ISSN:0003-2654    

DOI:10.1039/AN99419FX022

出版商:RSC    

年代:1994

数据来源: RSC

摘要:

13811 3871391139714031413141714211427Spectrophotometric Determination of Phenols by Coupling With Diazotized 2,4,6-Trimethylaniline in aMicellar Medium. S. Esteve Romero, L. Alvarez Rodrlguez, M. C. Garcla Alvarez-Coque, G.Ramis-RarnosExtractive Spectrophotometric Determination of Dimethoate with Molybdate and Methylene Blue by aFlotation-Dissolution Method4oyce Vanisha Das, K. N. Ramachandran, V. K. GuptaEffect of Tartrate on Vanadium-catalysed Chlorpromazine-Bromate Redox Reaction and Its Application tothe Determination of Vanadium in Natural Waters-Susumu Kawakubo, Bing Liang, Masaaki lwatsuki,Tsutomu FukasawaDirect Atomization Atomic Absorption Spectrometric Determination of Be, Cr, Fe, Co, Nil Cu, Cd, and Pb inWater With Zirconium Hydroxide Coprecipitation-Toshihiro Nakamura, Hideyuki Oka, Mikita Ishii, Jun Sat0Response Surfaces for the Determination of Arsenic(iii) by Hydride Generation Atomic AbsorptionSpectrometry and Flow Injection-Peter D.Wentzell, Nils G. Sundin, Cristet HogeboomDetermination of Formaldehyde in Reagents and Beverages Using Flow Injection-Hironori Tsuchiya,Shigeru Ohtani, Kuniaki Yamada, Mioko Akagiri, Nobuhiko Takagi, Masaru Sat0Sub-stoichiometric Isotope Dilution Analysis Method for the Determination of Iodine in Common Salts UsingIodine-131 Tracer-Vivek Singh, A. N. GargProcedure for the Determination of *l*Pb in Phosphate Ore, Gypsum and Phosphoric Acid byRadiochemical Separation and Gamma-ray Spectrometry-Andr6 Lagerwaard, Joost R. W. WoittiezGarcia-Alvarez-CoqueCUMULATIVE AUTHOR INDEX77N79N85N86N87N87N~ ~~~~~~~Book ReviewsConference DiaryCoursesPapers in Future IssuesNational Analytical Competition (RSC/Science Museum)1994 Benedetti-Pichler AwardCover picture: Toxic groundwater (contaminated by metals) discharging into the River Tame, WestMidlands. Reproduced with kind permission from GREENPEACE Communications Ltd.Typeset and printed by Black Bear Press Limited,Cambridge, Englan

ISSN:0003-2654    

DOI:10.1039/AN99419BX024

出版商:RSC    

年代:1994

数据来源: RSC

摘要:

DICTIONARY OF SUBSTANCES AND THEIR EFFECTS1Dictionary of Substances and their Effects (DOSE) is anew, unique, user-friendly guide to 5,000 chemicals and theimpact they have on life forms and the environment acrossthe globe.Compiled with the aid of official lists from the EC, UK,USA and Canada, DOSE is being published in sevenalphabetical volumes, which will be completed in 1994.Each volume contains an index of chemical names, CASregistry numbers and molecular formulae, as well as aglossary of biological organisms. A separate volumecontaining cumulative indices of all volumes will bepublished after Volume 7.DOSE LISTS EACH CHEMICAL'S:IDENTIFIERS USESOCCUPATIONAL EXPOSURE ECOTOXICITYSTATUS IN LEGISLATION WORLDWIDE MAMMALIAN TOXICITYEFFECTS ON SEWAGE WORKS PROCESSES PHYSICAL PROPERTIESDOSE enables the user to make rapid hazard assessments of chemicals, facilitating riskassessment and further action.Such a store of information is of critical importance to scientists,environmentalists, industry professionals, regulators and researchers - indeed anyone affected byor concerned about chemicals and their potential effects on the environment the world over.ORDER NOW FOR LOW PRICES DOSE AND HIGH SAVINGS!ROYAL &- SOCIETYOFC H EM I STRYServicesDOSE Prices All volumes approximately 1,000 pagesVolume 1 Hardcover (A to B) ISBN 0 851 86 331 0 (1 992) Price f 180.00Price f 180.00Price f 180.00 && InformationVolume 2 Hardcover (C) ISBN 0 85186 341 8 (1993)Volume 3 Hardcover (Da to Dim) ISBN 0 85186 351 5 (1993)Volume 4 Hardcover (Din to H) ISBN 0 85186 361 2 (May 1994) Price f 180.00Volume 5 Hardcover (I to M) ISBN 0 85186 371 X (July 1994) Price f 180.00Volume 6 Hardcover (N to R) ISBN 0 851 86 330 2 (September 1994) Price f220.00 (pre-pubn.f 180.00)Volume 7 Hardcover (S to Z) ISBN 0 85186 340 X (December 1994) Price f220.00 (pre-pubn. f180.00)Complete Set ISBN 0 85186 381 7 Price f 940.00 before publication of Volume 4;f1020.00 before publication of Volume 5;f 1050.00 until the end of 1994.To order, please contact: Turpin Distribution Services Ltd., Blackhorse Road, Letchworth, Herts SG6 1 HN, United Kingdom.Tel: 4 4 (0) 462 672555 Fax: +44 (0) 462 480947RSC members should obtain members' prices and order from: Membership Administration, Royal Society of Chemistry,Thomas Graham House, Science Park, Milton Road, Cambridge CB4 4WF, United Kingdom.Tel: +44 (0) 223 420066. Fax: 4 4 (0) 223 42362

ISSN:0003-2654    

DOI:10.1039/AN99419BP028

出版商:RSC    

年代:1994

数据来源: RSC

摘要:

Euroanalysis Vlll76N Analyst, June 1994, Vol. 119 Foreword Euroanalysis VIII: Edinburgh, Scotland, September 5-11, 1993 given, 28 of which were ‘invited’. Another feature of the programme was the provision of poster sessions, which were The eighth Euroanalysis Conference was held on September 5-11, 1993, in Edinburgh. It was organized by the Analytical Division of The Royal Society of Chemistry, the Chairman of the Organizing Committee being Professor Duncan Thorbum Bums. The Scientific Programme was organized by a sub- committee chaired by Professor David Littlejohn, who had as colleagues Mr. R. I. Aylott, Professor K. D. Bartle, Professor D. T. Bums, Dr. J. Marshall, Professor J. N. Miller, Professor M. R. Smyth and Dr. A. M. Ure. The conference was attended by 749 people, of whom 649 were scientific participants.Following a pleasant opening ceremony, during which a number of awards, etc., were presented and a number of strathspeys and reels were played, the scientific programme got under way. The programme was made up of 4 or 5 parallel sessions each day, all lectures (including invited lectures) being of 20 minutes’ duration with 5 minutes for questions and discussion. In all 176 lectures were held on three afternoons in the Cmpressive McEwan Hall of the University of Edinburgh, the same venue as was used for the opening ceremony. In all, 350 posters were presented. Euroanalysis VIII was a truly international conference with scientific participants drawn from 46 countries other than the UK. A good number of these attended the closing ceremony which, like the lectures, was held in the University’s Appleton Tower. This special issue of The Analyst contains 28 papers and posters given at the conference; 25 of the invited papers will be the subject of a book to be published shortly by The Royal Society of Chemistry. The organizers of Euroanalysis VIII hope that you will find this collection of papers useful and instructive; we all look forward to Euroanalysis IX, which will be held in Bologna in 1996. R. A. Young

ISSN:0003-2654    

DOI:10.1039/AN994190075N

出版商:RSC    

年代:1994

数据来源: RSC

摘要:

77N Analyst, June 1994, Vol. 119 Book Reviews Spectrochemical Analysis by Atomic Absorption and Emission By Lauri H. J. Lajunen. Royal Society of Chemistry. 1992. Pp. xii + 242. Price f18.50. ISBN 0-85186-873-8. There have recently been a number of new books published on atomic spectroscopy, some detailed in specific areas, others giving a more general overview for the non-specialist reader. This book should fall into the second category being designed as an undergraduate text covering the basic theory and application of AAS, plasma AES, AFS and ICP-MS. In practice however it falls somewhere between the two, giving details of some topics and a general overview of others. The first of the book’s ten chapters provides a brief historical review of the development of atomic spectroscopy , discusses milestones in development and the current status of the various techniques, and gives a list of definitions for terms employed later in the book.This section, although very short, gives a useful introduction to the background of atomic spectroscopy. The second chapter discusses the theory of atomic spectro- scopy with subsections on selected topics such as spectral line widths, the Zeeman effect, the absorption coefficient and basic concepts of analytical plasmas. It is here that readers first encounter the book’s tendency to describe some topics in great detail whilst giving other topics scarce mention. however, most of the important aspects of theory are covered, although some topics, e.g., the Lambert-Beer law, are covered elsewhere in the book.Some readers may find the condensed style of presentation in this chapter difficult to follow. The third chapter covers atomic absorption spectrometry and is subsectioned into instrumentation, calibration, flame atomization, electrothermal atomization, background correc- tion and special methods. This chapter forms the back-bone to this book and fills 121 pages. The chapter gives a comprehen- sive coverage of both flame and electrothermal AAS and contains many useful figures and tables. The section on special methods describes hydride generation methods in some detail, cold vapour techniques, flow injection analysis, the use of atom retarders and a section on indirect methods (methods based on the formation of compounds in solution, and methods based on the formation of compounds in the atom cell).The final part of this chapter discussed molecular absorption spectrometry with electrothermal improvization. In comparison with Chapter 3, Chapter 4 on flame atomic emission is surprisingly short (less than a page of text and one table) and the reader is left feeling that this ‘chapter’ would have been better expanded and integrated with the following chapter on plasma emission. The plasma chapter itself (Chapter 5 ) is reasonably comprehensive although does not go into the same detail as the previous chapter on AAS. Again, however, there is the dichotomy between subjects which are covered in detail, e.g., solid sample introduction, and important subjects that are omitted totally, e.g., the spatial and temperature characteristics of plasmas.‘Although this book contains much useful Momtion the author has probably been too ambitious with regard to the scope of the material to be included in what is basically an introductory text.’ The final chapters in the book are very brief, particularly Chapter 6 on inductively coupled plasma mass spectrometry. This chapter consists of six pages, of which half are in the form of tables. The contents of this section do not warrant a chapter, indeed this chapter does neither the subject nor the book justice. Chapter 7 is on atomic fluorescence spec- trometry and although short (7 pages) serves to give an introduction to the technique. Chapter 8 however, on sample preparation, is probably outside the scope of the book, and again leaves the reader wanting more detail, e.g., on microwave digestion and the use of slurries.The last two chapters provide a comparison between the various tech- niques and some suggested further reading although both these areas would be better incorporated into earlier chapters. or as an appendix. In conclusion, although this book contains much useful information the author has probably been too ambitious with regard to the scope of the material to be included in what is basically an introductory text. Although I am sure this book will find its way onto library bookshelves, I am not convinced that lecturers will place it high on recommended reading lists for undergraduate students. S. J. Hill Department of Environmental Sciences University of Plymouth ~~ ~ Glycoprotein Analysis in Biomedicine Edited by Elizabeth F.Hounsell. Methods in Molecular Biology. Volume 14. Pp. xii + 308. Humana. 1993. Price f 49.50. ISBN 0-89603-226-4. Those of us interested in the analysis of glycoproteins have been able to draw on a range of laboratory manuals for the characterization and analysis of the protein part, but have not been so well served in dealing with the oligosaccharide portion. This manual is in the Methods in Molecular Biology series and follows the general format of a spiral bound volume which folds flat on the bench, so that the detailed recipes for the procedures described can be sampled at the bench-side. I wish more cookery books were like this. There are 22 chapters covering a very wide range of applications, headed by Dr. Hounsell herself with a chapter on general strategy that sets the scene for the first seven chapters, which are written more in terms of analytical techniques.The majority of the remainder deal with methodological aspects of specific groups of proteoglycans, including mucins, poly- sulphated glycosaminoglycans and bacterial glycoproteins. There is a certain amount of duplication, but on the whole this serves to illustrate the different approaches to adapting a particular technique, and is quite a useful feature. One problem of a multi-author volume such as this is that techniques are not necessarily set out in any logical order (the phenol sulfuric reaction for sugars is lurking at the end of a chapter dealing with enzymic cleavage of 0-glycans, for instance) but the book is well indexed, even if not perfectly so (deglycosylation is listed under trifluoromethanesulfonic acid: logical if you know about TFMS deglycosylation, but difficult if you are just looking for a method of removing the oligosaccharide).One of the functions of the introduction is to pull together the related analytical protocols dotted through- out the individual contributions. ‘Indispensable for anyone starting work on the analysis of glycoproteins’ For any printed publication there will always be some recent methods or adaptations which fail to make the cut. The latest78N Analyst, June 1994, Vol. 11 9 manifestation of reductive amination (using fluorescent dyes with reaction products analysed by polyacrylamide gel electro- phoresis) is not here, although there is a very comprehensive chapter on pyridylamination by Hase, nor is there any reference to the very latest twist in the application of glycosidase digestion to structure determination (comparison of ‘signatures’ of combined aliquots digested with selected cocktails of glycosidases of differing specificity), although there are at least four other methods of structure determina- tion described.The discussion of mass spectrometry is confined to FAB- and LSI-MS, and more recent ionization developments such as electrospray or matrix assisted laser desorption are not covered. There is, however, a chapter on scanning tunneling microscopy, rather longer on promise than examples. All of the traditional methods are here: methyla- tion analysis, exoglycosidase digestion analysed by size exclusion chromatography, and also some new ones, capillary electrophoresis for instance.The first half of the book is probably the part of most relevance to workers with a chemical background, but there are a number of interesting biological applications in the second half (the use of enzyme-linked lectins and the manufacture of ‘neoglycoproteins’ are two) Overall, I think the book fully achieves its object in providing a comprehensive scaffolding of basic methods, covering a very wide range of potential interests, and must be indispensable for anyone starting work on the analysis of glycoproteins, as well as, I should have thought, a good many experienced workers. P. H. Corran National Institute for Biological Standards and Control Hertfordshire Practical NIR Spectroscopy With Applications in Food and Beverage Analysis By B.G. Osborne, T. Fearn and P. H. Hindle. Pp. 227. Longman. 1993. Price f65.00. ISBN 0-582-09943-3. This book is a both a revision and an expansion of a first edition published originally in 1986. In this edition, Peter Hindle, an expert in the design of NIR optical systems, joins the original authors and the result is the scope of the book is broadened. After a brief outline of the development of near-infrared spectroscopy (NIR) the basic principles on which NIR is based are discussed: starting with the physical processes of molecular vibration which produce the fundamental mid-infrared absorptions from which NIR overtone and combination bands originate. There are sections dealing with the interpretation of NIR spectra and the physical processes involved in the interaction of NIR radiation with the type of samples prevalent in the food industry.Particularly useful are tables showing the position of the most common bands and their chemical assignments. This section of the book is largely unchanged from the first edition. Two chapters deal with instrumentation and differ substan- tially from the first edition. Instead of a chapter surveying instrumentation, which quickly became obsolete, there is a chapter which deals with properties of the optical geometries which are used in the current generation of instruments and a second dealing with the general principles involved in collecting data in a variety of industrial situations. ’This edition should also do well as it is g d ~ ~ e d to a high standard and is excellently referenced throughout’.Calibration techniques are covered in two chapters. The first, largely unchanged, deals with multiple linear regression. The second is expanded substantially and reflects the success of full spectrum techniques such as Principal Components Analysis (PCA) and Partial Least Squares (PLS), not only for deriving regression models which predict composition but also to provide insights into the physical and chemical basis on which these models depend. There are also brief descriptions of other techniques such as regression on Fourier coefficients, Discriminate Analysis, and Neural Networks which are currently being explored as alternatives to PLS and PCA. We then come to a chapter dealing with applications of NIR in the food industry. The original text is expanded by useful tables listing the accuracy expected in calibrations for moisture, protein and fat in a number of foods. Minor changes have been made to the section dealing with wheat and flour quality and additions include details on quality parameters for tea and chocolate, as well as techniques for dealing with aqueous solutions. The final chapter gives practical tips for deriving an NIR calibration. Again, it expands on the first edition reflecting how knowledge in this area has expanded in the last few years. The first edition was successful in that, unlike most NIR publications which consist of collections of monographs of varying quality by different authors, it provided a unified overview of the subject at a level suitable not only for beginners in the field but also for research workers who used it as a handy reference. This edition should also do well as it is produced to a high standard and is excellently referenced throughout. Whether there is enough new information to persuade those who already have the first edition to upgrade is debatable. Ian A . Cowe Multispec Ltd. York

ISSN:0003-2654    

DOI:10.1039/AN994190077N

出版商:RSC    

年代:1994

数据来源: RSC

摘要:

Analyst, June 1994, Vol. 119 79N Conference Diary Date 1994 July 3-7 11-14 18-22 20-22 Conference Location August International Chemometrics Research Veldhoven Meeting (Eindhoven) , The Netherlands Spectroscopy Across the Spectrum IV: Techniques and Applications of Analytical Norwich, UK Spectroscopy XIIIth International Congress on Electron Microscopy France Paris, VIIth Biennial National Atomic Spectroscopy Symposium UK Hull, 2-6 8-10 8-12 14-18 21-26 24-26 28-219 29-2l9 IInd Changchun International Symposium on Analytical Chemistry(C1SAC) XLth Canadian Spectroscopy Conference IGARSS '94: 1994 International Geoscience and Remote Sensing Symposium International Symposium on Bacterial Polyhydroxyalkanotes (ISBP '94) Changchun, China Halifax, Canada Pasadena, USA Quebec, Canada 208th ACS National Meeting (with Sessions of Washington, Analytical Chemistry, Environmental USA Chemistry, Chemical Health and Safety, etc ) International Symposium on Capillary York, Electrophoresis UK CLEOIEUROPE-EQEC European Amsterdam, Conference on Lasers and Electro-Optics/ European Quantum Electronics Conference Holland XLIIth International Mass Spectrometry Budapest, Conference Hungary Contact Mrs.Gerrie Westerlaken, Conference Organizing Bureau VNW, Postbus 1558,6501 BN Nijmegen, The Netherlands Tel: +3180 234471. Fax: +3180 601159 Dr. D. L. Andrews, School of Chemical Sciences, University of East Anglia, Norwich, UK NR4 7TJ Fax: +44 (0) 603 259 855 B. Jomrey, SFME 67, rue Maurice Gunsbourg, 94205, Ivry sur Seine cedex, France Tel: +33 1 46702844.Fax: +33 146708846 Dr. Steve Hill, Department of Environmental Sciences, University of Plymouth, Drake Circus, Plymouth, Devon, UK PL4 8AA Professor Quinhan Jin, Department of Chemistry, Jilin University, Changchun 130023, China Tel: +86 431 82233 (ext. 2433). Fax: +86 431 823907 Dr. W. D. Jamieson, Fenwick Laboratories Ltd., 5595 Fenwick Street, Suite 200, Halifax, NS B3H 4M2, Canada Tel: +(902) 420 0203. Fax: +(902) 420 8612 Meetings Department, Optical Society of America, 2010 Massachusetts Avenue, NW, Washington, DC 20036-1023, USA Tel: + 1 202 223 9034. Fax: + 1 202 416 6100 ISBP Secretariat, Conference Office, McGill University, 550 Sherbrooke St. West, West Tower, Suite 490, Montreal, Quebec, H3A lR9, Canada Tel: +1514 398 3770. Fax: +1514 398 4854 Mr.B. R. Hodson, American Chemical Society, 115516th Street N.W., Washington, DC 20036, USA Dr. T. L. Threlfall, Industrial Liaison Executive, University of York, Department of Chemistry, Heslington, York, UK YO1 5DD Tel: Direct line: 0904 432576 General Office: 0904 432511. Fax: + O M 432516 Meetings and Conference Department, The Institute of Physics, 47 Belgrave Square, London, UK SWlX 8QX Tel: +44 71 235 6111. Fax: +44 71 259 6002 Hungarian Chemical Society, H-1027 Budapest, Hungary Tel: +36 1201 6883. Fax: +36 1 15 6121580N Analyst, June 1994, Vol. 119 Date Conference September Location 4-7 5-6 5-9 6-8 11-16 12-15 12-15 12-15 13-18 14-15 18-22 19-20 19-21 19-21 19-23 21-23 East European Furnace Symposium Warsaw, Poland Ist International Symposium on Neuroelectrochemistry Coimbra, Portugal VIIth International Symposium on Synthetic Membranes in Science and Industry RSC Autumn Meeting (with Analytical Session on Analytical Challenges in Toxicology and Pollution) Tubingen, Germany Glasgow , UK EUCMOS XXII: XXIInd European Congress on Molecular Spectroscopy Germany Essen, Separations for Biotechnology Reading, UK IIIrd International Symposium on Krakow, Environmental Geochemistry Poland The 108th AOAC International Annual Meeting and Exposition USA Portland, IIIrd International Symposium on Mass Spectrometry in the Health and Life Sciences San Francisco, USA Waterborne Coatings and Additives Manchester, UK Geoanalysis 94: An International Symposium on the Analysis of Geological and Environmental Materials Ambleside, UK Chiral Europe '94 Nice, France IInd International Conference on Applications of Magnetic Resonance in Food Science IVth Annual CIM Field Conference Aveiro , Portugal Ontario, Canada Xmth International Symposium on Medicinal Paris, Chemistry France Wth International Symposium on Bournemouth, Environmental Radiochemical Analysis UK Contact Dr.Ewa Bulska, University of Warsaw, Department of Chemistry, UI. Pasteura 1,02 093 Warsaw, Poland Fax: +48 (22) 22 59 96 Profa. Dra. Ana Maria Oliveira Brett, Departamento de Quimica, Universidade de Coimbra, 3049 Coimbra, Portugal Tel: +351 39 22826. Fax: +35139 27703 Dechema, P.O. Box 970146, D-W-6000 Frankfurt am Main 97, Germany Dr. J. F. Gibson, The Royal Society of Chemistry, Burlington House, Piccadilly, London, UK W1V OBN Tel: +44 71 437 8656.Fax: +44 71 734 1227 GDCh-Geschliftsstelle, Abt. Tagungen, Varrentrappestr. 4042, Postfach 90 04 40, D- 6OOO Frankfurt am Main 90, Germany Tel: +49 69 79 17 358. Fax: +49 69 79 17 475 SCI Conference Office, 14/15 Belgrave Square, London, UK SWlX 8PS Tel: +44 71 235 3681. Fax: +44 71 823 1698 Helios Rybicka, Faculty of Geology, Geophysics and Environmental Protection, University of Mining and Metallurgy, Al. Mickiewicza 30, PL-30-059 Krakow, Poland Tel: +48 12 333290. Fax: +48 12 332936 Margaret Ridgell, AOAC International, 2200 Wilson Blvd, Suite 400, Arlington, Tel: +1 (703) 522 3032. Marilyn Schwartz, Department of Pharmaceutical Chemistry, University of California, San Francisco, CA 9413-0446, USA Mrs. C. L. Sharp, Conference Secretary, 41 Exeter Road, Davyhulme, Manchester, UK M41 O R F Tel: +061747 4961.Fax: +Of31747 4961 D. L. Miles, Analytical Geochemistry Group, British Geological Survey, Kingsley Dunham Centre, Keyworth, Nottingham, UK NG12 5GG Tel: +44 602 363100. Fax: +44 602 363200 Spring Innovations Ltd, 216 Moss Lane, Bramhall, Stockport, UK SK1 1BD Tel: +44 (0)61440 0082. Fax: +44 (0)61440 9127 Dr. A. M. Gil, Department of Chemistry, University of Aveiro, 3800 Aveiro, Portugal VA 22201-3301, USA 1994 CIM Field Conference, c/o Sudbury Geological Discussion Group, P.O. Box 1233, Station B, Sudbury, Ontario, Canada, P3E 4S7, CONVERGENCESnSMC '94,120 avenue Gambetta, 75020 Paris, France Fax: +33 1 40 31 0165 Dr. P. Warwick, Department of Chemistry, Loughborough University of Technology, Loughborough, Leicestershire, UK LEll 3TU Tel: +44 509 222585 or +44 509 222545.Fax: +44 509 233163Analyst, June 1994, Vol. 119 81N Date 21-24 22-24 25-28 25-30 26-28 26-30 29-30 Conference Location Vth International Symposium on Stockholm, Pharmaceutical and Biomedical Analysis Sweden XIIth National Conference on Analytical Chemistry Romania Constanta, Vth International Symposium on Chiral Discrimination Sweden Stockholm, 1994 European Workshop in Chemometrics Bristol, UK Protozoan Parasites and Water York, UK XVIth International symposium on Capiuary Chromatography Italy Riva del Garda, Food and Feed Analysis: A Focus on Methods Nyon, with Mineral Hazards to Health and the Switzerland Environment October 2-7 3-6 1&13 14-15 17-19 XXMth Annual Meeting of the Federation of Analytical Chemistry and Spectroscopy Societies PREP '94: XIth International Symposium on Preparative and Industrial Chromatography International Symposium on Chromatographic and Electrophoretic Techniques CITAC '94 Hong Kong Symposium on Traceability and Comparability of Analytical Measurements IIIrd International Symposium on Supercritical Fluids 30411 OPTCON '94 31-2/11 ANABIOTEC '94: Vth International Symposium on Analytical Methods, Systems and Strategies in Biotechnology November 6-12 IIIrd Rio Symposium on Atomic Spectrometry St.Louis, USA Baden-Baden, Germany Bled, Slovenia Hong Kong Strasbourg, France Boston, USA Minneapolis, USA Caracas, Venezuela Contact Swedish Academy of Pharmaceutical Sciences, P.O. Box 1136, S-11181 Stockholm, Sweden Tel: +46 8 245085.Fax: +46 8 205511 Dr. G.