039/JA992070389R

出版商:RSC    

年代:1992

数据来源: RSC

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JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY DECEMBER 1992 VOL. 7 1157 Investigations into the Application of Methane Addition to the Nebulizer Gas in lnductively Coupled Plasma Mass Spectrometry for the Removal of Polyatomic Interferences Steve J. Hill Michael J. Ford and Les Ebdon Plymouth Analytical Chemistry Research Unit Department of Environmental Sciences University of Plymouth Drake Circus Plymouth Devon UK PL4 8AA The addition of methane to the nebulizer gas in inductively coupled plasma mass spectrometry is assessed as a method for the reduction of polyatomic interferences. The effect of nebulizer gas flow rate power and percentage methane on a range of species in the plasma was studied. The analyte response was not seriously affected by the addition of methane but the responses of the interfering ions ArCI+ ArO+ CIO+ and MO+ and also the random background were reduced when compared with those of an unmodified plasma. Simplex optimization was used to optimize operating parameters for maximum removal of these interferences with methane addition to the plasma.Complete removal of ArCI+ was achieved with methane addition to the nebulizer gas yielding a detection limit for As of 0.75 ng ml-' in 10% HCI. The ArO+ and ClO+ were much reduced the detection limit for Fe being 0.48 and V 2.52 ng ml-' in 10% HCI. The MO+ was reduced by a factor of 10 under the optimum conditions. Recovery tests for As Se and V further demonstrated the utility of these optimal conditions in removing interferences when compared with typical operating conditions. Several certified reference materials high in chloride were successfully analysed for As Se and V.Keywords lnductively coupled plasma mass spectrometry; mixed gases; methane addition; simplex optimiza- tion; arsenic selenium vanadium and iron determination Analysis by inductively coupled plasma mass spectrometry (ICP-MS) can be limited by the formation of polyatomic ions which interfere with the elements of interest particu- larly below mlz 80.1-4 These polyatomic ions typically come from precursors in the Ar support gas entrained atmo- spheric gases (nitrogen and oxygen) or from the sample matrix (0 OH- C1 S and P). Reduction of these can be achieved by careful setting of the instrumental parame- t e r ~ ~ * ~ * ~ especially the nebulizer gas flow rate and the foward power.s Other methods to overcome these polyatomic interferences such as hydride generati~n,~ electrothermal vaporization* or laser ablationg can involve longer sample preparation or analysis times or as in the example of high- resolution ICP-MS,'O entail greater cost.A more direct method of polyatomic interference re- moval is the use of molecular and inert gases bled into or replacing one of the three gas flows of the ICP. Evans and Ebdon11J2 first reported the use of nitrogen arid oxygen addition to the nebulizer gas for polyatomic interference removal with the former being particularly useful in reducing ArCl+. Several workers have also reported the use of nitrogen addition in ICP-MS. Lam and H ~ r l i c k ' ~ reported that polyatomics could be reduced and analyte signals enhanced with the addition of nitrogen to the outer gas.Lam and McLaren14 reduced UO+ and ArO+ levels with the addition of 8% of nitrogen to the outer gas. Beauchemin and Craigls also added nitrogen to the outer gas to reduce the interferences on Fe and Se. Hill et a1.16 reported the simplex optimization of nitrogen addition to all three gas flows of the ICP and found that nitrogen addition to the outer and nebulizer gases dramatically reduced the ArCl+ and C10+ interferences on As and V respectively. To date the majority of research has focused on the use of nitrogen addition with limited studies on oxygen and air,l1-I3 but recently attention has been turned to other gases. Smith et al.I7 investigated Xe addition to the nebulizer gas and found it reduced polyatomic interfer- ences.Allah et a1.I8 added methane to the nebulizer gas and investigated enhancements in analyte response. This paper reports a range of work performed with the addition of methane to the nebulizer gas. Initially the effect of nebulizer gas flow rate power and methane level on a range of species was assessed with and without methane addition to the plasma. Simplex optimization experiments aimed at removing ArCl+ ArO+ C10+ and CeO+ with added methane have been performed and the optimal operating conditions defined have been tested by determin- ing detection limits and recoveries of the obscured elements and also analysis of certified reference materials (CRMs) rich in chloride for these elements. Experimental Instrumentation The instrument used was an ICP mass spectrometer (PQ2 VG Elemental Winsford Cheshire UK).The sample introduction system included a modified high solids nebu- lizer (Ebdon type PSA Sevenoaks Kent UK) which allowed higher nebulizer gas flow rates than those of the standard high solids nebulizer. Methane addition to the nebulizer gas was achieved by using a gas blender (Series 850 Signal Camberley Surrey UK). For simplex optimi- zation experiments involving oxygen-based polyatomic interferences the spray chamber temperature was main- tained at around 1 "C by the use of an ice-water mixture circulated by means of a conventional water pump (Tem- pette TE 8A Techne Duxford Cambridge UK). The methane used was 99% pure. Materials and Chemicals Five CRMs that had high levels of chloride were analysed Sargasso (NIES No.9 National Institute for Environmental Studies Tsukuba Ibaraki Japan) Oyster Tissue [NIST Standard Reference Material (SRM) No. 1566a National Institute of Standards and Technology Gaithersburg MD USA] Lobster Hepatopancreas [TORT- 1 National Re- search Council of Canada (NRCC) Marine Analytical Chemistry Standards Programme Ottawa Canada] Sea- water (NASS-2 NRCC) and Urine (Seronorm reference urine Nycomed AS Oslo Norway). Standard solutions were prepared from 1000 pg ml-'1158 JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY DECEMBER 1992 VOL. 7 stock solutions of Sb As Co Pb and Se (Merck Poole Dorset UK) Be and In (Aldrich Milwaukee WI USA) and Ce U and V [prepared from Ce20 U02(N03)2.6H20 and NH,V03 respectively].Internal standardization involving use of either Sb Co or In at 100 ng ml-" was used in all experiments. All standard solutions were made up in 2% HN03 (Aristar grade; Merck). The hydrogen peroxide used in the digestion of the CRMs was 30% (Aristar; Merck). Chloride spiking of standard solutions involved use of hydrochloric acid (Aristar; Merck). Sample Preparation Approximately 0.5 g of Oyster Tissue Lobster Hepatopan- creas and Sargasso CRMs were all digested by microwave bomb digestion. The procedure has been reported else- where;I6 5 ml of nitric acid were used for the digestion of the Sargasso and a nitric acid-hydrogen peroxide mixture (3 + 2) was used for the Oyster Tissue and Lobster Hepato- pancreas digestions. After digestion the solutions were quantitatively transferred into calibrated flasks (50 ml) and made up with distilled de-ionized water.Samples were spiked with Co to a final concentration of 100 ng ml-1 as an internal standard. The sea-water and urine were diluted (2- and 50-fold respectively) and