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ANPRDI 28(9) 281-308 (1 991 ) ISSN 0144-557X President J. D. R. Thomas Hon. Publicity Secretary Dr. J. D. Green, BP Chemicals Ltd., Research and Development Department, Hull Laboratories, Saltend, Hull HU12 8DS Editor, Analytical Proceedings Roger A. Young Editorial Secretary Claire Harris Analytical Proceedings Proceedings of The Analytical Division of The Royal Society of Chemistry Analytical Division Officers: Hon. Assistant Secretary F. W. Sweeting Hon. Secretary C. A. Watson Analytical Division Secretary Miss P. E. Hutchinson Editorial Manager, Analytical Journals Judith Egan *H. M. Frey D. E. Games S. J. Hill D. L. Miles Senior Assistant Editor Paul Delaney Publication of Analytical Proceedings is the responsibility of the Analytical Editorial Board: A.G. Fogg (Chairman) K. D. Bartle D. Betteridge *J. Egan R. M. Miller B. L. Sharp "Exofficio members All editorial matter should be addressed to The Editor, Analytical Proceedings, The Royal Society of Chemistry, Thomas Graham House, Science Park, Milton Road, Cambridge CB4 4WF, UK. Telephone 0223 420066. Telex 818293 ROYAL. Analytical Proceedings (ISSN 0144-557x3 is published monthly by The Royal Society of Chemistry, Thomas Graham House, Science Park, Milton Road, Cambridge CB4 4WF, England. All orders, accompanied by payment, should be sent to The Royal Society of Chemistry, Turpin Transactions Ltd., Blackhorse Road, Letchworth, Herts. SG6 IHN, England. 1991 Annual Subscription price if purchased on its own: EC f l l O .O O , Rest of World f126.00, US $258.00, including air speeded delivery. 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, N.Y. 11003. USA Postmaster: Send address changes to: Analytical Proceedings, Publications Expediting Inc., 200 Meacham Avenue, Elmont, N.Y. 11003. Second class postage paid at Jamaica, N.Y. 11431. All other despatches outside the UK by Bulk Airmail within Europe, Accelerated Surface Post outside Europe. PRINTED IN THE UK. Nb: Turpin Transactions Ltd., distributors, is wholly owned by the Royal Society of Chemistry. @The Royal Society of Chemistry 1991.All rights reserved. No part of this publication may be reproduced, stored in a retrieval system, or transmitted in any form, or by any means, electronic, mechanical, photographic, recording, or otherwise, without the prior permission of the publishers. ANALYTICAL JOURNALS 1991 The Analyst ISSN 0003-2654 12 issues per annum plus index EC f246.00 USA $580.00 Rest of World f283.00 Analytical Proceedings ISSN 0144-557X 12 issues per annum plus index EC f l l O . O O USA $258.00 Rest of World f126.00 Published by the Royal Society of Chemistry Journal of Analytical Atomic Spectrometry (JAAS) ISSN 0267-9477 8 issues per annum (including two special issues) plus index EC f309.00 USA $728.00 Rest of World f355.00 Analytical Abstracts ISSN 0003-2689 12 issues per annum EC f380.00 USA $765.00 Rest of World f420.00 SPECIAL PACKAGES (Non-RSC Members only) The Analyst, Analytical Abstracts and Analytical Proceedings Journal Ref.No. 000&0124 EC f648.00 USA $1527.00 Rest of World f745.00 The Analyst and Analytical Proceedings Journal Ref. No. 0000-0140 EC $313.00 USA $738.00 Rest of World f360.00 The Analyst and Analytical Abstracts Journal Ref. No. 0000-0132 EC f551.00 USA $1299.00 Rest of World f634.00 ORDERING: Non-RSC Members should send their orders to: The Royal Society of Chemistry, Turpin Transactions Ltd, Blackhorse Road, Letchworth, Herts SG6 lHN, UK. RSC Members should obtain members prices and send their orders to: Membership Affairs, The Royal Society of Chemistry, Thomas Graham House, Science Park, Milton Road, Cambridge CB4 4WF, UK. Turpin Transactions Ltd, distributors, is wholly owned by The Royal Society of Chemistry September 1991 Hon. Treasurer T. B. Pierce ROYAL SoClETyOF CHEMISTRY lnformat ion Services

ISSN:0144-557X    

DOI:10.1039/AP99128FX033

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年代:1991

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ANPRDI 28(9) 281-308 (1 991) Proceedings of the Analytical Division of The Royal Society of Chemistry 281 Royal Society of Chemistry Awards 1990 281 Continuing Postgraduate Education in Analytical Chemistry 283 Analytical Viewpoint 283 'Some Recent Trends in Instrumental Analysis of Environmental Materials' by T. Braun and S. Zsindely 287 SUMMARIES OF PAPERS 287 Short Papers in Pharmaceutical Analysis 287 289 'Preliminary Investigations Into the Use of Supercritical Fluid Extraction to Extract a Novel Corticosteroid (Tipredane INN) From Rodent Diet' by Melvin R. Euerby, Richard J. Lewis and Steven C. Nichols 'Chromatographic Analysis of Novel Pharmaceutical Excipients for Liquid Filled Capsules' by Adam R. Hawley, Geoff Rowley, W. John Lough and Sarah M. Chatham 293 Research and Development Topics in Analytical Chemistry 293 294 297 Equipment News 303 Death 304 Conferences and Meetings 305 Courses 306 Publications Received 308 Analytical Division Diary 'Field Sampling Technique for Mercury Speciation' by Wei Jian and C. W. McLeod 'Sodium-selective Poly(viny1 chloride) Membrane Ion-selective Electrode Based on a Novel Calix[4]arene lonophore' by Kieran Cunningham, Gyula Svehla, Stephen J. Harris and M. Anthony McKervey September 1991 Analytical Proceedings CONTENTS Typeset and printed by Black Bear Press Limited, Cambridge, England

ISSN:0144-557X    

DOI:10.1039/AP99128BX035

出版商:RSC    

年代:1991

数据来源: RSC

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ANALYTICAL PROCEEDINGS, SEPTEMBER 1991, VOL 28 28 1 Continuing Postgraduate Education in Analytical Chemistry The Royal Society of Chemistry and the Royal Pharmaceutical Society both stress the importance of continuing education. This offers mid-career scientists the opportunity to update earlier training, acquire new skills, familiarize with newer or more sophisticated techniques, and even facilitate a change of direction or specialism. At the same time in the analytical community emphasis is growing on the following: the need for demonstrating credibility in test laboratory management systems, e . g . , through comprehensive accreditation schemes (such as NAMAS in the UK or HOKLAS in Hong Kong); ongoing demonstration of adequate skill in testing through proficiency schemes (such as AQUACHECK in the water provision industry and enforcement sector); establishment of nationally or internationally approved methodology through ring tests (as is supported by agencies such as the Codex Alimentarius and the Association of Official Analytical Chemists); and the provision of accepted values for standard reference substances and, where appropriate, natural matrix reference materials (notably the work in Europe of the Bureau Communautaire de Reference).All of these factors may be seen as key aspects of analytical quality assurance (AQA). They have been given particular focus in the UK by the Labora- tory of the Government Chemist through its ‘Validity of Analytical Measurement’ (VAM) programme, with financial sup- port and encouragement by the Depart- ment of Trade and Industry (for a sum- mary of the first 3 years work on the VAM programme, see Anal.Proc. ,1991, 28, 125). Because of the pressure of their man- agement responsibilities, and the difficul- ties consequent upon protracted absence from their workplace, middle grade science managers can profit from continu- ing education through ‘open learning’ schemes. Concurrent professional and governmental interest is also being shown in the particular value of open learning modules as another opportunity for in- service training. One particularly valu- able scheme in recent years has been the ACOL (Analytical Chemistry through Open Learning) programme developed as a series of stand-alone self correcting modules. Such considerations are especially valid in the pharmaceutical industry.A dramatic degree of sophistication has overtaken pharmaceutical analysis in the 20 years since implementation of the Medicines Act in the UK and monographs in national and world-regional pharmaco- poeias have made greater demands on technique and the supply of authentic reference substances. These factors, together with the increasing requirements of national registration authorities world- wide to ensure the safety, quality and efficacy of medicinal products, have placed a heavy responsibility on quality controllers for ensuring the adequacy and credibility of their analytical staff and the282 ANALYTICAL PROCEEDINGS, SEPTEMBER 1991, VOL 28 audit accessibility and general validity of their analytical measurements. Already, certain other aspects of con- tinuing education for scientists in the pharmaceutical industry have been addressed by an initiative of the Univer- sity of Manchester.Their Department of Pharmacy, in co-operation with the Industrial Pharmacists Group of the Royal Pharmaceutical Society, has gener- ated a Pharmaceutical Industry Advanced Training (PIAT) programme. Its objec- tive is to provide an integrated postgrad- uate portfolio for experienced industry staff that should meet ‘the requirements of industry and individual students for a cost-effective, flexible, high quality, industry recognized, continuing educa- tion programme’. The direct involvement of the University is to assure the quality of the programme and provide the facility, through acquisition of credits in sufficient modules, for achieving the award of University qualifications.It is also pos- sible to study one or more individual modules of value to student and employer without necessarily registering for a university postgraduate qualification. The topics addressed in 11 current modules include several aspects of pre- formulation studies, various presen- tations of dosage forms, manufacturing, quality assurance (of products), pack- aging and product registration. There are plans to add five more modules if evi- dence of industry interest is forthcoming. Analytical scientists should note that whereas existing Module 9 deals with the philosophy, organization and manage- ment of product quality assurance, one of the proposed five additional modules would be directed to an advanced treat- ment of analytical methods and equip- ment for examining drug substance and medicinal products.This clearly would go some way to meet the more general concern I have identified in appreciating modern demands of pharmaceutical analysis and its validation. The Joint Pharmaceutical Analysis Group (a subject group jointly sponsored by the Analytical Division and Pro- fessional Affairs Board of the RSC and by the Royal Pharmaceutical Society) has, through its committee of management, asked me to explore interest in this analytical module proposed for addition to the PIAT programme of postgraduate education. All members of the JPAG will receive a note with further details of the PIAT proposals, with a request to discuss these with relevant colleagues. They are asked then to send me a brief note by the end of September, indicating the degree of interest there would be in studying such a course, together with any specific suggestions of material they consider it important to include, or warnings of items to avoid. I plan to present a consolidated report to JPAG in late October. It may be that this initiative of the University of Manchester will evoke wider interest than just in the pharma- ceutical industry, and promote similar proposals in allied analytical sectors. Spe- cific comments on the PIAT analytical option should be addressed to me at LGC, while more extensive commen- taries or proposals would be welcomed by the Editor of Analytical Proceedings. Geoffrey F. Phillips Laboratory of the Government Chemist, Queens Road, Teddington, Middlesex