-L. Radu, Romanian Society of Analytical Chemistry 13 Bul. Carol I, Sector 3,70346 Bucharest, Romania Swedish Academy of Pharmaceutical Sciences, P.O. Box 1136, S-11181 Stockholm, Sweden Tel: +46 8 245085. Fax: +46 8 205511 Janice Green, School of Chemistry, University of Bristol, Cantock's Close, Bristol, UK BS8 1TS Tel: +44 (0)272 303030 (ext. 4421) or +44 (0)272 303672. Fax: +44 (0)272 251295 IFAB Communications, Institute for Applied Biology, University of York, York, UK YO1 5DD Tel: +44 (0)904 432940. Fax: +44 (0)904 432917 Professor Dr. P. Sandra, 1.0 .P.M.S., Kennedypark 20, B-8500 Kortrijk, Belgium Tel: +32 56 204960. Fax: +32 56 204859 T. Rihs, Swiss Federal Research Station for Animal Production, CH- 1725 Posieux , Switzerland Tel: +41 37 877 111.FACSS, P.O. Box 278, Manhattan, KS 66502- 0003, USA Tel: +1301846 4797. GDCh-Geschiiftsstelle, Abt. Tagungen, Varrentrappestr. 4042, Postfach 90 04 40, D- 6OOO Frankfurt am Main 90, Germany Tel: +49 69 79 17 358. Fax: +49 69 79 17 475 Dr. M. ProSek, National Institute of Chemistry, SLO-Ljubljana, Slovenia Fax: 386 61 12 59 244 Dr. T. L. Ting, CITAC '94 Secretariat, c/o Government Laboratory, Ho Man Tin Government Offices, 88 Chung Hau Street, Hong Kong Tel: +852 762 3706. Fax: +852 714 4083 Congres 'Fluides Supercritiques' Mle Brionne, ENSIC B.P. 451-1, rue Grandville, F-54001 Nancy Cedex, France Tel: +33 83 17 50 03. Fax: +33 83 35 08 11 Meetings Department, Optical Society of America, 2010 Massachusetts Avenue, NW, Washington, DC 20036-1023, USA Tel: +1202 223 9034.Fax: +1202 416 6100 Anabiotec Conference Secretariat, Elsevier Advanced Technology, Mayfield House, 256 Banbury Road, Oxford, UK OX2 7DH Tel: +44 (0)865 512242. Fax: +44 (0)865 310981 Professor Jod Alvarado, Universidad Simon Bolivar, Departamento de Quimica, Laboratorio de Absorci6n Atbmica, Apartado postal No. 89000, Caracas, 1080-A, Venezuela Fax: +58 2 938322/5719134/5763355/962169582N Analyst, June 1994, Vol. 119 Date 9-1 1 10-11 18-22 24-26 Conference XItb Montreux Symposium on Liquid Chromatography-Mass Spectrometry (LC/ MS; SFC/MS; CE/MS; MSMS) XVIIth International Conference on Chemistry, Bio Sciences, and Environmental Pollution Joint Oil Analysis Program International Condition Monitoring Conference Vth International Symposium on Advances in Electrochemical Science and Technology 1995 January 8-13 1995 Winter Conference on Plasma Spectrochemist r y Location Montreux, Switzerland New Delhi, India Pensacola, USA Madras, India Contact M.Frei-Hausler, Postfach 46, CH-4123 Allschwil 2, Switzerland Tel: +41614812789. Fax: +41614820805 Dr. V. M. Bhatnagar, Alena Chemicals of Canada, P.O. Box 1779, Cornwall, Ontario, Canada K6H 5V7 Tel: +1613 932 7702. Technical Support Center, Joint Oil Analysis Program, Bldg. 780, Naval Air Station, Pensacola, FL 32508, USA Tel: +1904 452 3191. The Secretary, Society for Advancement of Electrochemical Science and Technology, Karaikudi, 623 006, India Cambridge, UK Janice M. Gordon, Winter Conference on Plasma Spectrochemistry, Royal Society of Chemistry, Thomas Graham House, Science Park, Milton Road, Cambridge, UK CB4 4wF Tel: +44 (0)223 420066.Fax: +44 (0)223 420247 February 19-24 OFC '95: Optical Fibre Communication San Diego, Meetings Department, Optical Society of Conference USA America, 2010 Massachusetts Avenue, NW, Washington, DC 20036-1023, USA Tel: + 1 202 223 9034. Fax: + 1 202 416 6100 April 10-13 Annual Chemical Congress (with Analytical Edinburgh, Dr. J. F. Gibson, The Royal Society of Session) UK Chemistry, Burlington House, Piccadilly, London, UK W1V OBN Tel: +44 71 437 8656. Fax: +44 71 734 1227 May 7-11 XVIIth International Symposium on Virginia, USA Capillary Chromatography and Electrophoresis 21-26 CLEO '95: Conference on Lasers and B a1 timore, Elect ro-Optics USA 21-26 QELS '95: Quantum Electronics and Laser Baltimore, Science Conference USA Dr.Milton L. Lee, Department of Chemistry, Brigham Young University, Provo, Tel: +(801) 378-2135. Fax: +(801) 378-5474 Meetings Department, Optical Society of America, 2010 Massachusetts Avenue, NW, Washington, DC 20036-1023, USA Tel: +1202 223 9034. Fax: +1202 416 6100 Meetings Department, Optical Society of America, 2010 Massachusetts Avenue, NW, Washington, DC 20036-1023, USA. Tel: +1202 223 9034. Fax: +l 202 416 6100 UT 84602-4672, USAAnalyst, June 1994, Vol. 119 83N Date Conference Location Contact June 5-8 Vth Symposium on our Environment and Ist Convention City, Asia-Paciiic Workshop on Pesticides Singapore Environment, do Department of Chemistry, The Secretariat, 5th Symposium on our National University of Singapore, Kent Ridge, Republic of Singapore 0511 Fax: +65 779 1691 July 9-15 SAC95 Hull, UK Analytical Division, The Royal Society of Chemistry, Burlington House, Piccadilly , London, UK W1V OBN Tel: +44 71 437 8656.Fax: +44 71 734 1227 1&13 Vth COMTOX Symposium on Toxicology Vancouver, F. William Sunderman, Jr., M.D., Departments of Laboratory Medicine and Pharmacology, University of Connecticut Medical School, P.O. Box 1292, Farmington, CT 06034-1292, USA Tel: +1203 679 2328. Fax: +1203 679 2154 and Clinical Chemistry of Metals Canada August 27-U9 CSI XXIX: Colloquium Spectroscopicum Leipzig, Interna tionale Germany 27-1/9 XLVth Annual Meeting of the International Xiamen, Society of Electrochemistry (ISM) China September 68 Vth Workshop on Chemistry and Fate of Paris, Modern Pesticides France 12-15 Vth International Symposium on Drug Leuven, Analysis Belgium GDCh-Geschiiftssklle, Abt.Tagungen, Varrentrappestr. 4042, Postfach 90 04 40, D- 6OOO Frankfurt am Main 90, Germany Tel: +49 69 79 17 358/360/366. Fax: +49 69 79 17 475 Secretariat, 46th ISE Annual Meeting, P.O. Box 1995, Xiamen University, Xiamen 361005, China Tel: +86 592 2085349. Fax: +86 592 2088054 Professor M-C. Hennion, ESPCI, Labo. Chimie Analytique, 10 rue Vauquelin, 75005 Paris, France Professor J. Hoogmartens, Drug Analysis '95- Leuven, Institute of Pharmaceutical Sciences, Van Evenstraat 4, B-3000 Leuven, Belgium Tel: +32 16 28 34 40. Fax: +32 16 28 34 48 October 1-5 XXIst World Congress of the International The Hague, Mrs.J. Wills, ISF Secretariat, P.O. Box 3489, Champaign, IL 618263489, USA Tel: +217/359 2344. Fax: +217/3518091 Society for Fat Research (Ism The Netherlands November 5-10 OPTCON '95 San Jose, USA Meetings Department, Optical Society of America, 2010 Massachusetts Avenue, NW, Washington, DC 20036-1023, USA Tel: + 1 202 223 9034. Fax: + 1 202 416 610084N Analyst, June 1994, Vol. 11 9 Date Conference 1996 February Location Contact 6-9 IVth International Symposium on Bruges , Dr. R. Smits, Royal Flemish Chemical Society Hyphenated Techniques in Chromatography Belgium (KVCV), Working Party on Chromatography, (HTC 4); Hyphenated Chromatographic BASF Antwerpen N.V., Central Laboratory, Analysers Haven 725, Scheldelaan 600, B-2040 Antwerp, Belgium Tel: +32 3 561 28 31. Fax: +32 3 561 32 50 April 16-21 8-12 1-7 15-20 HPLC '96: XXth International Symposium on San Francisco, High Performance Liquid Chromatography USA XVI International Congress of Clinical Chemistry UK London, Euroanalysis M Bologna, Italy XXIst International Symposium on Stut t gart , Chromatography Germany Mrs. Janet Cunningham, Barr Enterprises, P.O. Box 279, Walkersville, MD 21793, USA Tel: +1301898 3772. Fax: +1301898 5596 Mrs. Pat Nielsen, XVI International Congress of Clinical Chemistry, P.O. Box 227, Buckingham, UK MK18 5PN Fax: +44 280 6487 Professor Luigia Sabbatini, Euroanalysis IX, Dipartimento di Chimica, Universith di Bari, Via Orabona, 4, 70126 Bari, Italy Tel: +39 80 242020/16/14. Fax: +39 80 242026 GDCh-Geschiiftsstelle, Abt. Tagungen, Varrentrappestr. 40-42, Postfach 90 04 40, D- 6OOO Frankfurt am Main 90, Germany Tel: +49 69 79 17 358/360/366. Fax: +49 69 79 17 475