spiked with Co as above. Five replicates of each sample were prepared. Standard solutions and calibration solutions were pre- pared fresh from the stock solutions as required. Procedure Experiments to assess the influence of the instrumental operating parameters [nebulizer gas flow percentage meth- ane (v/v) and power] on various species were performed. In these experiments a standard solution of Be Ce Co In Pb and U (1 00 ng ml-1 each) and chloride (1 0 000 pg ml-I) was analysed to enable the effect of the operating parameters on analyte elements polyatomic interferences and metal oxides to be assessed.In addition the effect on the random background was monitored. These experiments were under- taken with and without methane addition to the nebulizer gas under the following operating conditions outer gas 15 1 min-l; intermediate gas 1.0 1 min-l; nebulizer gas 0.6-1.2 1 min-l; power 1200-1800 W; and CH4 either absent or variable up to 1.5%. Four separate variable step-size simplex optimizations of the operating parameters with the addition of methane to the nebulizer gas were performed to find the optimum conditions for reducing or removing ArCl+ ArO+ C10+ and CeO+. The criterion of merit for these optimizations was the Co response divided by the interference signal except for Ce where the Ce response divided by the cerium oxide signal was used.The optimal conditions defined by these simplex optimizations were tested by determination of the detection limits for As Se and V in the presence of increasing levels of chloride (0 100 1000 10000 and 33000 pg rnl-l) and Eu Gd and Sm in the presence of increasing levels of Ba Ce and La (0 1 10 and 100 pg ml-I) and also for Fe. Recovery tests under different operating conditions of similarly spiked solutions of the above elements were also Table 1 Typical ICP-MS operating parameters Parameter Value Outer gad1 min-' 15 Nebulizer gad1 min-' 0.90 Power/W 1400 Intermediate gas11 min-' 1.0 Chiller temperature/"C =z 18-20 performed. Analysis of the CRMs was undertaken under the optimum conditions for each analyte and at 'typical' operating parameters (Table 1).Results and Discussion It was found that the addition of methane to the nebulizer gas had far less profound effects on the plasma than the addition of nitrogen.I6 At the maximum possible input of methane of 1.5% v/v (so determined as above this level carbon deposition led to rapid cone blockage) there was no visible change in the plasma when compared with a plasma without addition. This is contrary to nitrogen addition to the nebulizer gas where low levels of nitrogen cause the central channel to become wider. Reflected power was approximately 10-20 W with the addition of methane. It is important to note that sample flow had to be maintained at all times when methane was being added to the plasma as without the water the carbon was not 'burnt' off the cones and they rapidly became blocked.The characteristic C2+ emission observed in organic analysis was not noted in or around the plasma. Response curves were generated with plasmas containing from 0 to 0.5% v/v methane in the nebulizer gas. These were found to be visually similar in all instances and this was supported by the elemental re- sponses which changed little with increasing methane. Effect on Various Types of Instrumental Operating Parameters With and Without the Addition of Methane to the Nebulizer Gas Effect of nebulizer gas variation Fig. l(a) and (6) shows the effect of nebulizer gas flow rate on Co+ response in area counts per second (acps) and In+:Co+ ratio respectively with and without methane addition to the nebulizer gas.Fig. l(a) shows two main features firstly the addition of methane to the nebulizer gas resulted in a reduction in the Co+ signal at most nebulizer gas flow rates when compared with the data without added 5000 I I I I + 0 C u - 0.3 0.5 0.7 0.9 1.1 Nebulizer flow rate/! min-' Fig. 1 Effect of nebulizer gas flow rate on (a) Co+ and (b) In+:Co+ ratio with A no methane added to the nebulizer gas and B 1.0% methane added to the nebulizer gas at a forward power of 1600 WJOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY DECEMBER 1992 VOL. 7 1159 240 + 180 (2 p - = 120 methane and secondly the maximum response was at a higher nebulizer gas flow rate with methane addition. The maximum responses were similar showing that with adjustment of the nebulizer gas flow rate the addition of methane did not result in a major loss of signal The need for a higher nebulizer gas flow rate could reflect a change in the shape and size of the plasma which would alter the sampling depth though this was not visibly apparent.The other analytes (Be Ce In Pb and U) all behaved similarly to co. Fig. 2(a) and (b) shows the effeFt of nebulizer gas flow rate on the UO+ response and the UO+:U+ ratio respectively. The response of UO+ was seen to be reduced at all but the highest nebulizer gas flow rates with the addition of methane to the nebulizer gas and this is more clearly demonstrated in Fig. 2(b). The percentage oxide formation was lower at all nebulizer gas flow rates when methane was added with the lowest levels being at 0.8-0.9 1 min-' for both sets of conditions with methane addition resulting in a 3-fold decrease in oxide formation.Methane addition to the nebulizer gas could reduce UO+ by effective scavenging of oxygen. The sharp increase above 1 1 min-l could reflect the role of entrained oxygen in oxide formation. The CeO+ was seen to behave similarly to the UO+. It was found that methane addition to the nebulizer gas reduced the ArCl+ response and increased the In+:ArCI+ ratio [Fig. 3 (a) and (b) respectively] when compared with the unmodified plasma. This decrease in ArCl+ could be as a result of changes in the plasma chemistry caused by the enhanced hydrogen levels present in the centre of the plasma. These results indicated that methane addition to the nebulizer gas would be of use in removing the ArC1+ interference.The random background signal at mlz 220 was seen to behave similarly to that for ArCl+. Fig. 4(a) and (b) shows the ArO+ response and In+:ArO+ ratio respectively and reveals that the introduc- - - - 60 U - m m 100 r 10000 8000 v1 CL 9 6000 c 4000 - m 0 2000 6.5 0.7 0.9 1.1 Nebulizer gas flow rate/l min-' Fig. 2 Effect of nebulizer gas flow rate on ( a ) UO+ and (6) UO+:U+ ratio x 100 (percentage oxide formation) with A no methane added to the nebulizer gas and B 1 .O% methane added to the nebulizer gas at a forward power of 1600 W - - - - - tion of methane afforded a small reduction in the ArO+ response at all but the lowest nebulizer gas flow rates and modest improvements in the In+:ArO+ ratio at most 100 000 10000 f? s 1000 1 c la) l o o t 10 J I i I 300 1 ( b ) Fig.3 Effect of nebulizer gas flow rate on (a) ArC1+ response and (b) In+:ArCl+ ratio with A no methane added to the nebulizer gas flow and B 1.0% methane added to the nebulizer gas at a forward power of 1600 W 160 000 8 120000 9 5 80000 i7j 0 40 000 0 6 5 4 b p 3 C - 2 1 0 0.5 0.7 0.9 1.1 Nebulizer gas flow rate/l min-' Fig. 4 Effect of nebulizer gas flow rate on (a) ArO+ response and (b) In+:ArO+ ratio with A no methane added to the nebulizer gas and B 1 .O% methane added to the nebulizer gas at a forward power of 1600 W1160 60000 48000 $ 36000 1 C .9J 24000 v) 12000 0 - JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY DECEMBER 1992 VOL. 7 - ( a ) - . - ' I I I 500 000 400 000 $ 300000 (0 1 C .P 200000 v) 100 000 0 0 0 + K - 0.5 0.7 0.9 1.1 Nebulizer gas flow rate/l min-' Fig.5 Effect of nebulizer gas flow rate on (a) ClO+ response and (b) In+:CIO+ ratio with A no methane added to the nebulizer gas and B 1 .Oo/o methane added to the nebulizer gas at a forward power of 1600 W 000 000 100 000 10 000 ( a ) 1000 ' 1 I I 1 100 ( b ) 10 0.1 0.01 0.5 0.7 0.9 1.1 Nebulizer gas flow rate/l min-' Fig. 6 Effect of nebulizer gas flow rate on (a) Arc+ response and (b) In+:ArC+ ratio with A no methane added to the nebulizer gas and B 1 .O% methane added to the nebulizer gas at a forward power of 1600 W nebulizer gas flow rates. The effect of nebulizer gas flow rate on the ClO+ response and the In+:ClO+ ratio is shown in Fig. 5(a) and (b) and similarly reveals only a small reduction in response and a small increase in ratio when methane is added and this only at higher nebulizer gas flow rates.The less dramatic effect of methane addition on ArO+ and ClO+ than on ArCI+ probably reflects the influence of spray chamber cooling on the oxygen based interferences as during these experiments the spray chamber was at ambient temperatures. The Arc+ response and In+:ArC+ ratio are shown in Fig. 6 ( a ) and (b) respectively and as was expected a larger response and correspondingly poorer In+:ArCl+ ratio was found when methane was added to the nebulizer gas. The difference was most apparent at 0.8 1 min-' where methane addition resulted in an Arc+ response of over 5 x lo5 acps compared with a response of less than 400 acps without methane addition.EiTect of power variation Fig. 7(a) and (b) shows the effect of power on the Co+ response and the In+:Co+ ratio respectively. The flat curve obtained without the addition of methane is atypical; previous power univariate searches have yielded plots which mirror that obtained with methane addition. In this instance the addition of methane reduced the response and increased the In+:Co+ ratio at lower powers and the reverse of this at higher powers. These data were reflected in those found for the other analytes. The changes in UO+ response and UO+:U+ ratio are shown in Fig. $(a) and (b) and demonstrate that the addition of methane reduced the level of oxide formation at all powers to the best value of 1.5% UO+ at 1700- 1800 W with methane addition nebulizer gas.Similar data were found with CeO+. 1.50 1.35 1.20 + u 'c 1.05 - to the 0.90 t d A 0 .75 I I I 1100 1300 1500 1700 PowerMl Fig. 7 Effect of forward power on (a) Co+ response and (6) In+:Co+ ratio with A no methane added to the nebulizer gas and B 1 .Oo/o methane added to the nebulizer gas at a nebulizer gas flow rate of 0.9 I min-IJOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY DECEMBER 1992 VOL. 7 1161 100000 10000 1000 100 6000 4800 v) m 1. m 3600 $2400 1200 . ' ' 0' I I l-O t I L I 1 1100 1300 1500 1700 01 PowerNV Fig. 8 Effect of forward power on (a) UO+ response and (6) UO+:U+ ratio x 100 (percentage oxide formation) with A no methane added to the nebulizer gas and B I .O% methane added to the nebulizer gas at a nebulizer gas flow rate of 0.9 1 min-' 1 000 000 1 ( a ) 101 I 1 I J 100 10 1 0.1 ' I 1 1100 1300 1500 1700 PowerNV Fig.9 Effect of forward power on (a) ArCI+ response and (b) In+:ArCI+ ratio with A no methane added to the nebulizer gas flow and B 1.0% methane added to the nebulizer gas flow at a nebulizer gas flow rate of 0.9 1 min-l The effect of power on the ArCl+ response and the In+:ArCl+ ratio is demonstrated in Fig. 9 (a) and (b) respectively and again shows the dramatic influence on ArCl+ formation. The addition of methane reduces the ArCl+ response by 10-to 100-fold and improves the In+:ArCl+ ratio by a similar factor when compared with all the Ar conditions. The random background and C10+ behaved similarly to ArCl+ though the level of interference removal was much lower. Fig. 1 O(a) and (b) shows the effect of power on the ArO+ response and the In+:ArO+ ratio respectively.These data show a clear improvement in the removal of ArO+ when methane was added to the plasma which was not apparent in the nebulizer gas experiments. The rather flat plots for both of the plasma types seem to indicate that power is not an important instrumental parameter in the formation of ArO+ although this is not supported by data on other polyatomic interferences or indeed from the ArO+ simplex optimization reported below where power was a critical parameter. The data obtained for Arc+ were similar to those for ArO+ although the methane addition data yielded the larger responses and poorer ratios. Eflect of methane variation Fig. 1 l(a) (b) and (c) shows the responses and ratios of Co+ UO+ and ArCl+ respectively.The Co+ response was found to fall and rise with initial methane addition then fall gradually to the 1.5% maximum while the In+:Co+ ratio increased then levelled out. The other analytes behaved similarly to Co+. The UO+ response and UO+:U+ ratio were both found to fall with increasing methane additions and this further demonstrates the scavenging of oxygen by free radicals formed from the methane. This fall in response and increase in ratio was also found with the ArC1+ and other interfering species with the exception of Arc+ which yielded the opposite results. 30 ( a ) 25 g 20 0 n > m 0 2 15 ; ~ j i a 5 0 ' I I 10 8 6 t! 3 = 4 2 0 6) B 1100 1300 1500 1700 PowerMl Fig. 10 Effect of forward power on (a) ArO+ response and ( 6 ) In+:ArO+ ratio with A no methane added to the nebulizer gas flow and B 1 .O% methane added to the nebdizer gas at a nebulizer gas flow rate of 0.9 1 min-'1162 JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY DECEMBER 1992 VOL.7 I '0 0 0.2 0.4 0.6 0.8 1.0 1.2 1.4 ~ 6 12 - 5 1' ~~ 0 0.30 0.60 0.90 1.20 1.50- 30 24 18 12 6 0 350 I 1 t 150 c - E - 120 O C W N c c - 90 E- f? .s -60 2 5 A 2 -30 8 112 a4 56 28 0 I '0 0 0.30 0.60 0.90 1.20 1.50 Methane (%) Fig. 11 Effect of percentage methane in the nebulizer gas on (a) Co+ (b) UO+ and (c) ArCI+ A response; B In+:Co+ UO+:U+ x 100 (percentage oxide formation) and In+:ArCl+ re- spectively for (a) (b) and (c) at a nebulizer gas flow rate of 0.9 1 min-I and a forward power of 1600 W Simplex Optimization of the Plasma With Methane Added to the Nebulizer Gas for the Removal of ArCI+ Simplex procedures are as previously reportedt6 with any exceptions noted.The optimum conditions for the removal of ArCl+ with the addition of methane to the nebulizer gas are listed in column one of Table 2. It was noted that these conditions are similar to those obtained with the addition of nitrogen to the nebulizer gas with similarly high nebulizer flow rates and low power.16 The plasma under these conditions was seen to be dim and have a diffuse central channel though not as diffuse as had been seen with the nitrogen addition to the nebulizer gas.16 Univariate searches confirmed the optimal conditions to be as defined. Under these conditions the ArC1+ response was seen to fall from a typical level of 50000 acps to 10-20 acps with the aspiration of a 1% chloride solution These levels effectively represented the random background signal.Detection limits are reported in Table 3 and show that the detection limit for As was effectively the same in the