ISSN:0144-557X    

DOI:10.1039/AP991280281b

出版商:RSC    

年代:1991

数据来源: RSC

摘要:

ANALYTICAL PROCEEDINGS, SEPTEMBER 1991, VOL 28 283 Analytical Viewpoint The following is a member of a continuing series of articles providing either a personal view of part of one discipline in analytical chemistry (its present state, where it may be leading, etc.), or a philosophical look at a topic of relevance t o chemists in general or analytical chemists in particular. These contributions need not have been the subject of papers at Analytical Division Meetings. Persons wishing t o provide an article for publication in this series are invited t o contact the editor of Analytical Proceedings, who will be pleased to receive manuscripts or to discuss outline ideas with prospective authors. Some Recent Trends in Instrumental Analysis of Environmental Materials T. Braun*,t and S.Zsindelyt *Institute of Inorganic and Analytical Chemistry, L. Eotvos University, P.O. Box 123, 1443 Budapest, Hungary tlnformation Science and Scientometric Research Unit (ISSRU), Library of the Hungarian Academy of Sciences, Budapest, Hungary In our previous papers we have investigated recent trends in the use of instrumental analytical methods for trace metals' and organic analysis2 This paper is an evaluation of trends in the instrumental analysis of environmental materials. It is assumed that the open, formal journal literature contains the required raw data for determining the trends and tendencies in the fields which it c0ve1-s.~ We have computed the number of times the various instrumental analytical techniques were used to determine different components of environmen- tal matrices as reported in the AnalyticaE Abstracts4 database (1986-89).The data were then subjected to further manipulations. A classification of the various instrumental techniques according to the physical principles involved in the measure- ment process gave, according to the indexing rules of Analytical Abstracts, approximately 150 different instrumental techniques. Some of these overlap considerably. They were merged into seven groups (see Appendix). Two aspects of this approach should be noted. ( i ) The different instrumental techniques taken into account were selected on the basis of the subject index classification system of the Analytical Abstracts database; the same is true for the Table 1 Instrumental techniques used for analysing environmental matrix components, 1986-89.* All values in % OPT NUCL ELEC CHROM MISC HYPH CONV Air 37.8 10.4 5.4 37.4 0.9 7.1 1.0 Water 40.2 7.5 12.6 22.2 3.8 12.6 1.1 Effluent 30.5 6.6 10.9 25.4 4.7 19.8 2.1 Air Water Effluent OPT 27.7 65.5 6.8 NUCL 35.6 57.5 6.9 ELEC 14.6 76.4 9.0 CHROM 39.5 52.3 8.2 MISC 8.4 78.3 13.3 HYPH 17.3 68.0 14.7 CONV 23.2 59.7 16.1 *OPT = optical; NUCL = nuclear; ELEC = electrical; CHROM = chromatographic; MISC = miscellaneous; HYPH = hyphenated; and CONV = conventional.Table 2 Instrumental techniques used for analysing inorganic components in environmental matrices, 1986-89.* All values in % OPT NUCL ELEC CHROM MISC HYPH CONV Air 51.7 17.9 7.4 15.9 1.0 5.1 1.0 Water 45.2 9.3 14.7 11.9 4.4 13.3 1.2 Effluent 35.6 10.1 13.7 10.8 6.5 21.6 1.6 Effluent Water Air OPT 25.4 68.5 6.1 NUCL 35.8 57.1 7.1 ELEC 12.9 78.8 8.3 CHROM 28.1 65.2 6.7 MISC 6.1 80.3 13.6 HYPH 9.6 76.3 14.1 CONV 18.8 70.8 10.4 *Abbreviations as for Table 1.types of environmental matrices considered. (ii) Our analysis does not refer to the number of papers on instrumental analytical techniques but to the number of uses of these techniques; one paper can therefore refer to the use of many instrumental techniques. Table 3 Instrumental techniques used for analysing organic components in environmental matrices, 1986-89.* All values in % OPT NUCL ELEC CHROM MISC HYPH CONV Air 19.2 0.6 2.9 66.2 0.3 10.2 0.6 Water 23.7 1.1 5.4 57.1 1.7 10.7 0.3 Effluent 17.8 0.0 5.0 55.7 2.9 15.7 2.9 Air Water Effluent OPT 40.9 50.7 8.4 NUCL 36.4 63.6 0.0 ELEC 30.5 57.6 11.9 CHROM 48.7 42.2 9.1 MISC 11.8 64.7 23.5 HYPH 41.6 44.2 14.3 CONV 40.0 20.0 40.0 *Abbreviations as for Table 1.284 Results and Discussion Tables 1-5 present the results.In all the tables percentages sum up horizontally. Although the tables are self-explanatory, a few comments are in order. The upper part of Table 1 shows, for example, that in analysing environmental air samples, 37.8% of the total Table 4 Analysing environmental matrix components by different instrumental techniques, 1986-89.* All values in % OPT NUCL ELEC CHROM MISC HYPH CONV Ag A1 As Au B Ba Be Bi Br C Ca Cd Ce c1 c o Cr c s c u F Fe Ga Ge I In K Li Mn Mo N Na Ni 0 P Pb Pd Pu Rb Ru S Sb Se Si Sn Sr Te Th Ti T1 U V Y Zn Zr ME REE MEL aAs aC aCN aC1 aCr aN aP Hg Mg 64.7 17.6 5.9 53.6 8.7 8.7 54.7 18.8 9.4 100.0 0.0 0.0 47.1 5.9 5.9 44.4 14.8 7.4 60.9 0.0 4.3 58.3 4.2 20.8 13.3 20.0 6.7 25.0 16.7 8.3 32.7 23.6 1.8 52.1 7.8 19.4 14.3 42.9 0.0 21.8 6.9 19.8 44.5 10.9 15.5 45.0 18.3 12.5 28.6 57.1 0.0 50.4 6.9 20.2 23.9 2.2 28.3 45.2 21.0 7.3 80.0 20.0 0.0 75.0 0.0 0.0 56.0 13.0 14.0 21.1 13.2 18.4 60.0 20.0 0.0 35.1 24.3 8.1 44.4 0.0 0.0 37.1 11.4 5.7 56.0 10.3 10.3 37.5 12.5 16.1 47.6 4.8 0.0 30.4 21.7 0.0 43.9 10.8 20.9 44.4 5.6 27.8 54.3 5.7 0.0 54.2 6.7 20.6 83.3 16.7 0.0 22.2 66.7 0.0 12.5 75.0 0.0 40.0 40.0 0.0 26.9 11.5 7.7 56.5 13.0 15.2 54.4 19.3 10.5 64.7 29.4 0.0 63.6 9.1 9.1 30.4 30.4 4.3 100.0 0.0 0.0 26.7 53.3 0.0 24.0 24.0 8.0 50.0 3.8 19.2 32.0 32.0 16.0 35.8 17.0 11.3 14.3 28.6 0.0 45.8 11.4 17.5 27.3 36.4 0.0 41.3 10.9 17.4 28.6 28.6 14.3 32.4 27.1 6.4 88.9 0.0 0.0 12.5 0.0 12.5 47.1 0.0 14.7 41.2 0.0 41.2 40.0 0.0 0.0 43.1 0.0 5.4 47.7 4.5 9.1 0.0 4.3 6.3 0.0 0.0 7.4 13.0 4.2 36.7 16.7 18.2 6.0 0.0 25.7 15.5 6.7 14.3 6.9 32.6 5.6 0.0 12.5 10.0 18.4 0.0 16.2 33.3 22.9 4.3 3.6 14.3 30.4 6.5 11.1 11.4 3.4 0.0 11.1 12.5 0.0 23.1 2.2 5.3 0.0 0.0 8.7 0.0 13.3 0.0 3.8 10.0 3.8 0.0 6.6 0.0 13.0 0.0 13.8 11.1 37.5 20.6 0.0 60.0 36.2 22.7 0.0 11.8 2.9 21.7 0.0 10.9 0.0 0.0 0.0 41.2 0.0 22.2 0.0 21.7 0.0 12.5 3.3 16.7 12.5 16.7 3.6 18.2 0.5 13.8 0.0 42.9 14.9 5.9 1.8 11.8 2.5 15.0 0.0 0.0 2.8 12.5 8.7 2.2 4.0 16.1 0.0 0.0 0.0 12.5 2.0 5.0 7.9 21.1 0.0 20.0 2.7 13.5 0.0 22.2 5.7 14.3 3.4 14.7 3.6 26.8 19.0 4.8 0.0 17.4 0.7 17.3 5.6 0.0 11.4 17.1 1.3 13.4 0.0 0.0 0.0 0.0 0.0 0.0 0.0 20.0 7.7 19.2 0.0 13.0 1.8 8.8 0.0 5.9 0.0 18.2 0.0 26.1 0.0 0.0 0.0 6.7 4.0 40.0 0.0 23.1 2.0 6.0 5.7 26.4 0.0 57.1 0.6 18.1 0.0 36.4 2.2 15.2 0.0 28.6 3.2 16.0 0.0 0.0 12.5 12.5 11.8 0.0 5.9 0.0 0.0 0.0 12.3 2.3 11.4 2.3 0.0 0.0 0.0 0.0 0.0 3.7 0.0 0.0 3.3 4.2 1.8 0.5 0.0 5.0 0.0 0.0 0.0 0.4 2.2 0.8 0.0 0.0 0.0 0.0 0.0 0.0 0.0 2.9 0.9 0.0 9.5 0.0 0.0 5.6 0.0 0.4 0.0 0.0 0.0 0.0 3.8 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 2.0 0.0 0.0 0.0 0.0 0.0 0.0 1.1 0.0 12.0 5.9 11.8 0.0 0.8 2.3 ANALYTICAL PROCEEDINGS, SEPTEMBER 1991, VOL 28 Table 4 -continued OPT NUCL ELEC CHROM MISC HYPH CONV aS aSCN CH4 co COZ cos cs2 H20 H202 H2S HCl HF NH3 NO NO2 NO* 0 3 so2 cCa cN cs cSi ORG ORGHg ORGPb ORGSn PAH PCB IND 30.4 2.2 60.0 0.0 83.3 0.0 84.2 0.0 62.5 0.0 40.0 0.0 55.6 0.0 50.0 0.0 72.0 0.0 54.8 0.0 54.5 0.0 50.0 0.0 42.9 1.2 80.0 6.7 64.9 0.0 68.4 0.0 76.5 0.0 58.7 0.0 80.0 0.0 58.1 0.0 28.6 0.0 40.0 60.0 19.3 0.7 50.0 0.0 23.5 0.0 41.9 0.0 19.8 0.0 4.2 0.0 26.4 1.4 13.0 0.0 0.0 0.0 29.2 0.0 11.1 37.5 8.0 9.7 18.2 33.3 17.9 6.7 8.1 5.3 11.8 11.1 0.0 0.0 0.0 0.0 4.3 10.0 0.0 6.5 0.9 0.0 3.8 34.8 20.0 16.7 10.5 8.3 40.0 33.3 12.5 12.0 25.8 18.2 16.7 22.6 6.7 21.6 26.3 5.9 20.6 0.0 41.9 71.4 0.0 64.1 20.0 29.4 45.2 62.3 75.0 54.5 8.0 4.3 0.0 0.0 0.0 0.0 5.3 0.0 0.0 0.0 0.0 20.0 0.0 0.0 0.0 0.0 8.0 0.0 6.5 0.0 0.0 0.0 0.0 0.0 14.3 0.0 0.0 0.0 5.4 0.0 0.0 0.0 5.9 0.0 1.6 1.6 0.0 20.0 0.0 0.0 0.0 0.0 0.0 0.0 1.0 9.7 0.0 20.0 0.0 47.1 0.0 6.5 0.0 17.0 0.0 20.8 3.3 8.1 7.2 20.