ISSN:0003-2654    

DOI:10.1039/AN994190079N

出版商:RSC    

年代:1994

数据来源: RSC

摘要:

Analyst, June 1994, Vol. 119 85N Courses Date Conference Location Contact 1994 July 4-6 Problem Solving for Analytical Leaders York, Dr. T. L. Threlfall, Industrial Liaison Executive, UK University of York, Department of Chemistry, Heslington, York, UK YO1 5DD Tel: Direct line: 0904 432576 General Office: 0904 432511. Fax: +0904 432516 4-8 High Performance Liquid Chromatography Loughborough, Mrs. S. J. Maddison, Department of Chemistry, Short Course UK Loughborough University of Technology, Loughborough, Leicestershire, UK LEll 3TU Tel: + (0509) 222575. August 21-24 Capillary Electrophoresis Course York, UK Dr. T. L. Threlfall, Industrial Liaison Executive, University of York, Department of Chemistry, Heslington, York, UK YO1 5DD Tel: Direct line: 0904 432576 General Office: 0904 432511.Fax: +OW 432516 September 4-8 Molecular Graphics and Modelling Short York, Dr. T. L. Threlfall, Industrial Liaison Executive, course UK University of York, Department of Chemistry, Heslington, York, UK YO1 5DD Tel: Direct line: 0904 432576 General Office: 0904 432511. Fax: + O W 432516 5-9 AA/ICP-AES-ICP-MS Short CO- Loughborough, Mrs. S. J. Maddison, Department of Chemistry, UK Loughborough University of Technology, Loughborough, Leicestershire, UK LEll 3TU Tel: +(0509) 222575. 6-9 The Leeds Course in Clinical Nutrition Leeds, Mrs. Hilary L. Thackray, Department of UK Continuing Professional Education, Continuing Education Building, Springfield Mount, Leeds, UK LS2 9NG Tel: +(0532) 333233. Edward CharsleyBtephen Warrington, Thermal Analysis Consultancy Service, Leeds Metropolitan University, Calverley Street, Leeds, UK LS13HE Tel: +(0532) 833121/833122. Fax: +(0532) 833120 13-14 Recent Advances in Thermal Analysis Techniques Leeds , UK November 7-8 Short Course on LC/MS, SFCMS and cms December 15-17 Capillary Electrophoresis Short Course Montreux, Switzerland M. Frei-Hausler, Workshop Office IAEAC, Postfach 46, CH-4123 Allschwil2, Switzerland Loughborough, Mrs. S. J. Maddison, Department of Chemistry, UK Loughborough University of Technology, Loughborough, Leicestershire, UK LEll 3TU Tel: + (0509) 222575. Entries in the above listing are included at the discretion of the Editor and are free of charge. If you wish to publicize a forthcoming meeting please send full details to: The Analyst Editorial Office, Thomas Graham House, Science Park, Milton Road, Cambridge, UK CB4 4WF. Tel: +44 (0)223 420066. Fax: +44 (0)223 420247.

ISSN:0003-2654    

DOI:10.1039/AN994190085N

出版商:RSC    

年代:1994

数据来源: RSC

摘要:

86N Analyst, June 1994, Vol. 119 Future Issues will lnclude- Synthesis and Efficiency of a Polyacrylacylisothiourea Chelat- ing Fibre for the Preconcentration and Separation of Trace Amounts of Gold, Palladium and Ruthenium from Solution Samples-Xijun Chang, Zhixing Su, Guangyao Zhang, Xing- yin Luo and Wenyun Gao Application of a Picrolonate Ion Selective Electrode to the Assay of Calcium and Piperazine in Pharmaceuticals and Serum-Miltiades I. Karaynnis, Mamas I. Prodromidis and Panayiotis G. Veltsistas Direct and Rapid Determination of Potassium in Standard Solid Glasses by Excimer Laser Ablation Plasma Atomic Emission Spectrometry- Joseph Sneddon and Yong-I11 Lee Characterization of Inductively Coupled Plasma Mass Spec- trometry With Segmented-flow Injection-Diane Beauchemin and Jane M.Craig Fluorescent Detection of Hydrazine, Monomethylhydrazine, and 1,l-Dimethylhydrazine by Derivatization with Aromatic Dicarboxaldehydes4usan L. Rose-Pehrsson and Greg E. Collins Design and Characterization of a Thermochemical High- performance Liquid Chromatography Flame Photometric Detector Interface for the Speciation of Sulfur-Jean-Simon Blais, T. Nicodemo, N. N. Barthakur and J. Bernard Determination of Micro Amounts of Lanthanoids in Cast Iron after Solid-Liquid Extraction With Diethyldithiocarbamate- Xinzhen Du, Zingguo Hou, Su Zhao, Jingwan Kang and Jinzhang Gao Multivariate Statistical Analysis of Gas Chromatograms to Differentiate Cocoa Masses by Geographical Origin and Roasting Conditions-€. V. Hernhdez and D. N. Rutledge Extraction and High-performance Liquid Chromatographic Method for the Determination of Microcystins in Raw and Treated Waters-Linda A.Lawton, Christine Edwards and Geoffrey A. Codd Physico-chemical Properties of Oxybutyltin-Etsuko Miyam- oto, Susumu Kawashima, Yoshifumi Murata, Yoko Demizu, Yutaka Yamada, Hitoshi Kontani and Takeshi Sakai Electrode Function of Selective Membranes for Anions of Phthalic Acid Isomers-Ryszard Dumkiewicz Voltammetric Determination of Trace Metals and Organics After Accumulation at Modified Electrodes-Damien W. M. Arrigan Rapid Determination of Total Biomass from a Yeast Fermen- tation by Sequential Injection Ana1ysis-G. D. Christian, P. J. Baxter and J. R&ka Investigation of the Stability of Medicinal Additives in Animal Feedingstuffs to Prepare Reference Feeds-Indu Patel, Keith R.B. Marshall, Carole Williams, Hannah Othman and Neil T. Crosby Trace Enrichment of Chlorinated Phenols from Drinking Water on Chemical Bonded Sorbents for High-performance Liquid Chromatography-Jitka FrCbortovh and Vera Tatarkovicovh Determination of Thyroxine in Urine by Cathodic Stripping Square-wave Voltammetry-Lucas Hernhndez, P. Hernandez and 0. Nieto Fast Determination of Aluminium Reactive to 1,2-Dihydrox- yanthraquinone-3-sulfonic Acid in Sea-water- J. J. Herdn- dez-Brito, M. D. Gelado-Caballero, J. P6rez-Peiia and J. A. Herrera-Melian COPIES OF CITED ARTICLES The Royal Society of Chemistry Library can usually supply copies of cited articles. For further details contact: The Library, Royal Society of Chemistry, Burlington House, Piccadilly, London W1V OBN, UK. Tel: +44 (0)71-437 8656. Fax: +44 (0)71-287 9798. Telecom Gold 84: BUR210. Electronic Mailbox (Internet) LIBRARY@RSC.ORG. If the material is not available from the Society’s Library, the staff will be pleased to advise on its availability from other sources. Please note that copies are not available from the RSC at Thomas Graham House, Cambridge.