presence of 0 and 3.3% m/v chloride. The background equivalents at these two chloride levels was 0.8 ng ml-I further emphasizing the complete removal of ArCl+ that had been achieved under these conditions. The data for Se showed an improvement over data obtained for nitrogen addition to the nebulizer gas,I6 particularly for the 78Se 0 10 1~10' iX1o' lX1o4 ~ o j Chloride concentration/ pg ml-' Fig. 12 (a) Apparent As concentration for a 10 ng ml-I As solu- tion; (b) apparent 77Se concentration for a 100 ng ml-I Se solution; (c) apparent 78Se concentration for a 100 ng ml-1 Se solution; and (d) apparent %e concentration for a 100 ng m1-I Se solution with increasing levels of chloride under three sets of instrumental conditions A simplex optimized conditions for the removal of ArCl+ with the addition of methane to the nebulizer gas; B simplex optimized conditions for ArCI+ removal for an all argon plasma1'$ and C typical operating conditions (see Table 2) isotope with background equivalent concentrations of the order of 2-4 ng ml-I.Recoveries were determined by the analysis of standard solutions ( 10 ng ml-I for As and V and 100 ng ml-1 for Se) that had been spiked with chloride. Fig. 12(a-4 shows the apparent concentrations of As and Se plotted against chloride concentration for three sets of operating conditions methane addition to the nebulizer gas under optimum conditions all Ar optimum conditions16 and typical operating conditions (cited in Table 1) A B and C respectively.These plots particularly those for Se show the value of methane addition for the removal of the Arc]+ interference the other conditions resulting in a large positive error and imprecise data.JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY DECEMBER 1992 VOL. 7 1163 Table 2 Simplex optimized conditions for the removal of various polyatomic interferences with the addition of methane to the nebulizer gas Simplex For For For For Outer gas/] min-l 15 14 13.75 17.5 Intermediate gad1 min-' 1.4 1 .o 1.15 1 .o Nebulizer gad1 min-l 1 .o 1.05 1 .o 0.81 Methane (O/O v/v) 1 .o 1 .o 0.45 1 .o Power/W 1250 1200 1300 1320 Parameter ArCI+ removal ArO+ removal CIO+ removal CeO+ removal Results for the analysis of the CRMs are reported in Table 4 and further show the value of these conditions for the determination of As and Se.Once again they represent a particularly good improvement for the Se determinations yielding data that are close to the certified values and that are more precise. The results obtained when using the typical conditions were poorer than when using the meth- ane addition with large positive errors meaning that the certificate values were not achieved and that the precision was poorer. The results for the sea-water with use of methane addition while not matching the certificate values are a considerable improvement over the results obtained with use of the typical conditions.Simplex Optimization of the Plasma With Methane Added to the Nebulizer Gas for the Removal of ArO+ This simplex optimization involved use of the Co:ArO+ ratio as the criterion of merit and a solution containing 100 ng ml-' Co was analysed to obtain this. The optimum conditions found by the simplex optimization are listed in Table 3 Detection limits (ng m1-I) for As and Se at increasing chloride levels determined under the simplex optimized conditions for addition of methane to the nebulizer gas for ArCI+ removal Element Chloride level/pg ml-I As 17Se lase 82Se 0 0.60 6.8 4.2 18.9 100 0.63 7.2 6.0 23.5 1000 0.72 6.2 4.2 23.9 10 000 1.29 8.5 4.7 18.9 33 000 0.75 14.0 6.9 15.2 column two of Table 2 and once again characteristically low power and high nebulizer gas flow rates are displayed.The univariate searches once again confirmed the optimum conditions to be as defined. The response for ArO+ fell from approximately 10 000 acps to approximately 1000 acps while the Co+ response fell from approximately 60 000 acps to approximately 20 000 acps. The optimum conditions were ascertained by determin- ing the detection limits for Fe and these are reported in Table 5. Also shown in Table 5 are detection limits for Fe for these optimum conditions but with no added methane and for typical conditions (Table 1). The detection limit for 56Fe was less than 0.5 ng ml-I and the background c 200 120 ; Iz 0 10 iX1o3 iX1o4 1x10~ 3 Chloride concentration/l.Lg ml-' Fig.13 Apparent vanadium concentration for a 10 ng ml-' V solution with increasing chloride levels under three sets of instrumental conditions A simplex optimized conditions for the removal of C10+ with the addition of methane to the nebulizer gas; B simplex optimized conditions for C10+ removal for an all argon plasma16 and C typical operating conditions (see Table 2) Table 4 Arsenic and selenium concentrations in a range of CRMs under (a) the simplex optimized conditions for methane addition to the nebulizer gas for Arc]+ removal and (b) for typical operating parameters; n=5 and all values are k I SD Levels foundlpg g-'* Sample Arsenic- Oyster Tissue (NIST 1566) Lobster pancreas (TORT- 1) Sargasso (NIES 9) Seawater (NASS 2) Urine (Seronorm) Oyster Tissue Lobster Hepatopancreas Selenium- 12.4 k 0.5 1 1 0 f 6 20.1 f 0.6 0.26 f 0.0 1 0.05 k 0.0 1 2.43 f 0.18 6.55 k 0.32 -$ 596 f 48 40.2 * 16.5 2.74 f 0.1 1 7.6k 1.3 34.3 f 3.5 50a 18 Certified value 13.4f 1.9 24.6 f 2.2 1 1 5 a 9 0.00165 0.29 2.1 k0.5 6.88 a 0.47 * Seawater and urine values in pg ml-I.t See Table 2. -$ Value lower than the blank. 9 Range is 0.176-0.208.1164 JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY DECEMBER 1992 VOL. 7 ~~ ~ Table 5 Detection limits (ng ml-I) for Fe with use of three sets of instrumental operating parameters Isotope Instrument setting 54Fe 56Fe 57Fe (i) Simplex optimized conditions for methane (ii) As (i) but without methane addition 63.0 4.44 12.6 (iii) Typical conditions (see Table 1) 380 7.26 48.0 addition to the nebulizer gas for ArO+ removal 4.98 0.48 5.97 Table 6 Iron concentration in a range of CRMs under (a) the simplex optimized conditions for methane addition to the nebulizer gas for ArO+ removal and (b) for typical operating parameters; n=5 and all values are f 1 SD Levels found/pg g-I Sample Lobster Hepatopancreas (TORT-1) Sargasso (NIES 9) * See Table 1 .t Value lower than the blank. (a) (b)* Certified value 117&8.5 89 k 14.8 186k 1 1 1405~2.3 -t 187+6 Table 7 Detection lmits for V at increasing chloride levels determined under the simplex optimized conditions for addition of methane to the nebulizer gas for ClO+ removal Chloride level/ Detection limit/ mg ml-l ng ml-I 0 100 1000 10 000 33 000 0.5 1 1.68 0.96 1.86 2.52 equivalent concentration was 3.5 ng ml-l. The removal of the methane from the otherwise optimum conditions led to a 10-fold reduction in the detection limit and a 7-fold increase in the background equivalent concentration to 24 ng ml-l.The detection limit for the typical condi- tions where the water-bath was at 18 "C was surprisingly good but the background equivalent concentration was high at 63 ng ml-l and this seriously affected the analytical capabilities under these conditions. Attempts to determine Fe in CRMs were less successful. Results for the Lobster Hepatopancreas and Sargasso are reported in Table 6 and it was found that while the data were better with added methane than without they still failed