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 3.2 9.1 0.0 1.2 0.0 0.0 0.0 0.0 6.3 0.0 0.0 0.0 0.0 0.8 0.0 0.0 0.0 0.0 0.0 2.4 *a = anions of the elements(s) indicated; c = compounds of the element indicated but not mentioned individually; ME = metals; REE = rare earth elements; MEL = multi-element analysis; ORG = organic compounds without organometallics, PAH and PCB; ORG = organometallic compounds of the metal indicated; PAH = polycyclic aromatic hydrocarbons; PCB = polychlorinated biphenyls; IND = industrial products and wastes (oils, detergents, fertilizers, polymers, exhaust gases, etc.).No distinction has been made between metals and metal cations and between halogens and oxygen-free halogen anions. instrumental techniques used were optical, 10.4% nuclear, 5.4% electrical, etc. The lower part of Table 1 indicates, for example, that of the optical techniques used, 27.7% were dedicated to the analysis of air, 65.5% to the analysis of water, etc .In Table 1 it can be seen that optical methods and chromatographic techniques dominate the instrumental approach to analysing environmental samples. What is remark- able, however, is that hyphenated procedures are in third position. The distribution of instrumental techniques used for analysing the three types of environmental matrices indicates that water was the most frequently analysed matrix. The analytes determined were also considered separately; Table 2 indicates that the frequency ranking of instrumental techniques for inorganic analytes shows a different picture. Optical procedures, mainly the different variants of atomic absorption spectrometry, occupy rank 1.If we consider air samples, we see that nuclear techniques rank second. Hyphen- ated procedures are also extensively used but chromatographic techniques have not yet become established for determining inorganic analytes in environmental samples. However, gas chromatography is increasingly employed in air analysis, and ion chromatography for water and effluents. Chromatographic techniques clearly dominate in deter- mining organic analytes in environmental samples (Table 3). The almost negligible use of nuclear techniques for the same purpose comes as no surprise. When considering individual analytes (Table 4) we see that in the determination of trace metals, optical procedures are the most frequently used but forANALYTICAL PROCEEDINGS, SEPTEMBER 1991, VOL 28 285 some elements (Br, Ce, Cs, Rb, Sr, Th, U, Y, Zr and the rare earth elements) nuclear techniques still occupy first rank.For inorganic anions, chromatographic techniques compete with spectroscopic techniques, mainly due to the progress in ion- chromatographic techniques. The absolute dominance of chromatographic techniques is most obvious in the analysis of organometallic compounds and some highly toxic organic compounds, for example, polycyclic aromatic hydrocarbons and polychlorinated biphenyls (see Table 4). Regarding the frequency with which different types of Table 5 Analysing matrix components in environmental samples, 1986-89.* All values in % Ag A1 As Au B Ba Be Bi Br C Ca Cd Ce c1 co Cr cs Cu F Fe Ga Ge I In K Li Mn Mo N Na Ni 0 P Pb Pd Pu Rb Ru S Sb Se Si Sn Sr Te Th Ti T1 U V Y Zn Zr ME REE MEL aAs aC aCN Hg Mg Air 0.0 15.9 14.1 0.0 17.7 3.7 13.0 8.3 30.0 45.8 23.6 6.5 14.3 16.8 8.2 19.2 0.0 6.0 26.1 15.3 0.0 0.0 20.0 18.4 20.0 27.0 0.0 22.9 14.7 7.1 19.0 21.7 10.8 22.2 5.7 13.5 0.0 11.1 25.0 60.0 50.0 15.2 10.5 41.2 21.2 17.4 33.3 13.3 12.0 7.7 12.0 17.0 0.0 9.0 18.2 13.0 0.0 42.6 11.1 0.0 17.7 Water 100.0 78.3 78.1 100.0 82.3 77.8 78.3 91.7 63.3 50.0 67.3 83.4 85.7 76.3 87.3 59.2 100.0 85.5 69.6 77.4 60.0 100.0 63.0 79.0 80.0 62.2 100.0 77.1 78.4 91.1 52.4 78.3 77.0 77.8 65.7 78.1 100.0 88.9 75 .o 40.0 38.5 80.4 89.5 58.8 75.8 78.3 50.0 80.0 64.0 80.8 84.0 77.4 100.0 78.3 72.7 76.1 100.0 53.3 88.9 100.0 50.0 Effluent 0.0 5.8 7.8 0.0 0.0 18.5 8.7 0.0 6.7 4.2 9.1 10.1 0.0 6.9 4.5 21.6 0.0 8.5 4.3 7.3 40.0 0.0 17.0 2.6 0.0 10.8 0.0 0.0 6.9 1.8 28.6 0.0 12.2 0.0 28.6 8.4 0.0 0.0 0.0 0.0 11.5 4.4 0.0 0.0 3.0 4.3 16.7 6.7 24.0 11.5 4.0 5.6 0.0 12.7 9.1 10.9 0.0 2.1 0.0 0.0 32.3 Table 5-continued aC1 aCr aN aP aS aSCN CH4 co CO2 cos cs2 H20 H202 H2S HC1 HF NH3 NO NO2 NO, 0 3 so2 cCa cN cs cSi ORG ORGHg ORGPb ORGSn PAH PCB IND Air 11.8 0.0 20.8 6.8 20.3 0.0 83.3 94.7 66.7 100.0 88.9 87.5 44.0 83.9 100.0 100.0 46.4 93.3 97.3 100.0 70.6 92.1 100.0 83.9 100.0 60.0 46.6 20.0 47.1 3.2 64.1 25.0 19.6 *Abbreviations as for Table 4.Water 82.3 80.0 72.3 86.4 71.0 60.0 16.7 5.3 33.3 0.0 11.1 12.5 56.0 12.9 0.0 0.0 42.9 6.7 2.7 0.0 29.4 7.9 0.0 12.9 0.0 40.0 43.2 70.0 47.0 96.8 32.1 62.5 64.6 Effluent 5.9 20.0 6.9 6.8 8.7 40.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 3.2 0.0 0.0 10.7 0.0 0.0 0.0 0.0 0.0 0.0 3.2 0.0 0.0 10.4 10.0 5.9 0.0 3.8 12.5 15.8 environmental matrices are analysed, we see in Table 5 that inorganic components are mainly determined in water samples.Finally, Table 6 shows rankings of instrumental techniques on the basis of their reported use in analysing environmental matrices. Table 6 Instrumental techniques used for analysing inorganic and organic matrix components, 1986-89.* All values in % Compound OPT NUCL ELEC CHROM MISC HYPH CONV Inorganic 45.9 11.3 13.0 12.7 3.8 12.1 1.2 Organic 20.8 0.7 4.0 61.9 1.2 10.6 0.9 OPT 84.6 15.4 NUCL 97.6 2.4 ELEC 89.1 10.9 CHROM 33.8 66.2 MISC 88.6 11.4 HYPH 74.0 26.0 CONV 77.4 22.6 Inorganic Organic *Abbreviations as for Table 1. For inorganic analytes the ranking is: optical > electrical > chromatographic > hyphenated > nuclear > miscellaneous > conventional techniques.For organic analytes, the ranking is: chromatographic > optical > hyphenated > electrical > miscellaneous > conven- tional > nuclear. The above-mentioned results are in accordance with some evaluations5 and prognostications of the growth of the analytical instrument industry which have shown a bright commercial future for chromatographic, spectroscopic and hyphenated analytical instruments during the period 1980-90.286 ANALYTICAL PROCEEDINGS, SEPTEMBER 1991, VOL 28 The assistance of Lilian Vasvari in the data processing is gratefully acknowledged. References Braun, T., and Zsindely, S., Trends Anal. Chem., 1990,9, 144.Braun, T., and Zsindely, S., Trends Anal. Chem., 1990,9,309. Braun, T., Bujdosd, E., and Schubert, A., The Literature of Analytical Chemistry: A Scientometric Evaluation, CRC Press, Boca Raton, FL, 1987. Anal. Abstr., Royal Society of Chemistry, Cambridge, 1979-88. Wilkinson, G., The Analytical Instrument Zndustry in the 1980’s: Strategic Overview, 1980 . . . 1985 . . . 1990, SAMA Senior Management Conference, October 6-8, 1985, Amelia Island, FL, USA. APPENDIX Instrumental Analytical Techniques Optical methods. Colorimetry, photometry, turbidimetry , fluorimetry, ultraviolet, visible and infrared spectrometry, spectroscopy, polarimetry , mass spectrometry, nuclear mag- netic resonance spectrometry, X-ray spectrometry, X-ray diffractometry and related methods. Nuclear methods.Neutron-activation analysis, radiometry, gamma-spectrometry, X-ray fluorimetry and related methods. Electrical methods. Potentiometry , coulometry , ampero- metry, conductimetry, polarography , voltammetry and related methods. Chromatography. All types of chromatographic methods (gas-liquid, gas-solid, solid, gel, thin-layer, paper, capillary, ion chromatography and other related methods, including pyrolysis gas chromatography). Miscellaneous. Thermal methods (thermometry, thermo- gravimetry , enthalpimetry , calorimetry, etc. ), kinetic, enzymic methods, and methods which are not covered by any other group. ‘Hyphenated methods’. Combined instrumental methods , i. e., gas chromatography-mass spectrometry, etc. Conventional methods. ‘Classical’ analytical methods , i. e. , gravimetry, titrimetry (end-point indication with chemical indicators), extraction methods, pyrolysis (combustion meth- ods) , gas volumetry. The Sixth Biennial National Atomic Spectroscopy Symposium will be held at the Polytechnic South West, Plymouth tifh BNASS gfh BNASS 22-24 July 1992 The symposium will provide a forum where interesting and useful applications of atomic spectroscopy can be reported and discussed. In addition to plenary, invited and submitted lectures, a particular feature of the meeting will be the presentation of posters. There will also be an exhibition and a social programme for delegates and their guests. This meeting is organized by the Atomic Spectroscopy Group, Analytical Division of The Royal Society of Chemistry. Further information can be obtained from the Chairman of the organizing committee: Dr S Hill, Department of Environmental Sciences, Polytechnic South West, Drake Circus, Plymouth, Devon PL4 8AA, UK.