ISSN:0003-2654    

DOI:10.1039/AN994190086N

出版商:RSC    

年代:1994

数据来源: RSC

摘要:

Analyst, June 1994, Vol. 119 87N The Science Museum and The Royal Society of Chemistry Launch a National Competition The high standard of living enjoyed in developed countries depends largely on the products and processes made possible by chemistry. In particular it is analytical chemistry that allows the monitoring and control of these chemical processes. The Science Museum is looking for new ways to explain and demonstrate how the methods used in analytical chemistry work. The intention is to develop a series of exhibits that will give ‘hands-on’ and interactive experience where possible, which will enable people of all ages to understand the basic principles of analytical chemistry techniques, to appreciate how they have been developed and applied, and to be made aware of their importance.Analytical chemists employ all the properties of matter and the forces of nature to distinguish chemicals and determine their concentrations. There are hundreds of variations on the basic themes of spectroscopy, chromatography, magnetic resonance, chemical and biochemical interactions, each being suitable for different cases. Much of our understanding of environmental processes and the political pressure to end polluting practices stems from the chemist’s ability to detect ever smaller quantities of chemicals. The ‘hole’ in the ozone layer is caused by a change of a few parts per million; dioxins in soil and water can be detected in parts per trillion-which is like finding a particular grain of sand on a beach. Analytical techniques can also lead on to new and unexpected technologies.Who could have predicted that interest in the behaviour of chemicals in a magnetic field would have led first to the development of nuclear magnetic resonance as an analytical tool and then to magnetic resonance imaging in hospital scanners? The Royal Society of Chemistry (RSC) and the Science Museum have decided to consult widely to find ways to show the best of chemistry by novel and entertaining methods. To engage as many people as possible in the process, the two organizations are pleased to announce a national competition to promote the design of new displays that will meet the requirements for interactive and informative exhibits. The panel of judges will be chaired by Dr. Mary Archer, CChem, FRSC, a trustee of the Science Museum and Chairman of the National Energy Foundation. Suitable entries may be deve- loped into exhibits to be installed in the Science Museum in the first instance, and could possibly form the basis of a planned refurbishment of the Chemistry Galleries of the museum. The RSC may consider further sponsorship to help the museum improve public understanding of chemistry. Prizes totalling 25000-with a first prize of 1000 guineas- will be provided by the Analytical Chemistry Trust of the Royal Society of Chemistry. Details of the competition, together with rules and entry forms, may be obtained by writing to: Chemistry in Action Competition The Royal Society of Chemistry Burlington House Piccadilly London W1V OBN Tel: 071 437 8656 Completed entries should be returned by 31st August, 1994. The prize winners will be announced during National Chem- istry Week, which takes place 9-16 November, 1994.

ISSN:0003-2654    

DOI:10.1039/AN99419087Na

出版商:RSC    

年代:1994

数据来源: RSC

摘要:

Analyst, June 1994, Vol. 11 9 1109 Study of the Stability of Extractable Trace Metal Contents in a River Sediment Using Sequential Extract ion* H. D. Fiedler, J. F. L6pez-SBnchez, R. Rubio and G. Rauret Departament de Quimica Analitica, Universitat de Barcelona, Av. Diagonal 647, 08028 Barcelona, Spain Ph. Quevauviller Commission of the European Communities, Community Bureau of Reference (BCR), Directorate General for Science, Research and Development, Rue de la Loi 200, B-1049 Brussels, Belgium A. M. Ure Department of Pure and Applied Chemistry, University of Strathclyde, Glasgow, UK GI 1XL H. Muntau Environment Institute, Joint Research Centre, CEC, I-21 020 Ispra (Varese), Italy Sequential extraction schemes have been used in recent years to study the environmental behaviour of trace metals present in soils and sediments.Owing to the variety of the different extraction procedures, the results obtained were not comparable as they were highly dependent on the procedure. Moreover, the lack of suitable reference materials for this type of analysis prevents quality control of the measurements. In 1987 the Community Bureau of Reference (BCR, now Measuring and Testing Programme) started a programme to harmonize the methodology and to produce certified reference materials. This paper presents the work carried out to prepare a river sediment sample to be analysed in an intercomparison exercise using a common sequential extraction scheme adopted at Sitges by a group of European experts. The studies of homogeneity and stability with time of the extractable trace metal contents in the sample are also reported.Keywords: Sequential extraction scheme; extractable trace metal content; sediment; homogeneity; stability Introduction The determination of extractable trace metal contents in soils and sediments is currently performed in many laboratories to assess the bioavailable metal fraction (and related potential phytotoxic effects) and the importance and possibility of mobilization of trace metals from polluted soil, sludge or sediment used for landfill. Various methods have been developed in the last two decades involving both single and sequential extraction schemes. Although some schemes have received wide acceptance, such as those described by Tessier et al.1 and Salomons and Forstner,2 none of them has been developed into a commonly accepted procedure.The lack of uniformity in the different extraction procedures used does not allow the results to be compared or the procedures to be validated. This has led to many criticisms in the past few years. Indeed, the results obtained are highly dependent on the extraction procedures used. Moreover, the lack of suitable Presented at Euroanalysis VIII, Edinburgh, Scotland, UK, September 5-11, 1993. reference materials for this type of analysis does not enable the quality of the measurements to be controlled. In this context, in 1987 the Community Bureau of Refer- ence (BCR, now Measuring and Testing Programme) started a programme to harmonize the methodology used in single and sequential extraction schemes for the determination of extractable trace metals in soils and sediments and also to produce certified reference materials (CRMs).After a thor- ough study of the state-of-the-art,3 a single scheme was suggested and accepted by all the participants in the BCR programme and tested in an intercomparison.4 This scheme, especially if it is backed up by reference materials, will facilitate the achievement of good quality control of analysis. At this stage it is necessary to demonstrate the feasibility of the preparation of material that fulfils the basic requirements of a CRM for stability and homogeneity,5-7 not as regards the total metal content but for the sequentially extractable metal contents determined by applying the common scheme adop- ted by the participants in the BCR programme.In this paper we present the work carried out to prepare a river sediment sample to be analysed in a second intercomparison exercise organized in 1992 using the common scheme and to study the homogeneity and the stability with time of this sample. These preliminary studies are of great importance in order to obtain stable reference materials,g particularly for the determination of extractable metals in soils and sediments. Experimental The preparation of the sample for the second intercomparison exercise on extractable trace elements in sediments was conducted in different subsequent phases: sampling, sample treatment, homogenization and bottling, homogeneity and stability studies and, finally, delivery to the participants in the intercomparison.A flow chart of the sample preparation and characterization operations is given in Fig. 1. Sampling Sediment sample was collected in the River Beds (Catalonia, N.E. Spain) on June 12, 1991. The river is characterized, like other small Mediterranean rivers, by irregular flows that are1110 Analyst, June 1994, Vol. 119 0.1 1 mol r' HAc; 40 ml g-'(v/m) 20 "C, shaking overnight heavily dependent on rainfall. The basin is the most polluted area in Catalonia, mainly owing to the high discharge of industrial and domestic effluents and the lack of sufficient wastewater treatment plants. Sediment was collected with a 0.1 mol r' NH, OH. HCI (PH = 2 with HNO,) 40 ml g-'(v/m); 20 "C; shaking overnight Air drying Fig. 1 Flow chart of the sample preparation and characterization studies.grab at a depth of 10-15 cm on a bank in a zone where the water was not turbulent and the flow was extremely low, and was placed in polyethylene containers. The containers were stoppered and taken to the laboratory. Sample Treatment The containers containing the sample were left to settle for 2 weeks, the supernatant water was removed and the sediment was spread out on a polyethylene sheet and left to dry. After drying, the aggregates were broken down and the <63 pm particle size fraction was retained after sieving. The sieve used was made of wood with nylon mesh. Finally, the amount of sample obtained (4.1 kg) was homogenized and bottled in dark glass bottles; about 60 bottles were each filled with 50 g of the material. Apparatus and Reagents A Perkin-Elmer Model 4O00 atomic absorption sepctrometer equipped with a Perkin-Elmer Model HGA 500 graphite Sequential Extraction Procedure ~ ~ ~~~ Table 2 Percentages of total (C,), organic (CO) and inorganic carbon (C,) determined in sediment samples Fig.2 Schematic diagram of the sequential extraction procedure to determine extractable trace metals in soils and sediments. Table 1 Major components, as percentage of oxides, determined by XRF and moisture content [mean (X), standard deviation (s), relative standard deviation (sr) and number of independent determinations @)I Major components Si02 CaO A1203 Fez03 p20.5 MgO K20 MnO Ti02 Na20 Moisture content X(%o) 27.72 22.46 7.71 3.43 2.32 1.43 1.41 0.45 0.36 0.42 1.9 S (%) 0.36 0.12 0.15 0.02 0.08 0.02 0.014 0.005 0.016 0.003 sr(%) 1.31 0.53 1.92 0.62 3.54 1.47 1.01 1.04 4.47 0.76 n 20 20 20 20 20 20 20 20 20 10 Bottle No.C, (%) CO (%) CI ("/I 3 9.68 5.32 4.36 7 9.69 5.95 3.74 9 9.80 5.73 4.07 Table 3 Percentages of sulfur (total, as sulfate and as sulfide) determined in sediment samples ST(%) sso42- (%) ss2- (Yo) ss2- (Yo) Bottle No. (GC-TCD)* (GC-TCD)' (GC-TCD)* (SM)* 3 1.33 1.30 0.03 0.022 fO.01 8 1.27 1.24 0.03 - 9 0.025 fO.O1 - - - 0.022 fO.O1 10 1.32 1.29 0.03 * GC-TCD = gas chromatography with thermal conductivity detection. SM = spectrophotometric method. & = total sulfur; Sso42- = sulfur in the form of sulfates; Ss2- = sulfur in the form of sulfides. Table 4 Cd,Cr, Cu, Ni, Pb and Zn total contents in sediment samples Analytical Compon- method* ents XRF c u Ni Pb Zn FAASt Cr c u Pb Ni Zn ICP-AES Cr ETAAS Cd ZEAAST Cd X k g- 139 205 1120 1343 127 237 64 1138 1338 56.4 1.79 1.95 S/cLg g-I 1.0 0.70 1.49 5.9 175.0 0.91 0.95 1.25 20.0 87.0 0.29 0.10 s r ("/.I 0.69 1.24 0.73 0.53 0.72 0.40 2.00 1.76 6.55 4.95 13.0 16.1 n 10 10 10 10 6 6 6 6 6 6 6 8 * XRF = X-ray fluorescence spectrometry; FAAS = flame atomic absorption spectrometry; ICP-AES = inductively coupled plasma atomic emission spectrometry; ETAAS = electrothermal atomic absorption spectrometry; ZEAAS = Zeeman effect electrothermal atomic absorption spectrometry.t Following triple acid attack (HN03-HF-HC104).1111 Analyst, June 1994, Vol. 119 Table 5 Relative standard deviations obtained in the within- and between-bottle homogeneity study s, (%)* (Us,)t (within-bottle) s r (%I* (us,)’ (between-bottle) Bottle 3 Bottle 7 Bottle 9 Element Step1 Step2 Step3 Step1 Step2 Step3 Step1 Step2 Step3 Step1 Step2 Step3 20.1 3.9 3.9 4.1 9.8 -5 - - - - - - - 13.4 5.2 5.4 12.9 8.3 24.3 4.8 5.1 6.5 12.4 14.9 6.5 5.8 6.6 5.7 9.5 (4.5) (3.0) (3.3) (0.9) (1.2) (1.5) (0.9) (1.3) (1.2) (2.9) (1.8) (1.5) (1.3) (1.5) (1.5) (0.9) (1.9) - (2.1) - (2.7) (2.2) (5.4) (1.1) (1.1) - - Cd Cr c u Ni Pb - - - - - - - - - - - - - - - 6.9 - - 7.5 - 3.6 - - (0.8) - - - - ., 4.9 5.9 4.9 4.9 7.3 5.7 6.8 7.0 6.4 5.0 5.7 4.9 (1.1) (1.3) (1.1) (1.1) (1.6) (1.3) (1.5) (1.6) (1.4) (1.1) (1.3) (1.1) Zn * Single determination on the content of each of 10 bottles. t us, = s, (%)/(2n)k Ten replicates of the determination on the content of one bottle. 5 Dashes indicate concentration below the determination limit.furnace and a Perkin-Elmer Model 1100 B atomic absorption spectrometer with an air-acetylene flame were used for metal determination in sample extracts and for total Co, Cr, Ni, Pb and Zn determination after a triple acid digestion of the sample. A Varian Model SpectrAA-40 atomic absorption spec- trometer equipped with a graphite furnace and Zeeman-effect background corrector and a Jobin-Yvon Model JY-38 induc- tively coupled plasma atomic emission spectrometer were also used for total Cd and Cr determination, respectively. A Carlo Erba Model EA 1108 elemental analyser, equipped with a ‘flash combustion’ furnace, a chromatographic column (Porapak, PQS) to separate the combustion gases (C02, H20, N2 and S02) and a thermal conductivity detector, was used to determine C and S.A Philips PW-1400 X-ray spectrometer with Rh and Au excitation tubes was used to determine major components. All reagents used were of analytical-reagent grade or Suprapur from Merck. Doubly de-ionized water, obtained with a Culligan Ultrapure-GS system, resistivity 18.3 MQ cm, was used. Stock standard solutions (1 g 1-1 of metal) acidified with nitric acid were prepared, All standard and reagent solutions were stored in polyethylene bottles. All trace metal analyses were performed in a clean laboratory equipped with a Class-100 work bench. All glassware and plasticware used for experiments was previ- ously soaked in 10% v/v nitric acid overnight and rinsed five times with doubly de-ionized water.Procedures Determination of major components Samples for X-ray fluorescence (XRF) measurements were prepared as lithium tetraborate melts for the determination of major components (si, Ti, A], Fe, Mg, Ca, Na, K, Mn and p)- Calibration was carried out using a Series Of natural geological Fig. Results of the homogeneity study of sediment sample. The length of the error bar on each block represents 2. A = Between bottle; B = within bottle 3; C = within bottle 7; and D = within bottle 9. reference materials. Table 6 F values obtained on comparing the within- and between-bottle variances of the homogeneity study Bottle 3 Bottle 7 Bottle 9 Element Step 1 Step 2 Step 3 Step 1 Step 2 Step 3 Step 1 Step 2 Step 3 - 2.250 Cd Cr - - 1.563 - - 1.174 - - 1.778 c u - - 1.154 - - 1.121 - - 1.917 Ni 4.340* - 3.820 2.507 - 3.939 3.674 - 9.899* Pb - - 1.310 - - 2.232 - - 1.394 Zn 1.OOO 1.531 1.353 1.926 1.408 1.706 1.041 1.071 1 .OOo value of Ffor a two-tailed test (P = 0.05) is 4.026.