to match the certificate values. Simplex Optimization of the Plasma With Methane Added to the Nebulizer Gas for the Removal of C10+ This simplex optimization involved use of the Co:ClO+ ratio as the criterion of merit and a solution of 100 ng ml-1 Co and 10 000 pg ml-I chloride was analysed to obtain this.The optimum conditions found by the simplex optimiza- tion are listed in column three of Table 2 and once again characteristically low power and high nebulizer gas flow rate are displayed. The optimum methane percentage which was lower than that found previously was attributed to the fact that the 52ArC+ peak interfered with the peak at mlz 5 1 at higher methane levels. Univariate searches confirmed the optimum conditions to be as defined. The analytical capabilities under these conditions were tested as with the ArCI+ conditions but with analysis of just two of the CRMs (Lobster Hepatopancreas and Sargasso) under both the optimum and typical conditions.Detection limits for V are reported in Table 7 and these were found to be generally better than those determined with use of the optimum conditions for addition of nitrogen ~ to the nebulizer gas.I6 Similarly the optimum conditions were found to improve greatly recoveries of V over all Ar optimized and typical conditions as shown in Fig. 13. Table 8 shows the results for the analysis of the Lobster Hepatopancreas and Sargasso for V. Good agreement with the certificate values was obtained only when methane was added. Simplex Optimization of the Plasma With Methane Added to the Nebulizer Gas for the Removal of CeO+ This final simplex optimization involved the use of the Ce to CeO+ ratio as the criterion of merit and a solution of 100 rig ml-l of Ce was analysed to obtain this.The optimum conditions found by the simplex optimization are listed in column four of Table 2. The ratio of Ce to its oxide was improved from typically 20 with no methane to 180 under the optimum conditions equivalent to about 0.6% oxide formation. Univariate searches were found to confirm the optimum conditions to be as defined. The analytical utility of these conditions was tested by determining the detection limits and recoveries for Eu Sm and Gd in the presence of increasing concentrations of Ba Ce and La (0 1 10 and 100 pg ml-I) which form strong oxides. The recoveries were determined under the optimum conditions and under typical conditions (see Table 2).Detection limits are reported in Table 9 and still clearly show the oxide interferences which become more severe at higher levels of Ba Ce and La. Data for the recoveries when plotted showed the two sets of conditions to yield effectively the same results and this indicated that the optimum conditions offered little or no advantage over normal conditions. One exception to this is lS8Gd which is subject to interference from I4*Cel6O. The optimum condi- tions are shown in Fig. 14 to be more effective at removing this interference. Conclusions This work has shown that interfering species such as ArCl+ ArO+ C10+ and CeO+ can be greatly reduced and in the example of ArC1+ effectively removed by the addition of methane to the injector gas. Simplex optimization of the operating parameters has been demonstrated to be an efficient way to identify rapidly the best conditions for interference removal.The success of this work has been shown by the analysis of CRMs by the improved detection limits and by the enhanced recoveries obtained.JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY DECEMBER 1992 VOL. 7 1165 Table 8 Vanadium concentration in a range of CRMs with use of (a) the simplex optimized conditions for methane addition to the nebulizer gas for C10+ removal and (b) typical operating parameters; n = 5 and all values are k 1 SD Levels found*/pg g-I Sample (a) (b) Certified value Lobster Hepatopancreas (TORT- 1) 1.26 k 0.04 2.54 k 0.22 1.4 t- 0.3 Sargasso (NIES 9) 1.37 k 0.04 9.9 1 ? 1.07 1.OkO.1 * See Table 1. Table 9 Detection limits for Eu Sm and Gd with increasing levels of Ba Ce and La under the simplex optimized conditions for addition of methane to the nebulizer gas for CeO+ removal Detection limit/ng ml-I Ba Ce and La level/ pg ml-1 lslEu Is3Eu ls2Sm ls4Sm lssGd lS6Gd Is8Gd 0 0.2 1 0.18 0.45 0.45 0.66 0.54 1.32 1 0.24 0.15 0.15 0.30 2.13 1.14 1.08 10 0.30 0.78 0.57 4.23 17.5 13.9 2.43 100 3.27 6.18 6.78 50.5 173 151 13.4 Comparison with work performed with the addition of nitrogen to all three gas flows of the ICP16 is only possible for the chloride interferences.Detection limits for As Se and V are generally better with the addition of methane to the nebulizer than with the addition of nitrogen to any of the gas flows. This is particularly apparent for the proble- matic element Se.The choice of whether to use methane or nitrogen addition would be determined by a number of factors. Nitrogen will be generally preferable as it is an inert gas; use of methane requires the adoption of safety requirements for a flammable gas e.g. flash-back arrestor and safe venting of unburnt methane. Methane appears to show particular advantage for some elements e.g. Se in authentic samples. This work has demonstrated the analytical potential of the methane-doped Ar plasma for practical interference re- moval in ICP-MS. 1 10 100 Ce concentration/pg rnl-' Fig. 14 Apparent Gd concentration for a 10 ng mi-' Gd solution with increasing cerium levels under A simplex optimal conditions for the removal of CeO+ with the addition of methane to the nebulizer gas and B typical operating conditions (see Table 2) and for a 100 ng ml-' Gd solution with increasing cerium levels under C simplex optimized conditions for the removal of CeO+ with the addition of methane to the nebulizer gas and D typical operating conditions (see Table 2) The authors gratefully acknowledge the financial support through the co-operative award in science and engineering (CASE) scheme of the Science and Engineering Research Council and VG Elemental to M.J.F.which has made this work possible. 1 2 3 4 5 6 7 8 9 10 1 1 12 13 14 15 16 17 18 References Tan S. H. and Horlick G. Appl Spectrosc. 1986 40 445. Vaughan M. A. and Horlick G. Appl. Spectrosc. 1986 40 434. Munro S. Ebdon L. and McWeeny D. J. J. Anal. At. Spectrom. 1986 1 21 I . Gray A. L. Spectrochim. Acta Part B 1986 41 15 1. Gray A. L. and Williams J. G. J. Anal. At. Spectrom. 1987 2 599. Hutton R. C. and Eaton A. N. J. Anal. At. Spectrom. 1987 2 595. Branch S. Corns W. T. Ebdon L. Hill S. J. andO'Neil1 P. J. Anal. At. Spectrom. 1991 6 155. Whittaker P. G. Lind T. Williams J. G. and Gray A. L. Analyst 1989 114 675. Gray A. L. Analyst 1985 110 551. Bradshaw N. Hall E. F. H. and Sanderson N. E. J. Anal. At. Spectrom. 1989 4 80 1.27. Evans E. H. and Ebdon L. J. Anal. At. Spectrom. 1989 4 299. Evans E. H. and Ebdon L. J. Anal. At. Spectrorn. 1990 5 425. Lam J. W. H. and Horlick G. Spectrochim. Acta Part B 1990,45 13 13. Lam J. W. H. and McLaren J. W. J. Anal. At. Spectrom. 1990 5 4 19. Beauchemin D. and Craig J. M. Spectrochim. Acta Part B 199 1 46 603. Hill S. J. Ford M. J. and Ebdon L. J. Anal. At. Spectrum. 1992 7 719. Smith F. G. Wiederin D. R. and Houk R. S. Anal. Chein. 199 1,63 1458. Allain P. Jaunault L. Mauras Y. Mermet J. M. and Delaporte T. Anal. Chem. 1991 63 1497. Paper 2/02182J Received April 28 1992 Accepted July 27 1992