ISSN:0144-557X    

DOI:10.1039/AP9912800283

出版商:RSC    

年代:1991

数据来源: RSC

摘要:

ANALYTICAL PROCEEDINGS, SEPTEMBER 1991, VOL 28 287 Short Papers in Pharmaceutical Analysis The following are summaries of two of the papers presented at a Meeting of the Joint Pharmaceutical Analysis Group held on October 18th, 1990, in the Royal Pharmaceutical Society of Great Britain. Preliminary Investigations into the Use of Supercritical Fluid Extraction to Extract a Novel Corticosteroid (Tipredane INN) From Rodent Diet Melvin R. Euerby, Richard J. Lewis and Steven C. Nichols Analytical Chemistry, Research and Development Laboratories, Fisons Pharmaceuticals plc, Bakewell Road, Loughborough, Leicestershire LE 1 I ORH The principle of supercritical fluid extraction (SFE) has been known for over 100 years. 1 However, only relatively recently has its potential use in analytical chemistry been recognized.2-5 SFE can offer many advantages over more traditional extrac- tion techniques such as: (i) reduced sample preparation time; (ii) ease of separation of the analyte from the supercritical fluid (SF); (iii) fractionation during collection; and (iv) potential compatibility with on-line analysis techniques.This paper describes the preliminary results relating to the optimization of SFE conditions in order to extract a novel corticosteroid (tipredane INN, Fig. 1) at a level of 10 ppm from SCH3 Fig. 1 Tipredane INN a complex matrix, rodent diet, which is a complete and balanced food source. The optimized extraction has been compared with the more conventional extraction procedures of Soxhlet and ultrasonic agitation. Reagents All solvents used were Fisons high-performance liquid chro- matography (HPLC) grade, except the dichloromethane which was Fisons specified-reagent grade.The COZ (industrial grade) was supplied by BOC. The diet was supplied by Special Diet Services, product number R/M 1(E) SQC F.G. Equipment The SFE system consisted of two Jasco 880-PU HPLC pumps; the head of one was cooled to -20 "C using fluid from a Techne tempette TE-8A cooling bath. Extractions were carried out in a Jasco 860-CO column oven and were followed at 240 nm with a Jasco 875-UV (ultraviolet) detector connected to an ABB SE120 chart recorder. A Jasco 880-81 back-pressure regulator (BPR) was used to control the pressure of the SF in the system. Jasco 1 ml extraction cells were used to contain the diet. Methods Preparation of Diet Standards The spiked diet was produced by mixing tipredane with the diet in a pestle and mortar using increasing portions of diet until a 10 ppm mixture was produced.General SFE Extraction A typical extraction was carried out as follows. About 0.7 g of the spiked diet mixture was weighed into the extraction cell. The cell was closed and connected in the oven and the temperature allowed to settle. The sample was extracted for 2 min, then the system alone flushed with the SF for 1 min. The extracts were collected in a 5 ml calibrated flask containing about 1 ml of methanol through which the expanded gases were passed. The extracts were allowed to warm to room tempera- ture and the contents of the flask made up to volume with methanol before HPLC analysis.HPLC Analysis The HPLC analysis was performed on a Hewlett-Packard 1090M chromatography system. The separation was achieved with a NovaPak CI8 column using a mobile phase of 0.025 mol dm-3 KH2P04 in 60% acetonitrile. The recovery was calculated on the basis of the mass of diet used and the expected concentration of tipredane in the diet. The average of two extractions under each of the conditions is given in the results tables. Soxhlet Extraction Soxhlet extraction was performed on about 2 g of diet using 100 mi of methanol. After 6 h the solvent was removed in vacuo and the residue washed into a 5 ml calibrated flask using Table 1 Comparison of different modifiers. Extraction conditions: pressure, 180 kg cm-*; oven temperature, 70°C; C 0 2 flow rate, 3.0 ml min-l; modifier flow rate, 0.3 ml min-1; BPR temperature, 40°C; and collection time, 2 min Modifier* Recovery (%) Dichloromethane 77 Acetone 83 Ethanol 82 Acetonitrile 82 Ethanol-water (50 + 50) 48 * Arranged in order of increasing polarity based on the relative permittivity.'288 ANALYTICAL PROCEEDINGS, SEPTEMBER 1991, VOL 28 methanol.After making up to volume, the sample was analysed as described above. Ultrasonic Extraction About 2 g of diet were ultrasonicated with 20 ml of methanol for 30 rnin in a conical flask. The solvent was removed, and the process repeated with further solvent. The two extracts were filtered and combined, the solvent was removed in vacuo and then the residue treated as described above. Results and Discussion In theory, the collection of the analyte is straightforward, as evaporation of carbon dioxide (C02) after decompression should yield the analyte, alleviating the necessity of a separate concentration step.However, the evaporation of the C02 and the subsequent collectiodtrapping of the analyte can be problematical,3.4 in that analyte losses can be incurred via analyte entrainment in the vaporizing C02 and through loss of volatile analytes. A number of collection methodologies were investigated; these varied from adsorption of the tipredane on to an on-line CI8 silica guard column, to trapping all of the eluent by freezing with liquid nitrogen, with the subsequent slow natural evapora- tion of the COz at -18°C. The most efficient and convenient collection method was found to be direct collection from the BPR through a short length- of poly(tetrafluoroethy1ene) (PTFE) tubing into a calibrated flask containing about 1 ml of methanol; the flask was stoppered with a small piece of cotton wool to trap any spray that might be lost.The cotton wool was rinsed into the flask after the extraction was complete. Supercritical C02 alone has a very low polarity, and when extracting moderately polar molecules, a suitable organic modifier needs to be added.4.6 In the extraction of tipredane, the use of C02 alone was found to give low or zero recoveries and, therefore, the use of different modifiers was investigated. The results (Table 1) suggest that a modifier of intermediate polarity gives optimum recovery. On the basis of recovery, efficiency and toxicity, ethanol was chosen for further investi- gations.The flow rate of ethanol was altered, keeping the C02 flow rate constant. The results (Table 2) show the optimum ethanol flow rate; this value probably reflects the optimum polarity for the SF and the optimum collection efficiency.3.8 It is interesting that the use of ethanol alone gives a lower recovery than C02 modified with ethanol. This is probably a reflection of the benefits of the use of an SF over liquid, i.e., that the SF has a higher diffusivity and lower viscosity and, therefore, is better able to penetrate the extraction matrix. The time course of the extraction was followed by collecting extractants for different times between 0.5 and 10 min. The results showed no significant difference between the recoveries, indicating that extraction was very rapid and occurred within 0.5 rnin under these conditions [average recovery = 84%, relative standard deviation (RSD) = 6% , n = 16 (for eight different collection times).The extraction conditions were as follows: pressure, 200 kg cm-2; oven temperature, 45 "C; C02 flow rate, 3.0 ml min-1; ethanol flow Table 2 Comparison of ethanol flow rates. Extraction conditions: pressure, 180 kg cm-2; oven temperature, 70°C; C02 flow rate, 3.0 ml min-1; BPR temperature, 40 "C; and collection time, 2 rnin Ethanol flow rate/ml min-1 Recovery (Yo) 0.00 0.17 0.33 0.50 0.67 1.00" * C02 flow rate, 0 ml min-1. 0 83 88 83 76 55 Table 3 Effect of extraction temperature. Extraction conditions: pressure, 200 kg cm-2; C02 flow rate, 3.0 ml min-l; ethanol flow rate, 0.3 ml min-1; BPR temperature, 40°C; and collection time, 2 rnin TemperaturePC Recovery (YO) 35 81 45 84 60 87 80 87 rate, 0.3 ml min-1; and BPR temperature, 40"CI.Neverthe- less, a collection time of 2 rnin for the optimum recovery was employed to allow for changes in the extraction rates under different conditions. The effect of oven temperature is shown in Table 3. The change of extraction efficiency is not sufficiently large to be significant. However, a general trend of increased recovery with increased temperature was observed, rather than a decrease, which might have been expected as the solubility of a component in an SF decreases with increasing temperature.9 This suggests that the extraction is not limited by the solubility of tipredane in the SF, but rather by the rate at which the tipredane can dissolve.An increase in temperature would have two effects that might increase the rate of solution: firstly, an increase in the diffusivity of the substance in the matrix, and secondly, a decreased viscosity of the SF (meaning that it can penetrate the matrix more easily). The temperature at the BPR can also be controlled, but variations of between 35 and 80 "C were found not to affect the efficiency of recovery (data not shown). Unexpectedly, there was no change in the efficiency of the extraction of tipredane from the diet, on varying the pressure at which the SFE was