- - 3.049 - - 1.236 - * Values in italics indicate that a significant difference exists between standard deviations because the Fvalue is above the critical value. Critical1112 Analyst, June 1994, VoE. 11 9 The determination of the total carbon content using the EA 1108 elemental analyser requires the use of the V2O5 catalyst in the combustion step. To determine the organic carbon content, samples were digested overnight with 2 mol 1-1 HCl with continuous stirring at room temperature in order to eliminate carbonates and then analysed with the elemental analyser.The inorganic carbon was calculated as the differ- ence between the total carbon and organic carbon contents. The determination of the total sulfur content using the EA 1108 elemental analyser requires the use of the V205-Sn catalyst in the combustion step. To determine sulfur present as sulfate, samples were digested overnight with 6 mol 1-1 HCl with continuous stirring at 60 "C. The sulfur content present as sulfide was determined by the Methylene Blue spectropho- tometric methodgJ0 and was also calculated as the difference between total and sulfate sulfur. Moisture content was determined by drying at 105 "C in an electric oven to constant mass. Determination of trace metals Samples for XRF measurements were prepared with Elvactite 2044 agglutinative for trace determinations of Cu, Ni, Pb and Zn.Samples for atomic absorption spectrometric (AAS) and inductively coupled plasma atomic emission spectrometric (ICP-AES) measurements were digested with a triple acid mixture [HF-HN03-HC104 (5 + 4 + l)] at 120 "C. Sequential extraction procedure The detailed protocol (Fig. 2) for sequential extraction used in this work to study extractable trace metal contents in sediment samples is described el~ewhere.~ The extraction procedure has three steps, using sequentially dilute acetic acid (0.1 moll-*), a reducing agent (0.1 mol 1-1 hydroxylammonium chloride) and an oxidizing agent (8.8 moll-' hydrogen peroxide). Results Sample Characterization In order to establish the total composition of a sediment sample, different sets of analyses were carried out, using XRF, AAS and carbon and sulfur analysers.The results obtained are summarized in Tables 1-4. In Table 1 the mean value X, the standard deviation, s, the relative standard deviation, s,, and the number of independent determinations, n , are given for XRF measurements. As the sediment was collected from a calcareous basin the high Ca content was to be expected and the value found was comparable to those obtained in previous studies for samples collected in this zone11?1*. In Table 2 the total carbon, C,, the organic carbon, Co, and the inorganic carbon, CI, contents are given. Important levels of organic and inorganic carbon were also found correspond- ing to high levels of organic matter and carbonates. These carbon contents approximately correspond to 20% of carbo- nate and 9.6% of organic matter, the latter calculated by multiplying the percentage of organic carbon by 1.7.13 In Table 3 the percentages of total sulfur, ST, sulfates and sulfides are given.The remarkably high content of sulfate was probably due to oxidation of the original sulfide during the sample pre-treatment. The sum of the total inorganic components (Table 1) accounts for 70.71% of the material. This, together with the approximately 20% carbonate and the estimated 9.6% organic matter, makes up a total of approximately 100.3% and accounts for all major constituents of the material. In Table 4 the results for total contents determined by different methods are given. Each element was determined by means of two different techniques, Cu, Ni, Pb and Zn by XRF and flame AAS (FAAS) and Cr by FAAS and ICP-AES.In all instances the results obtained by different techniques were in good agreement. Cd was only determined by electrothermal AAS (ETAAS) but using different background correctors [deuterium lamp and Zeeman effect (ZE)]. No significant Table 7 Stability study during 8 months. The values found at t = 0 (September 1992) were taken as a reference Element Cd Cr c u Ni Pb Zn * RT = Xt/xI=o, where Time (months) 1 2 4 8 1 2 4 8 1 2 4 8 1 2 4 8 1 2 4 8 1 2 4 8 Step I Step 2 Step 3 RT* UT* - X X X X X X X X X X X X - - - - - - - - - - - 1.08 0.08 1.07 0.06 1.04 0.07 0.88 0.06 - X X X X - - - 0.88 0.05 0.94 0.04 0.98 0.04 1.01 0.05 RT* UT* - X X X X X X X X X X X X X X X X X X X X - - - - - - - - - - - - - - - - - - - 0.88 0.06 0.93 0.07 0.96 0.06 0.91 0.06 RT* 0.90 1.05 0.90 0.97 0.95 1.01 0.96 0.91 0.97 1.01 1.03 0.94 1.01 0.94 1.10 0.95 0.90 0.94 0.92 0.97 1.05 1.04 1.17 - UT* 0.12 0.23 0.11 0.07 0.08 0.07 0.06 0.04 0.06 0.03 0.03 0.07 0.04 0.07 0.05 0.12 0.11 0.14 0.13 0.05 0.05 0.05 0.07 - X, = mean value ( t = 1, 2, 4, 8 months), six measurements on each of the three bottles, and X,=O = mean value, six measurements on each of the three bottles ( t = 0).U, = (sr: + srt=02)i R~/100.Analyst, June 1994, Vol. 11 9 1113 difference was found in the results using the two different background correction systems. Homogeneity The ‘between-bottle’ homogeneity of extractable trace metal contents was verified by the application of the sequential extraction procedure for Cd, Cr, Cu, Ni, Pb and Zn of 500 mg sub-samples taken from ten bottles selected randomly from the total set of 60 bottles.The ‘within-bottle’ homogeneity was assessed by ten replicate determinations on the well mixed content of one bottle. This test was performed with three different bottles selected randomly from the set of ten bottles. Before sub-sampling, each bottle was shaken manually for 5 min to eliminate segregation that might have occurred during transport and storage. The metal content in the extracts obtained in the sequential extraction protocol were deter- mined by FAAS or ETAAS depending on the concentration. The relative standard deviations (s,) for the elements extrac- ted in the different steps, and the uncertainty of s,, Us,, are presented in Table 5 and summarized in Fig.3. Us, was estimated using the equation Us, = s,./(2n)4, where n is the number of replicates. In Table 5, the Usr values are given in parentheses. The Cd, Cr, Cu, and Pb contents in the first and second steps and the Ni content in the second step were below the limit of determination, and an accurate determination by ETAAS was not possible. The high s, values obtained for Cd can be explained by the low content of this metal, less than 2 pg g-l, compared with the contents of other elements, which are one to three orders of magnitude higher. In Table 6 the values obtained when applying the F-test at a significance level of 0.05 are given. These values did not reveal significant differences between the within- and between-bottle variances for Cd, Cr, Cu, Pb and Zn.However, a significant difference was obtained for Ni, especially when comparing the within- and between-bottle variances for bottle 9 in the third step. These local differences were attributed to random errors in the analytical process, and they can be considered more an analytical artifact than an indication of inhomogeneity. It should be emphasized first that the metal content extracted in some steps is very low, approaching the detection limit, and second that the experimental conditions must be followed rigorously. It was therefore concluded that the material was sufficiently homogeneous for samples of 500 mg and above to be representative of the whole material. Fig. 4 Results of the stability study of sediment sample.The length of the error bar on each block represents 2UT. A = Month 1; B = Month 2; C = Month 4; and D = Month 8. Stclbility The stability of the extractable trace metal contents was tested to determine the suitability of this kind of material as a candidate reference material. The sequential extraction pro- cedure was applied at the beginning of the storage period and after 1, 2, 4 and 8 months. Instability would be detected by comparing the contents of different elements obtained at the beginning of the storage period ( t = 0) with those obtained later. Table 7 gives the ratios (RT) of the mean values (X,) of six measurements made at t = 1,2,4 or 8 months versus the mean value (X,=,) from six determinations made at t = 0. The uncertainty, U, was obtained from the relative standard deviation of six measurements obtained at the beginning of the storage period (t = 0) and at various occasions of analysis (t): UT = (srt + srt = o2)t RT/IOO Fig.4 shows the calculated RT values and the uncertainty (error bar). With complete stability RT should be 1. In practice, however, there are some random variations due to errors in the analytical process. In this study errors have an effect on both the values obtained at the beginning of the storage period (taken as reference) and the values obtained later. In all instances the values RT L- UT overlap with the range 1 k 0.1, considering a variation of 10% as usual in this kind of analysis. On the basis of these results, it can be concluded that no instability could be demonstrated.Conclusions From the results obtained it can be concluded that it is possible to prepare a homogeneous and stable candidate sediment reference material for the certification of extractable contents of trace metals by applying a common sequential extraction procedure proposed and accepted by a large group of European experts working in this field. The authors thank Serveis Cientifico T&cnics (University of Barcelona) for their support with some measurements (XRF, elemental analyser, ZEAAS and ICP-AES). H. Fiedler thanks the Conselho Nacional de Desenvolvimento Cientifico e Technol6gico (CNPq) and Fundaqao Estadual de ProteCao Ambiental (FEPAM-RS), Brazil. References Tessier, A., Campbell, P. G. C., and Bisson, M., Anal.Chem., 1979,51,844. Salomons, W., and Forstner, U., Environ.Technol. Lett., 1980, 1, 506. Ure, A., Quevauviller, Ph., Muntau, H., and Griepink, B., EUR Report 14763 EN, CEC, Brussels, 1993. Proceedings of the Workshop on the Sequential Extraction of Trace Metals in Soils and Sediments, eds. AlbaigCs, J., Rauret, G., and Quevauviller, Ph., Special Issue, Znt. J. Environ. Anal. Chem., 1993,51, Nos. 1-4. Faure, U., and Wagstaffe, P. J., Fresenius’ J. Anal. Chem., 1993,345, 124. Broderick, B. E., Cofino, W. P., Cornelis, R., Heydorn, K., Horwitz, W., Hunt, D. T. E., Hutton, R. C., Kingston, H. M., Muntau, H., Baudo, R., Rossi, D., van Raaphorts, J. G., Lub, T. T., Schramel, P., Smyth, F. T., Wells, D. E., and Kelly, A. G. Mikrochim. Acta, Part IZ, 1991, 523. Kurfiirst, U., Pauwels, J., Grobecker, K. H., Stoeppler, M. S., and Muntau, H., Fresenius’ J. Anal. Chem., 1993,345, 112. Maier, E. A., TrAC, Trends Anal. Chem., 1991, 10,340. Photometric and Fluorometric Methods of Analysis, Nonmetals, Wiley, New York, 1981.1114 Analyst, June 1994, Vol. 119 10 Standard Methods for the Examination of Water and Wastewater, eds. Franson, M. A. H., Clesceri, L. S., Greenberg, A. E., and Trussell, R. R., American Public Health Association, American Water Works Association, Water Pollution Control Federation, Washington, DC, 17th edn., 1989. 11 Rauret, G., Rubio, R., Mpez-SBnchez, J. F., and Casassas, E., Water Res., 1988,22,449. Paper 3105636H 12 Rubio, R., Mpez-SBnchez, J. F., and Rauret, G., An. Quim., Received September 20, 1993 1991,87,599. Accepted November 16, 1993 13 Olausson, E., Methods for the Chemical Analysi~ of Sediments, FA0 Fisheries Technical Paper No. 137, Food and Agriculture Organization of the United Nations, Rome, 1975.

ISSN:0003-2654    

DOI:10.1039/AN9941901109

出版商:RSC    

年代:1994

数据来源: RSC