ISSN:0267-9477    

DOI:10.1039/JA9920701157

出版商:RSC    

年代:1992

数据来源: RSC

摘要:

JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY DECEMBER 1992 VOL. 7 1167 Anion Exchange for the Elimination of Spectral Interferences Caused by Chlorine and Sulfur in Inductively Coupled Plasma Mass Spectrometry Jan Goossens and Richard Dams Laboratory of Analytical Chemistry Institute for Nuclear Sciences University of Gent Proeftuinstraat 86 8-9000 Gent Belgium An easily applicable separation method has been developed for the accurate and simultaneous determination of V Cr Cu Zn As and Se in biological clinical and environmental samples by inductively coupled plasma mass spectrometry. Chlorine and sulfur which cause spectral interference with these elements are retained as anions on an anion-exchange resin column (Dowex-1) whereas the analytes are eluted with dilute nitric acid and collected in the eluate.In most of the examples the sample preparation is limited to a reduction with SnCI,. This new approach to the elimination of spectral interferences has been applied to soils percolate water sewage and human serum. The results are in good agreement with certified values and results obtained by d.c. plasma atomic emission spectrometry and electrothermal vaporization atomic absorption spectrometry; differences between mean values are 4%. Keywords Inductively coupled plasma mass spectrometry; spectral interference; anion exchange; determina- tion of vanadium chromium copper zinc arsenic and selenium Inductively coupled plasma mass spectrometry (ICP-MS) is a relatively new technique combining high-speed analysis multi-element capabilities and high sensitivity.However owing to the limited resolution of the quadrupole mass analyser spectral overlap occurs when ion masses differ by less than 0.5 u. In biological and environmental samples many of these interferences are caused by the matrix elements C1 and S.lJ These elements give rise to polyatomic species leading to spectral overlap with analytes of physio- logical and toxicological importance (V Cr Cu Zn As and Se). A survey of these interferences is presented in Tables 1 and 2. Several solutions to this problem have already been suggested. 'Simulated blank solution^',^ containing equal concentrations of interfering matrix elements as the sample solutions can be prepared and the apparent analyte concentrations determined. However since the formation Table 1 Interferences due to sulfur Species subject to interference Interfering polyatomic Element Isotope species Chromium 50Cr(4.35%) 34S160 Zinc 64Zn(48.90/o) 3 2 s 1 6 0 I 6 0 66Zn(27.80/o) 34S160160 67Zn(4.1 O/o) Copper 65Cu( 30.9%) 32Sl60160lH 34S160160 I H 68Zn( 18.6%) 34S160180 Table 2 Interferences due to chlorine Species subject to interference Interfering polyatomic Element I sot ope species Vanadium 51 V( 99.7%) 3 5 ~ 1 1 6 0 Chromium Wr(8 3.8%) 3 5 ~ 1 1 6 0 1 ~ 53Cr( 9.5%) 3 7 ~ 1 1 6 0 Iron 54Fe(5.80h) 3 7 ~ 1 1 6 0 1 ~ 67Zn(4. 1 Oh) 35C1160160 Zinc Arsenic 7 5 A ~ ( 1 OOOh) 40Ar35C1 Selenium 77Se( 7.5%) *OAr3'CI of polyatomic species strongly depends on matrix condi- tions this procedure requires a complete knowledge of the sample matrix composition to allow the addition of the correct amounts of all matrix elements to the blank solution. An interesting alternative is the retention of the analyte elements on cation-exchange resin columns while interfer- ing matrix ions are el~ted.~9~ A serious drawback of this method is the fact that all analyte elements have to be present as cations which implies decomposition of organo- metallic complexes and the loss of some interesting anions (e.g.As033- and Se03z-). Ion chromatographyY6 gel filtra- tion,' electrothermal vaporization* and hydride generation9 have also been successfully applied. The use of mathematical correctionslO*ll could be useful but often these corrections suffer from uncertain assump- tions systematic errors and error amplification leading to inaccurate and imprecise results.The use of alternative plasma gases (e.g. He)12 in order to shift some of the interfering species to other mass regions seems very promising while the addition of Nz to the Ar plasma gasL3J4 in order to alleviate the formation of some polyatomic species is being investigated. In the present paper a new approach is presented whereby C1 and S anions are removed from the sample solution by retention on a Dowex-1 resin column in the NO3- form.15J6 Dowex-1 is a strongly basic anion-exchange resin with a quaternary ammonium functionality; C1- C104- S042- S032- and some other anions are retained on the resin while analyte elements including trace metals subject to interference (V Cr Cu Zn As and Se) are eluted. The main advantage of this procedure is that both anionic and cationic analytes can be simultaneously sepa- rated from C1 and S. Moreover there is no need for the analyte elements to be present in free cationic form.The only anions that cannot be held at all by the resin are complex anions or organic anions which because of their size and configuration cannot enter the interior of the resin particles. Experimental Instrumentation A VG PlasmaQuad (VG Elemental Winsford UK) was used for the ICP-MS measurements; details of the instru- ment and operating conditions are summarized in Table 3.1168 JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY DECEMBER 1992 VOL. 7 Table 3 PlasmaQuad operating conditions Plasma- R.f. power Forward/W Reflected/W Plasma/I min-l Nebulizer/l min-' Auxiliary/l rnin-l Gas flows Nebulizer Spray chamber Ion sampling- Sampling cone Skimmer cone Vacuum- 1350 ( 5 13.5 0.725 0.9 1 Meinhard concentric type Scott-type double bypass pumped at 0.9 ml min-'* water cooled Nickel 1.0 mm orifice Nickel 0.75 mm orifice Expansion stage/mbart 2.3 Intermediate stage/mbar 2.0 x 1 0 - 4 Analyser stage/mbar 4.6 x 1 0 - 4 * Increased up to 7 ml mind' for qualitative on line experiments.t 1 bar=105 Pa. The ion lens settings were optimized for the internal standard (74Ge or '%I). The measurements were performed in the mass scanning data-acquisition mode limited mass regions (Am) were scanned entirely. The number of chan- nels n was always chosen so that nlAm was a minimum of 20 and thus accurate integration of the signal peaks was possible.The dwell time per channel was 160 ,us. A standard number of 200 sweeps per measurement was applied. For some qualitative experiments data were collected by setting the quadrupole at a fixed mlz value with use of the multichannel analyser for time-resolved analysis at a single mass. Comparative analyses were carried out by electrothermal vaporization atomic absorption spectrometry (ETV-AAS) and d.c. plasma atomic emission spectrometry (DCP-AES). The ETV-AAS instrument used was a Perkin-Elmer (Nor- walk CT USA) Model 3030 equipped with a deuterium-arc background corrector and a Perkin-Elmer Model HGA 400 graphite furnace atomizer. The DCP instrument was purchased from Applied Research Laboratories (ARL) Ecublens Switzerland and was a DCP Spectrajet 111. Reagents and Solutions The anion-exchange resin Dowex-1 X8 (mesh size 100-200; technical grade) commercially available in C1- form (Serva Heidelberg Germany) was used.No pre-treatment or purification other than described under 'Column Prepa- ration' was carried out. Commercial standard solutions of 1 g 1-l [Fluka (Buchs Switzerland) Janssen Chimica (Beerse Belgium) Merck (Darmstadt Germany)] were used to prepare the synthetic samples. For calibration purposes use was made of com- mercial standard solutions (1 g 1-I) for V Cr and As (Fluka) whereas pure metals (>99.95%) were used to prepare standard solutions of Cu Zn and Se by dissolving the metal in concentrated nitric acid followed by appropri- ate dilution. All acids used were purified by sub-boiling distillation except for perchloric acid (Merck Suprapur) and hydrofluoric acid (J.T. Baker Instra-Analyzed; Philips- burg NJ USA; Suprapur). Millipore (Milford MA USA) Milli-Q water was used throughout. A Sn*I solution was prepared by dissolving approximately 15 g of SnCl2-2H20 (pro analysi) in 5 ml of boiling 10 moll-' HC1 followed by dilution to 100 ml with water. Sample Preparation A synthetic sample was prepared containing V Cr Mn Fe Co Ni Cu Zn As and Se at the 500 pg 1-l level in 0.14 rnol I-' HN03. Amounts of HCl and H2S04 equivalent to 3 g 1-l of C1 and 3 g 1-2 of S were added. Four authentic samples all containing high concentrations of C1 and/or S were analysed sewage percolate water