performed. As an increase in SF pressure should, theoretically, increase the solubility of the tipredane in the SF, this further supports the proposal that the extraction is not limited by the solubility of tipredane in the SF.The effect of total flow on the extraction was investigated, keeping the ethanol at a constant proportion of 9% of the total flow. The results shown in Table 4 indicate that a maximum recovery of tipredane was achieved on performing the extrac- tion at a 3.0 ml min-1 C02 flow rate. At higher flow rates, the decreased recovery is probably due to less efficient trapping of the ex tractan ts. Table 4 Effect of C02 flow rate. Extraction conditions: pressure, 200 kg cm-2; oven temperature, 45 "C; ethanol flow rate, 10% of C02 flow rate; BPR temperature, 40°C; and collection time, 2 rnin c02 flow rate/ml min-1 Recovery (YO ) 1 .o 2.0 3.0 4.0 6.0 8.0 76 80 84 83 82 67 By using the optimized SFE conditions (Table 5 ) , compar- able tipredane extraction efficiencies, as compared with ultrasonic agitation and Soxhlet extractions, were obtained from the complex matrix of rat diet.The advantage of SFE in this application is that the extraction is rapid and no separate concentration step is required; hence, the time per unit analysis is reduced. For example, typical unit sample preparation times for SFE, ultrasonic and Soxhlet extraction were 20 min, 2 h and 7 h , respectively. These investigations have demonstrated the applicability of SFE to the extraction of a steroid from a complex matrix. The sample preparation time is drastically reduced compared with conventional extraction methods. The preliminary results have demonstrated that the choice and amount of modifier and flowANALYTICAL PROCEEDINGS, SEPTEMBER 1991, VOL 28 289 Table 5 Comparison of extraction methods SFE* Ultrasound Soxhlet Average recovery (%) 85 92 94 Range (YO) 75-95 89-95 88-100 RSD (Yo) 6 3 6 n 12 6 4 * Extraction conditions: pressure, 150-200 kg cm-2; oven tempera- ture, 70°C; C02 flow rate, 3.0 ml min-'; ethanol flow rate, 0.3 ml min-1; BPR temperature, 40°C; and collection time, 2 min.~~ ~ ~ rate are the most important parameters in determining the extraction efficiency of tipredane from the rodent diet. With further improvement in instrumentation, such as automation, SFE should become an established technique in the analytical laboratory. We thank Dr. G. E. Taylor and P. Rowan for performing some of the ultrasonic extractions.References McHugh, M. A., and Krukonis, V. J., Supercritical Fluid Extraction: Principles and Practice, Butterworths, Boston, 1986, ch. 2. McHugh, M. A., and Krukonis, V. J., Supercritical Fluid Extraction: Principles and Practice, Butterworths, Boston, 1986, ch. 10. Vannoort, R. W., Chervet, J.-P., Lingeman, H., DeJong, G. J., and Brinkman, U.A.Th., J. Chromatogr., 1990, 505, 45. Hawthorne, S. B . , Anal. Chem., l990,62,633A. Berry, V . , LC-GC Int., 1990,3,56. Janicot, J . L., Caude, M., Rosset, R., and Veuthey, J. L., J. Chromatogr., 1990,505,247. Isaacs, N. S. , Physical Organic Chemistry, Longman, Harlow, 1987, p. 180. Wright, B. W., Wright, C. W., Gale, R. W., and Smith, R. D . , Anal. Chem., 1987, 59, 38. McHugh, M. A ., and Krukonis, V. J . , Supercritical Fluid Extraction: Principles and Practice, Butterworths, Boston, 1986, ch. 1. Chromatographic Analysis of Novel Pharmaceutical Excipients for Liquid Filled Capsules Adam R. Hawley, Geoff Rowley and W. John Lough School of Pharmaceutical and Chemical Sciences, Sunderland Polytechnic, Tyne and Wear Sarah M. Chatham Lilly Research Centre, Windlesham, Surrey Hard gelatin capsules can be filled with a molten drugexcipient mixture which solidifies on cooling in a capsule shell. Proved advantages of this system over powder filled capsules are numerous, including improved fill mass uniformity, elimina- tion of dust hazards during filling and improved protection against oxidation and humidity. Novel excipients with suitable physico-chemical properties were investigated and here one aspect of their chemical characterization is described.After favourable preliminary findings, Dynasan-114 (a myristic acid triglyceride, Fig. 1) and Dynafill (a polyethylene oxide-poly- propylene oxide block copolymer with palmitic acid end groups, Fig. 2) were selected for more detailed examination. H I ?\ H-C-O-C-( CH 2 11 2 - CH3 H Fig. 1 Chemical structure of Dynasan-114 A = palmitic acid end groups B = ethylene oxide groups C = propylene oxide groups x = number of ethylene oxide units y = number of propylene oxide units Fig. 2 Chemical structure of Dynafill Future processing of the two materials, Dynasan-114 and Dynafill, will involve melting and recrystallization, and the presence of impurities in molten systems can affect crystal form on solidification as can the rate of cooling from the molten state.It is necessary therefore to differentiate between any crystal change induced by impurities and those due to a change in the cooling rate. Moreover, a high temperature challenge of the two compounds, Dynasan-114 and Dynafill, could lead to degradation and release of fatty acids as breakdown products. Any fatty acid impurites likely to occur in these materials might be present either as triglycerides or as free fatty acids. Accordingly, the levels of each of these types of impurities must be quantified. Chromatographic analysis of fatty acids can be carried out by esterification to the methyl followed by capillary gas chromatography (GC). Alternatively, the acid can be esteri- fied with a marker chemical (with ultraviolet or fluorescence properties) and then analysed by high-performance liquid chromatography (HPLC).3" The former method is relatively simple.On the other hand, the latter can be more complex but is usually very sensitive7 and is therefore useful for detection of trace amounts of fatty acids. In another HPLC technique the untreated fatty acids were separated followed by post-column derivatization and ultraviolet detection.* Further examples of fatty acid separation without derivatization have been de- scribed in the literature; however, because of mobile phase solubility problems for Dynasan-114 and Dynafill, direct injection of sample solutions would not have been possible. A comparison of capillary GC and HPLC9 in the analysis of fatty acids showed that the former was preferable for the separation of fatty acid derivatives extracted from plasma (better resolution was achieved, thus allowing quantification of all the fatty acids of interest).The aim of this exercise, however, was to obtain quantitative results for free fatty acid and fatty acids as part of two different substances, Dynasan-114 and Dynafill, at concentrations of approximately 1%. As the GC method alone would not differentiate between these two290 ANALYTICAL PROCEEDINGS, SEPTEMBER 1991, VOL 28 types of impurity it was necessary to develop two separate analytical methods. An esterification technique involving established methods with minor modifications was used to evaluate total fatty acid by capillary GC; secondly, a novel HPLC analysis without preparatory steps was developed for detection of free fatty acid impurity.Experimental Determination of Fatty Acid Esters and Free Fatty Acids by Capillary GC Derivatization For the measurement of total fatty acid, samples were derivatized to their methyl esters. Sample masses for analysis were adjusted so as to contain an equivalent of 50 mg of free fatty acid. This required a knowledge of the relative molecular mass and chemical structure of the samples under analysis. The relative molecular mass of Dynasan-114 is 722; the relative molecular mass of Dynafill is unknown, but previous work suggested an estimate of 10 000 would be suitable. Each sample was dissolved in 10 ml of freshly prepared 2% NaOH (Merck, Poole, Dorset, UK) in methanol (analytical-reagent grade; Fisons, Loughborough, Leicestershire , UK) and the mixture refluxed for 15 min.A 2 ml volume of concentrated H2S04 (May and Baker, Dagenham, Essex, UK) was then added and the mixture refluxed for a further 30 min. The mixture was then cooled, 20 ml of distilled water were added and the organic content was extracted with analytical-reagent grade heptane (Fisons) . After drying over anhydrous magne- sium sulphate, a sample was removed for GC analysis. Equipment An SGE fused silica capillary column (25 m x 0.25 mm i.d.) was used in a Shimadzu GC-9A programmable oven (Dyson Instruments, Houghton-le-Spring, Tyne and Wear, UK) linked to a flame-ionization detector and a Shimadzu C-R4A integra- tor (Dyson Instruments). Injections were made on-column by using an SGE 5 pl syringe, steel needle and an SGE-OC13 on- column injection port.The carrier gas was helium and a temperature programme was employed starting at 100 "C and increasing to 200 oc at a rate of 20 "C min-'. The run time was 5 min and the injection volume was 1.0 pl. Calibration solutions of lauric, myristic, palmitic and stearic acid methyl esters were prepared by using the multiple internal standard technique with methyl tridecanoate as the internal standard. All injections were carried out a minimum of four times. The esters and fatty acids used were all purchased from Sigma (Poole, Dorset, UK) (except for myrisic, palmitic and stearic acids which were obtained from Merck) and all were at least 99% pure. Determination of Free Fatty Acid by HPLC Equipment The microbore column (Capital HPLC Specialists, Bathgate, West Lothian, UK) (100 x 2.1 mm i.d.) was packed with porous graphitic carbon (PGC), and from the limited range of solvent systems examined, a mixture of hexane (Fisons, HPLC grade) and isopropyl alcohol (IPA) (99.6 +0.4) was chosen as the mobile phase.The pump used was a Shimadzu LC-6A linked to a Shimadzu C-R5A integrator; the detector was a Shimadzu SPD-6AV (all Dyson Instruments). The injection volume was 20 p1 via a Rheodyne injection port. The ultraviolet detection wavelength was 211 nm, the flow rate 0.5 ml min-' and the run was completed after 6 min. The fatty acids used in this analysis were of the same grade as those used for the capillary GC analysis.A mixture of the four fatty acids (lauric, myristic, palmitic and stearic acids) most likely to be present as impurities in Dynasan-114 or Dynafill was prepared as a test mixture for the development of this analysis. Calibration solutions of lauric, myristic and palmitic acids with stearic acid as the internal standard were run on this system and a linear response was obtained over the concen- tration range 0.02-0.3 mg mi-' ( r B0.9995). Stearic acid was chosen as the internal standard. Apart from the calibration solutions two samples were analysed: Dynasan-114 with internal standard and Dynafill with internal standard. Samples were dissolved in mobile phase and all injections were performed in triplicate. Results and Discussion Capillary GC It was found that the fatty acids were esterified to different extents which decreased with increasing relative molecular mass.After an investigation of the esterification conditions it was shown that more thorough conditions (as described under Experimental) were necessary to give satisfactory results. Therefore, in addition to the samples of Dynasan-114 and Dynafill, a mixture of lauric, myristic, palmitic and stearic acids of known composition was examined and the relative extent of esterification was calculated. All the fatty acids were esterified to the same extent (<+1%). Tridecanoic acid (C13) was chosen as the internal standard as its chain length was within the range under investigation (C12- C18); in addition, it is unlikely that a carbon chain of odd number would be present in a material of vegetable origin such as Dynasan-114.Satisfactory linear responses were obtained with the calib- ration standards (all values of r >0.9999). Excellent separation was obtained from the GC results (Fig. 3) with good peak shape when the five methyl esters were injected. Initially, when sample solutions of Dynasan-114 were injected only two peaks were observed: methyl myristate, the known fatty component; and methyl tridecanoate, the internal standard (Fig. 4). Closer inspection of these solutions using higher attenuation settings revealed additional peaks with retention times comparable to those of lauric and palmitic acid methyl esters, indicating the presence of impurities in Dyna- san-114 but at levels which could not be reliably quantified in 0 1 2 3 4 5 Time/mi n Fig.3 Capillary GC of methyl ester mixtures. Peaks from left to right: methyl laurate, methyl tridecanoate, methyl myristate, methyl palmi- tate, methyl stearate this exercise and therefore less than 0.7%0, the limit of the quantification. Injection of Dynafill also resulted in only two peaks: methyl palmitate; and methyl tridecanoate, the internal standard (Fig. 5). Closer inspection at higher attenuation gave no indicationANALYTICAL PROCEEDINGS, SEPTEMBER 1991, VOL 28 L, 29 1 of trace contamination. It can be concluded that Dynafill is not contaminated with other fatty acids at concentrations >0.7%, the limit of quantification of the method. HPLC Examination of free fatty acid separation on the carbon column by injection of the free fatty acid mixture did not achieve complete resolution (Fig.6); however, a linear response was achieved over the calibration range. A wide variety of mobile phases were examined in order to achieve optimum resolution while attempting to retain acceptable peak shape. The mobile phase had to be very non-polar, otherwise precipitation of the sample resulted. A flow rate gradient was studied and rejected as there was no improvement in reproducibility. Certain solvents such as methanol and phosphate buffer were unaccep- table as they resulted in precipitation of the Sam le even at low concentrations; hence a documented method' could not be used. When the samples of Dynasan-114 and Dynafill were injected onto the carbon column, both produced peaks but with retention times that did not match those of the free fatty acids.From these results it was concluded that free fatty acids were not detected in either sample down to the limit of quantifica- tion of this method, i.e., 0.2% m/m. The trace impurity peaks in the capillary GC method for Dynasan-114 must therefore arise from fatty acid substitution in the Dynasan-114 molecule itself and not from free fatty acid contamination. By using a combination of these two analytical methods it was established that both Dynasan-114 and Dynafill are relatively free from fatty acid impurities, which is advan- tageous if these materials are to be used in pharmaceutical sys tems. In spite of the fact that low efficiency and only partial resolution were obtained with this HPLC technique, it has proved to be a valid and reasonably sensitive technique for the determination of free fatty acids.Improvement in resolution might be achieved by further investigation of: ( a ) a solvent gradient of increasing IPA (as higher concentrations of IPA would elute the later peaks faster and hence improve their shape); and ( b ) starting with a slow pump speed and steadily increasing it with time might improve the resolution of the 8 u 0 1 2 3 4 5 Time/min Fig. 4 Capillary GC of esterified Dynasan-114. Peaks from left to right: methyl tridecanoate, methyl myristate initial two peaks. The latter change would shorten the run time and produce narrower and therefore more easily quantifiable peak widths. Columns of conventional internal diameter (4.6 mm) can be more efficiently packed with PGC and therefore might give better peak shape and resolution.This might also be achieved by using Hypercarb (Shandon Southern 0 1 2 3 4 5 Timehi n Fig. 5 Capillary GC of esterified Dynafill. Peaks from left to right: methyl tridecanoate, methyl palmitate Products, Runcorn, Cheshire, UK), an advanced commercially available form of PGC. These options are now being investi- gated. Nevertheless, this method as it stands is one of very few techniques with such simple conditions for achieving free fatty acid separation in the presence of fatty acid triglycerides and is apparently the only technique developed to date for these particular materials. Conclusion The use of the above two techniques in combination provides a rapid and simple evaluation of the principal fatty acids present 0.0 1.0 2.0 3.0 4.0 5.0 6.0 Timehin Fig.6 HPLC of fatty acid mixture. Peaks from left to right: lauric acid, myristic acid, palmitic acid, stearic acid as myristate in Dynasan-114 and palmitate in Dynafill, in addition to any free fatty acids present as impurities. The HPLC technique described here can be applied to almost any system where quantification of small amounts of free fatty acid is indicated, provided the bulk material is compatible with the system and there is no direct overlap of fatty acid peaks and bulk material peaks. The capillary GC system could be applied to a wide variety of commercially available materials similar to292 ANALYTICAL PROCEEDINGS, SEPTEMBER 1991, VOL 28 Dynafill and also to other grades of Dynasan-114, or indeed to a wide range of unrelated triglycerides of mixed fatty acid composition. The composition of Dynasan-114 and Dynafill is now well defined and this will aid the interpretation of results from thermal analysis in relation to the crystallization and stability of the materials. The method can be used to investigate batch variability with respect to fatty acid impurities as the latter can affect the capsule filling process in addition to the structure and stability of the drugexcipient system. References 1 Arrendale, R. F., Chapman, G. W., and Chortyk, 0. T., J . Agric. Food Chem., 1983,31, 1334. 2 3 4 5 6 7 8 9 10 Brengartner, D. A., Anal. Chim. Acta, 1985, 173, 177. Tsuchiya, H., Hayashi, T., Sato, M., Tatsumi, M., and Takagi, M., J. Chromatogr., 1984, 309, 43. Shimomura, Y., Taniguchi, K . , Sugie, T., Murakami, M., Sugiyama, S . , and Ozawa, T., Clin. Chim. Acta, 1984,143,361. Wetzel, D. L., Wheling, R. L., Lee, M. J . , andTweeten, T. N., Dev. Food Sci., 1986, 12, 667. Yamaguchi, M., Matsunaga, R., Fukuda, K., Nakamura, M., and Ohkura, Y., Anal. Biochem., 1986, 155, 256. Hatsumi, M., Kimata, S., and Hirosawa, K., J. Chromatogr., 1986, 380, 247. Lawrence, J. F., and Charbonneau, C . F., J . Chrornatogr., 1988, 445, 189. Baty, J . D., Willis, R. G., andTavendale, R., J . Chromatogr., 1986, 353, 319. HPLC Technology Column Catalogue 1987-88, HPLC Tech- nology, Macclesfield.