light sandy soil and human serum. For the analysis of sewage and percolate water no further sample pre-treatment was carried out The sewage containing 1.1 g 1-l of C1- and 6.0 g 1-' of S042- was filtered and provided by LISEC (Limburgs Studiecen- trum voor Toegepaste Ecologie).The percolate water was analysed by several laboratories in the framework of a ring analysis campaign organized by VITO (Vlaams Instituut voor Technologisch Onderzoek). Further the aqua regia soluble content of a candidate BCR (Community Bureau of Reference) certified reference material (CRM 142R Light Sandy Soil) was determined. The aqua regia soluble phase of heavy metals in soils and sludges is often of more ecological importance than the total content since it can be considered as the bio-available fraction for plants and crops. Approximately 1 g of the Light Sandy Soil was heated under reflux in 10 ml of aqua regia (7.5 ml of HC1+2.5 ml of HN03) and filtered closely following the procedure described by the BCR (DIN 38 414-57).The filtrate obtained was diluted to 1000 ml with 0.14 mol 1-' HN03. Blank solutions were prepared in the same way. For the analysis of freeze-dried human serum 1 g of sample was digested with concentrated HN03 and HC104 and the digest was evaporated to near-dryness. The decom- position was necessary to convert the organically bound S into S042-. The sample was again diluted to 10 ml with 0.14 mol 1-l HN03. The freeze-dried human serum was the 'second generation' biological reference material prepared by Versieck et af.17 This material was collected and stored under rigorously controlled conditions in order to avoid contamination so that the concentrations of most trace elements were fairly similar to those expected in normal human serum.The addition of HN03 and of strong acids in general to the samples prior to elution was limited as much as possible to avoid column overload. To achieve complete separation lihe HNO concentration in the sample solutions should not exceed 0.3 rnol 1-l. Column Preparation ,4 40 ml (wet volume) portion of resin was transferred into a polyethylene tube (20 cm in length 2.7 cm i.d.) and converted into the NO3- form by rinsing the column with 1.4 mol 1-l HN03. The column was next washed with 0.0014 mol 1-l HN03 until the same pH value was measured at the inlet and outlet. A column of this size has a theoretical ion capacity of approximately 50 mequiv (1.2 mequiv ml-l wet resin) but the amount of adsorbable material in the sample should not exceed 10°/o of this value.For regeneration purposes the column was rinsed with 1.4 mol 1-1 HNO until the effluent no longer tested positive to C1- (precipitation of AgCl by addition of 0.01 mol 1-1 AgN03). The presence of HC104 could cause regeneration problems because of the high affinity of the resin for C104-. In this instance it was necessary to renew the resin partially before regeneration. For the experiments described below regeneration was carried out after each elution. Elution Procedure Depending on the analyte concentration and the amount of sample available 2.5-50 ml of the sample solution wereJOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY DECEMBER 1992 VOL.7 1169 applied to the column. After the sample drained into the resin bed a maximum volume of 120 ml of the eluent (0.0014 mol 1-I HN03) were added in small portions and elution was carried out. A constant elution rate of 10 ml min-l was obtained by using a peristaltic pump [Ismatec MS-4/8 (Zurich Switzerland)]. A single separation required about 15 min. Preliminary Studies Choice of a Suitable Reductant Owing to the relatively high acid strength of H3V04 H3As0 and H,SeO partial retention can occur for V As and Se if these elements are present in high oxidation states. Therefore when at least one of these elements has to be determined a suitable reductant has to be added to the sample for the reduction of Vv AsV and Sevl to VIV As111 and SeIV respectively.A theoretical approach to this problem is presented in Fig. 1. For a given pH the redox potential of the reductant should be situated in the region between lines 3 and 4. The upper limit is the maximum redox potential for quantitative (> 99%) reduction of the three elements mentioned above while a minimum value is imposed by the possible reduction of Asill to Aso. Taking this into consideration SnC12 and CuCl are suitable reductants; this was confirmed experimentally. Tin(I1) chloride was pre- ferred because of its greater stability and solubility and because of the fact that Cu may be an analyte of interest itself A standard volume of 100 pl of Sn1I solution was added to the samples unless mentioned otherwise. It is important to note that unreduced organometallic com- 1.2 1 0.8 .m 0.6 0.4 5.U C P 5 0.2 d o -0 -0.2 -0.4 0 1 2 3 4 5 6 7 PH Fig. 1 Maximum redox potential for quantitative reduction of SeV1 (line I) Vv (line 2) and AsV (line 3) to SeIV VvIv and As111 respectively. Minimum redox potential for quantitative oxidation of Aso ( 1 mg I-') to As111 (line 4). The redox potential of the reductant chosen should be situated in the region between lines 3 and 4 plexes (e.g. arsenobetaine) are not retained by the resin. A trace amount of HF (1 00 p1 of a 5% solution) was always added to the eluate to prevent the precipitation of Sn(OH)2. Effect of the Eluent Concentration on Retention and Recover- ies As already mentioned dilute HNO was used as the eluent for the separations. The concentration of the HN03 (0.00 14 moll-]) is a compromise suppression of the dissociation of acid analytes (e.g.H,As03) requires a higher concentration whereas a lower concentration is favourable in view of the competition between NO3- and all other adsorbable species for the active sites on the resin. The elution diagrams of Cr3+ and H3As03 are shown in Fig 2. It was found that all positively charged analytes (V3+ VOz+ Cr3+ MnZ+ Fe3+ Co2+ Ni2+ Cu2+ and Zn2+) show very similar elution characteristics. Arsenic however is slightly retarded and peak broadening can be observed. For a high elution yield a sufficient volume of eluate must be collected. Selenious acid (H2Se03) was eluted quantitatively with an eluent concentration of a0.014 mol I-* HNO only. Eluent concentrations in excess of 0.05 moll-' HN03 were however found to yield incomplete retention of C1-.The latter ion was chosen as an indicator for possible 'bleed off since it has the lowest selectivity coefficient of all the retained anions of interest (Table 4).18 This coefficient is the degree of preference of an anion-exchange resin for a certain anionic species relative to another (conventionally Cl-). It shows no rigid correlation with a simple chemical or physical property of the anions. However a certain propor- tionality to the acid strength is observed. The elution parameters applied for the analysis of all authentic samples are listed in Table 5. Amount of the Eluent and Elution Rate For complete elution of cationic species (V3+ Cr3+ etc.) H3As03 and H2Se03 a minimum eluent volume of 60 80 Table 4 Selectivity coefficients for anions on Dowex-1 resinI8 Hydroxide Fluoride Acetate Dihydrogen phosphate Hydrogen carbonate Chloride Hydrogen sulfite Nitrate Hydrogen sulfate Perchlorate 0.09 0.09 0.17 0.25 0.32 I .oo 1.3 3.8 4.1 (32)* * Selectivity coefficient measured for Dowex-2 and not for Dowex- 1 however both resins are similar and the selectivity coefficients are comparable for other anions.I ' 2 Table 5 Elution parameters 0 200 400 600 800 1000 1200 1400 Time/s Resin Type Dowex- I X8 (mesh size 100-200) Counter ion NO3- Wet volume 40 ml Eluent Concentration 0.0014 rnol I-' HN03* Volume 100- 120 ml Elution rate 10 ml min-' Samples Volume less than 50 ml; maximum equivalents of adsorbable materials 10% of the theoretical column capacity; maximum HN03 concentration for com- plete separations 0.3 rnol I-' Fig.2 Elution diagrams of I Cr3+ and 2 H3As03 * 0.014 mol-I HN03 if quantitative elution of Se is required.1170 JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY DECEMBER 1992 VOL. 7 Table 6 Analysis of a synthetic sample Recovery (O/o) after elution with 0.0014 rnol I-' HN03 on a NO3- Element (mlz value monitored) loaded column Vanadium (5 1) Chromium (53) Manganese (55) Iron (57) Cobalt (5 9) Nickel (60) Copper (65) Zinc (66) Arsenic (75) Selenium (77) Chlorine (35) Sulfur (48) 102.0 f 0.3* 103.0 ? 2.4 100.0 * 2.4 102.4+- 1.6 98.5 * 2.2 100.1 k 0.3 100.0 * 1.6 99.0 k 0.8 99.0 k 2.6 98.7k 1.1$ (0.1 t o . I * Uncertainties are expressed as standard errors of the mean. t Corrected for Arc interference.