ISSN:0144-557X    

DOI:10.1039/AP9912800287

出版商:RSC    

年代:1991

数据来源: RSC

摘要:

ANALYTICAL PROCEEDINGS, SEPTEMBER 1991, VOL 28 293 I-' HCI -Br03- SnCI2 Research and Development Topics in Analytical Chemistry - The following are summaries of two of the papers presented at a Meeting of the Analytical Division held on July 16th-17thr 1990, in ICI C and P Ltd., Runcorn, Cheshire. Summaries of fourteen other papers appeared in the January (p. 8), February (p. 37) and March (p, 82) issues. Field Sampling Technique For Mercury Speciation Wei Jian* and C. W. McLeod Chemical Analysis Research Centre, Sheffield City Polytechnic, Sheffield S1 1 WB There is a continuing need to improve our understanding of mercury transport and cycling in the biosphere on account of the toxicity of mercury. As is well known, organomercury compounds and particularly methylmercury are highly toxic relative to inorganic forms and hence analytical methodology capable of differentiating between the various species is essential.Many approaches have been reported for the determination and speciation of mercury and include: cold- vapour atomic absorption spectrometry with selective chemical reductan ts, 1 chromatographic methods based on gas chrornato- graphy2 and high-performance liquid chromatography,3 sol- vent extraction and inductively coupled plasma mass spec- trometry ,4 and electrochemical separation and atomic absorp- tion spectrometry.5 Recently, flow injection atomic fluores- cence spectrometry (FI-AFS) with microcolumn separation has been proposed as a novel speciation technique.6 In this latter approach a microcolumn of sulphydryl cotton is incorporated in the FI system to effect on-line separation of organomercury and inorganic mercury species.With reference to mercury in natural waters, reliable speciation data are scarce. This is partly because of the extremely low concentration of individual species (ng I-*) but also is a reflection of the difficulty, after sampling, of maintaining the natural speciation state until analysis is performed. As is often practised in official monitoring pro- grammes for mercury, speciation data are actually destroyed at the sampling site (addition of powerful oxidants to sample) and only total Hg data are reported. In the present work a field sampling technique has been developed to collect and preserve organomercury species. Water samples, on collection, are processed by passage through a microcolumn of sulphydryl cotton.The microcol- umns with retained analyte are then returned to the laboratory and incorporated in an FI-AFS system for elution and quantitative analysis. Preliminary studies for synthetic solu- tions and river water testify to a potentially valuable new speciation tool. S n I 0.1 mol Br- b) - Time Fig. 2 Fluorescence versus time responses for (a) 2.5 pg 1-I MeHgCl solution; ( b ) 2.0 pg I-* inorganic Hg solution; and (c) 2.5 pg 1-1 MeHgCl and 2.0 pg 1-1 inorganic Hg mixed solution. E = Injection of eluent Experimental The field sampling kit consisted of an on-line filter (0.45 pm, Anachem), a sulphydryl cotton microcolumn (5 cm X 1.5 mm i.d.) and a syringe (10 ml capacity). The sample solution on collection was adjusted to pH 3 4 with concentrated hydro- chloric acid (BDH, Aristar).Specified sample volumes (typic- ally 2-10 ml) were passed through the microcolumn twice by syringe action ( i . e . , fill and rinse sequence) to ensure retention of organomercury species (inorganic Hg not retained). The microcolumns were then disconnected, placed in a light-tight box and returned to the laboratory. Microcolumns were inserted into the FI-AFS system as shown in Fig. 1. The analysis procedure consisted of injection of hydrochloric acid (0.5 ml, 3 moll-1; BDH, Aristar) to elute retained organomercury species. Bromide-bromate reagent was used to convert organomercury into inorganic mercury and downstream merging with tin chloride generated elemental mercury for detection by cold-vapour AFS.Performance Fig. 1 FI-AFS system294 ANALYTICAL PROCEEDINGS, SEPTEMBER 1991, VOL 28 Results and Discussion In order to test the suitability of sulphydryl cotton for collection and preservation of methylmercury, initial exper- iments were performed in the laboratory using synthetic aqueous solutions. Solutions of methylmercury chloride (2.5 pg 1-1 MeHgCl= 2.0 pg 1-1 Hg), mercury(1r) (2.0 pg 1-1 Hg) and methylmercury chloride-mercury(i1) (2.5 pg 1- 1 MeHgC1- 2.0 pg 1-1 Hg) were subjected to field sampling and analysis (as described under Experimental) and typical responses are given in Fig. 2. The results indicated that methylmercury, in contrast to inorganic mercury, was retained by the sulphydryl cotton microcolumn and after incorporation in the FI system under- went desorption and additional post-chemical reactions before AFS detection. Hence field sampling in combination with AFS, by virtue of the separation of inorganic and organomer- cury, provided speciation information.- Time Fig. 3 Fluorescence response for river water after field sampling. E = injection of eluent An important operational feature of field sampling is the built-in trace enrichment capability, i.e., by processing rela- tively large sample volumes (e.g., 1G20 ml), method sensi- tivity is improved and determinations at and below the ng 1-1 level become possible. Field sampling was performed at an official sampling station on a polluted river in south Yorkshire. Water samples (5 ml) were processed in duplicate and microcolumns were returned to the laboratory for measurement, there being a delay of about 4 h between sampling and analysis. The FI responses shown in Fig.3 confirm the presence of significant concentra- tions of methylmercury and the feasibility of this new analytical methodology in natural water systems. The river water was also subjected to oxidation by bromide-bromate reagent, before and after filtration, in order to provide complementary data on mercury content. The results are summarized in Table 1 and indicate, as expected, that a major fraction of mercury was associated with colloidal/particulate matter. The data further indicate that the contribution of methylmercury to the dis- solved fraction was significant. Table 1 Determination of Hg in river water.All values in pg 1-l This work* Conventional analysis? Methylmercury Dissolved mercury Total Hg (2) 6.87 (1) 6.50 (1) (2) (1) (2) 0.230 0.226 0.207 0.198 * Field sampling-FI-AFS. 1- FI-AFS. A pilot study concerning methylmercury concentrations in south Yorkshire rivers is underway and new data together with information on microcolumn storage and stability will be reported shortly. We thank PS Analytical for collaboration and support for the project. References 1 Oda, C. E., and Ingle, J. D., Jr., Anal. Chem., 1981, 53,2305. 2 Official Methods of Analysis of the Association of Official Analytical Chemists, Association of Official Analytical Chemists, Arlington, VA, 15th edn., 1990, pp. 266-269. 3 Bushee, D. S., Analyst, 1988, 113, 1167. 4 Beauchemin, D., Siu, K.W. M., and Berman, S. S., Anal. Chem., 1988,60,2587. 5 ErguGyener, C., Aygun, S., Ataman, 0. Y., and Temizer, A., J. Anal. At. Spectrum., 1988, 3, 177. 6 McLeod, C. W., and Jian. W., Spectrosc. World, 1990. 2, 32. Sodium-selective Poly(viny1 chloride) Membrane Ion-selective Electrode Based on a Novel Calix[4]arene lonophore Kieran Cunningham and Gyula Svehla Department of Chemistry, University College Cork, Cork, Ireland Stephen J. Harris Research and Development, Loctite (Ireland) Ltd., Whitesto wn Industrial Estate, Tallaght, Dublin, Ireland M. Anthony McKervey Department of Chemistry, The Queen‘s University of Belfast, Belfast BT9 5AG, Northern Ireland Calixarenes’ are cyclic oligomers of phenol-formaldehyde condensates which show receptor ionophoric activity when derivatized.These derivatives containing certain functional groups, such as an ester or ketone, at the phenolic oxygen atom have the ability to complex alkali metal cations selectively into the cavity present in the cone c~nformation.~’~ The modified calixarene derivatives are therefore suitable for use as neutral carriers in ion-selective electrodes and have been successfully incorporated in poly(viny1 chloride) membrane (PVC) ion- selective electrode^.