$ 0.014 rnol I-' HN03 used as eluent. Recovery (O/O) after elution with 0.014 rnol I-' HN03 on an acetate loaded column t 60 98.2 f 0. It 100.2 f 1 .o 102.3 f 1.8 99.1 f 2.4 100.3 f 0 . 6 99.9 -+ 1.7 102.1 k 1.6 98.2 * 1.9 < 30 t o . 1 t o . 1 Table 7 Determination of Cr and V in sewage Determined valuelpg 1-1 Element ICP-MS DCP-AES ETV-AAS Chromium 1 14.0 f 3.4* 115.7k2.7 112.2k3.4 Vanadium 62.5 -+ 2.6 64.3f 1.8 60.7 k 4.1 * Uncertainties are expressed as standard errors of the mean. Table 8 Determination of Cr in aqua regia soluble phase of Light Sandy Soil Determined valuelpg g-I Sample ICP-MS DCP-AES ETV-AAS I 84.6 83.7 87.9 2 87.2 85.2 87.7 3 81.0 85.0 83.3 4 85.1 88.0 87.0 5 80.0 84.7 79.1 Mean 83.6k 1.3* 85.32 k 0.72 85.0 & I .7 * Uncertainties are expressed as standard errors of the mean.and 100 ml respectively is required. Further research on the possibilities of on-line connection of the resin columns to the ICP-MS system to limit sample dilution is being undertaken. Elution rates of 10 ml min-I were used for off-line separations whereas for the qualitative on-line experiments the rate was decreased to 7 ml min-I. Analysis of Synthetic Samples After reduction 10 ml of a synthetic sample were applied and elution was effected with 120 ml of 0.0014 mol 1-1 HN03. The eluate was collected and Ge was added as an internal standard. Further dilution to 150 ml was accomplished with 0.14 mol 1-I HN03. Recoveries of all metals and anions added were measured by ICP-MS. This procedure was repeated twice and average recoveries and standard deviations were calculated.All recoveries except for Se were near 100%. Elution with 0,014 mol 1-' HN03 yielded quantitative recoveries for all the elements includ- ing Se. In both instances the concentrations of C1- and Sod2- in the eluate were below ICP-MS detection limits (0.1 and 0.3 mg I-' for C1 and S respectively). Chlorine was monitored at mlz=35 for S the SO signal at mlz=48 was used. Analytical blanks for the procedure were below the ICP-MS detection limit for all elements. In an additional experiment the column was loaded with acetate anions by means of a 2 moll-' NH,Ac solution and 0.014 mol 1 - I HN03 was used as the eluent. The main advantages of this modification are that the HN03 concen- tration of the samples and the eluent is less critical and that complete retention of phosphates is possible.Both of these advantages are owing to the low selectivity coefficient of acetate for Dowex- 1. The most serious drawback is the low recovery of Se and V (the latter owing to reduction problems) and the possible Arc interference on Cr. The latter procedure can however be used to separate Cu Zn other cationic species and As from C1 S and P in samples with HN03 or other strong acids in too high concentrations for the columns loaded with NO3-. The capabilities of this modification were tested by elution and analysis of syn- thetic samples only. Instead of 0.0014 mol 1-' HN03 (see above) 0.014 mol 1-' HN03 was used as the eluent. The results of the analysis of the synthetic samples for both procedures are listed in Table 6.Results and Discussion Analysis of Sewage After reduction 20 ml of sewage were treated as described above. Germanium was added as an internal standard to the eluate in which Cr and V were determined. As can be seen from Table 7 the results for Cr and V are in good agreement with independent analyses by other techniques (DCP-AES and ETV-AAS). Originally the interference by Cl on 51V T r and 53Cr was 250 30 and 350% of the net signals respectively. Analysis of Percolate Water Percolate water (25 nil) was treated after reduction. Three replicates were prepared and Ge was added as an internal standard to the eluates. Arsenic was determined and a mean value of 49.9 -t- 2.8 ,ug 1-L was obtained which is in excellent agreement with the accepted value (50.0 pg 1-I).Before separation an 'apparent' As concentration of 85 ,ug 1-l was found. Analysis of Light Sandy Soil For the determination of the aqua rcgia soluble content of (3- in Light Sandy Soil five different solutions and severalJOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY DECEMBER 1992 VOL. 7 1171 Table 9 Determination of Cu and Zn in a human serum reference materialI7 Element Determined value/pg g-I Certified value/pg g-’ Copper 11.15 k0.5 I* 1 1 . 1 k0.4 Zinc 9.8 1 f 0.25 9.6 f 0.2 * Uncertainties are expressed as 95% confidence limits. blanks were treated 30 ml of each being applied to the column. After elution Ge was added to the eluates as an internal standard. Since V As and Se were of no interest no preliminary reduction was needed.Interference by Cl on 52Cr and 53Cr was about 30 and 3OO0h of the net signals respectively while after elution both isotopes yielded identical results. The determined contents for Cr are in good agreement with the results obtained by ETV-AAS and DCP-AES (Table 8). Analysis of Human Serum Copper and Zn both subject to interference from poly- atomic S species were determined in the human serum reference material. A digestion prior to elution was necessary to convert the organically bound S into S042-. After separation In was added to the eluate. Copper was determined with use of the T u isotope because 63Cu was still subject to interference from 40Ar23Na. Without separation the interference by S on the 65Cu isotope amounted to 25% of the net signal. The determina- tion of Zn in human serum is limited also since all isotopes are subject to interference from S (68Zn to a small extent only).After separation all the Zn isotopes yielded identical results. The contents determined are in good agreement with certified values for both elements and are listed in Table 9. Conclusions Spectral interference on V Cr Cu Zn As and Se caused by C1 and S in ICP-MS can be overcome by separation on a Dowex-1 column in the NO3- form. This allows the accurate determination of these elements together with other analytes in many environmental and biological samples. In most instances sample preparation can be limited to a reduction with SnC12 and analytical blanks of the procedure are below ICP-MS detection limits. Organi- cally bound C1 or S however necessitates acid digestion prior to the separation whereby the addition of mineral acids is limited as much as possible to avoid column overload.Sample volumes of up to 50 ml were used. A dilution of the sample by a factor of 3-10 is inherent to the separation method. Direct connection of the columns to the ICP-MS instrument could alleviate this drawback and will be the subject of further research. Grateful acknowledgement is made to Dr. C. Vandecasteele for his valuable scientific contribution. The authors are also grateful to Ing. R. Steegmans from LISEC (Limburgs Studiecentrum voor Toegepaste Ecologie) for providing sewage samples. References 1 Tan S. H. and Horlick G. Appl. Spectrosc. 1986 40 445. 2 Lyon T. D. B. Fell G. S. Hutton R. C. and Eaton A.N. J. Anal. At. Spectrom. 1988 3 265. 3 Vanhoe H. Vandecasteele C. Versieck J. and Dams R. Anal. Chem. 1989 61 149. 4 Plantz M. R. Fritz J. S. Smith F. G. and Houk R. S. Anal. Chem. 1989 61 149. 5 McLaren J. W. Mykytiuk A. P. Willie S. N. and Berman S. S. Anal. Chem. 1985 57 2907. 6 Sheppard B. S. Shen W.-I. Caruso J. A. Heitkemper D. T. and Fricke F. L. J. Anal. At. Spectrom. 1990 5 431. 7 Lyon T. D. B. Fell G. S. Hutton R. C. and Eaton A. N. J. Anal. At. Spectrom. 1988 3 60 1. 8 Whittaker P. G. Lind T. Williams J. G. and Gray A. L. Analyst 1989 114 675. 9 Branch S. Corns W. T. Ebdon L. Hill S. and O’Neill P. J. Anal. At. Spectrom. 1991 6 155. 10 Munro S. Ebdon L. and McWeeny D. J. J. Anal. .4t. Spectrom. 1986 1 2 1 1. 1 I Ridout P. S. Jones H. R. and Williams J. G. Analyst 1988 113 1383. 12 Montaser A. Chan S.-K. and Koppenaal D. W. .4nal. Chem. 1987 59 15 1. 13 Branch S. Ebdon L. Ford M. Foulkes M. and O’Neill P. J. Anal. At. Spectrom. 1991 6 151. 14 Evans E. H. and Ebdon L. J. Anal. At. Spectrom. 1989 4 299. I5 Faris J. P. and Buchanan R. F. Anal. Chem. I964,36 I 157. 16 Caletka R. Hausbeck R. and Krivan V. J. Radioanal. Nucl Chem. 1990. 142 383. 17 Versieck J. Vanballenberghe L. De Kesel A. Hoste J. Wallaeys B. Vandenhaute J. Baeck N. and Sunderman F. W. Anal. Chim. Acta 1988 204 63. 18 Peterson S. Ann. N. Y. Acad. Sci. 1954 57 144. Paper 2/02181A Received April 28 1992 Accepted July 7 1992

ISSN:0267-9477    

DOI:10.1039/JA9920701167

出版商:RSC    

年代:1992

数据来源: RSC