^ A recently synthesized calix[4]arene ionophore’ with a high selectivity for sodium ions, from stability constant6 and phase-transfer ~ t u d i e s , ~ was found to be a suitable ionophore for a PVC membrane sodium-selective electrode. Experimental Ionophore The ligand studied was p-tert-butylcalix[4]arene methoxyester as shown in Fig.1. Reagents The ligand was purified before incorporation in the e l e ~ t r o d e . ~ The other membrane components were potassium tetrakis(4-ANALYTICAL PROCEEDINGS, SEPTEMBER 1991, VOL 28 295 OCH2C02CH2CH20Me Fig. 1 electrode Structure of the ionophore incorporated in the PVC membrane chloropheny1)borate (KTpCIPB) 2-nitrophenyl octyl ether (NPOE) (99%), dibutyl sebacate (DBS) (97%), tetrahydro- furan (THF) (HPLC grade) and PVC (ISE grade). Solutions of the highest available purity grades of the alkali and alkaline earth metal chlorides were prepared in doubly distilled water, except for beryllium where the sulphate was used. 150 100 t 50 I '1 a' P 2 a -50 -100 -150 -200 ' I I I 1 I I -6 -5 -4 -3 -2 -1 0 Log [M+l Fig. 2 Response of sodium-selective electrode to the alkali metal, hydrogen and ammonium cations.Membrane composition: calixarene (0.66%), KTpClPB (0.17%), NPOE (65.84%) and PVC (33.33%). A, Na; B, Li; C, K; D, Rb; E, Cs; F, H; and G, NH4 Electrode Construction and Measurements The PVC electrode design was based on a method described by Moody and Thomas8 with subsequent modifications to suit the measuring apparatus which consisted of a thermostated potentiometric cell and stirring unit. The potentiometric readings were measured with a Metrohm 654 millivolt/pH meter and registered on a Linseis LM 24 chart recorder. A Metrohm saturated calomel reference electrode was always present in the measuring cell. The indicator electrode consisted of an Ag-AgCI wire inside the electrode body and immersed in an internal filling solution (0.1 mol dm-3 NaCI).An inter- changeable PVC tip was placed at the bottom of the electrode body and the PVC membrane with the composition given (Table 1) was glued to the PVC tip which was in contact with the analyte. Table 1 Composition of the PVC membrane. The ionophore, KTpCIPB, and plasticizer (NPOE or DBS) were dissolved by stirring. Then the PVC, dissolved in an appropriate amount of THF, was added. The mixture was stirred until a 'syrup' was obtained and this was cast leaving a membrane, on evaporation of the THF, which could be cut and pasted on the PVC electrodes tips (reference 8) Component Composition (YO d m ) Calixarene KTpClPB Plasticizer PVC 0.66 0.17 65.84 33.33 Electrode Performance The performance of the electrode was assessed by measuring parameters such as the slope, limit of detection and selectivity of the electrode.The response of the electrode was measured for the cations over the range from 1 x low6 to 1 x lo-' mol dm-3 and the slope determined from the linear region of the response and the limit of detection. The selectivity coefficients were calculated using both the separate' and mixed'' solution methods. 150 > O E -50 -100 -150 -200 1 I I I I I -6 -5 -4 -3 -2 -1 0 Log [Mn+l Fig. 3 Response of sodium-selective electrode to sodium and alkaline earth metal cations. Membrane composition: calixarene (0.66%), KTpClPB (0.17%); NPOE (65.84%) and PVC (33.33%). A, Na; B, Be; C, Mg; D, Ca; E, Sr; and F, Ba Results and Discussion The response of the sodium-selective electrodes to the alkali metal, alkaline earth metal, hydrogen and ammonium cations was evaluated in all of the studies.Figs. 2-5 show the various responses for a sodium-selective PVC membrane to separate 100 r I 0 > E -50 G -100 - 1 5 0 Y I I I I -6 -5 -4 -3 -2 -1 0 Log [M+l -200 - I Fig. 4 Response of sodium-selective electrode to the alkali metal, hydrogen and ammonium cations. Membrane composition: calixarene (0.66%), KTpClPB (0.17%), DBS (65.84%) and PVC (33.33%). A, Na; B, Li; C, K; D, Rb; E, Cs; F, H; and G, NH4 Table 2 Logarithms of selectivity coefficients for the sodium-selective electrodes. (l), Membrane composition for Figs. 4 and 5. (2), Membrane composition for Figs. 2, 3, 6 and 7. SS, Separate solution determination at 0.1 mol dmP3 of analyte at 298 K.MS, Mixed solution determination in 0.01 mol dmP3 background at 298 K Cation Li + Na+ K+ Rb+ cs+ Be2+ Mg2+ Ca2 + SI2+ Ba2+ H+ NH4+ (1) ss -2.38 0 -1.83 -2.09 - 1.80 -2.70 -2.86 -2.86 - 1.73 - 1.90 -1.91 -0.85 (2) ss -3.75 0 -2.54 -2.59 -3.40 -3.21 -4.29 -4.27 -3.10 -4.08 -2.80 -2.76 (2) MS -2.7 0 -2.2 -2.4 -2.0 -3.7 -3.5 -3.5 -3.2 -3.1 -2.3 -2.0296 I I I I I ANALYTICAL PROCEEDINGS, SEPTEMBER 1991, VOL 28 solutions of various cations. The response of a sodium-selective electrode with the composition given in Table 1 was evaluated for two plasticizers. Figs. 2 and 3 were obtained for NPOE while the membrane with DBS gave the responses shown in Figs. 4 and 5. The performance of the membrane containing NPOE was then studied in solutions of the primary ion, sodium, with a constant background of interferent present, as shown in Figs.6 and 7, allowing a mixed solution determi- nation of the selectivity coefficients. 100 I I 50 I 0 > -50 -100 -150 -200 I 1 I I I I -6 -5 -4 -3 -2 -1 0 Log [Mn+l Fig. 5 Response of sodium-selective electrode to sodium and alkaline earth metal cations. Membrane composition: calixarene (O.66%), KTpClPB (0.17%), DBS (65.84%) and PVC (33.33%). A, Na; B, Be; C, Mg; D, Ca; E, Sr; and F, Ba The selectivity coefficients evaluated from Figs. 2-7 are summarized in Table 2. The sodium-selective electrode with membrane (1) (Fi s. 4 and 5) showed a limit of detection of 10-4.5 mol dm-'for sodium ions and a slope of 46.6 mV decade-' for the response at concentrations above this concentration.The selectivity coefficients indicate that the sodium-selective electrode has selectivity over all of the cations studied with the most -200 I I I 1 I I -6 -5 -4 -3 -2 ' - 1 0 Log "a+] Fig. 6 Response of sodium-selective electrode to sodium ions in a constant background of the alkali metal, hydrogen and ammonium cations. Membrane composition: calixarene (O.66%), KTpClPB (0.17%), NPOE (65.84%) and PVC (33.33%). Background present (0.01 mol dm-3): A, none; B, Li; C, K; D, Rb; E , Cs; F, H; and G , NH4+ 5 significant interferent being the ammonium ion. Membrane (2 (Figs. 2 and 3) showed a limit of detection of 10-4-6 mol dm- for sodium ions and a slope of 53.6 mV decade-' for the response over the linear portion. The selectivity coefficients are again favourable with increased selectivity over membrane (1).The selectivity coefficients determined by the mixed solution method for membrane (2) (Figs. 6 and 7) show a similar trend to the separate solution determinations, but the selectivity is lower as indicated by the log kp"' values given in Table 2 showing differences in the method of determination. 100 50 0 > E -50 a -100 The results presented in this work indicate that the PVC membrane electrode containing the ionophore is sodium selective as predicted. The membrane based on the more polar NPOE plasticizer shows a better performance in terms of sensitivity and selectivity. Another important feature is the favourable selectivity of these membranes over hydrogen ions, thus eliminating any of the pH effects suffered by the glass membrane sodium-selective electrodes. A patent has been applied for the sodium-selective electrode developed in this work.s 1 2 3 4 5 6 7 8 9 10 References Gutsche, C. D., Top. Curr. Chem.. 1984, 123, 1. McKervey, M. A., Seward, E. M., Ferguson, G., Ruhl, B., and Harris, S. J . , J. Chem. SOC., Chem. Commun., 1985, 388. Ferguson, G., Kaitner, B., McKervey, M. A., and Seward, E. M., J. Chem. Soc., Chem. Commun., 1987, 584. Diamond, D., Svehla, G., Seward, E. M., and McKervey, M. A., Anal. Chim. Acta, 1988, 204, 223. Harris, S. J . , McKervey, M. A., Svehla, G., and Diamond, D., Irish Pat. Appl., December 1990. Cremin, S., and McKervey, M. A., unpublished results. Owens, M. J., and McKervey. M. A., unpublished results. Moody, G. J., and Thomas, J. D. R., in Chemical Sensors, ed. Edmonds, T. E., Blackie, London and Glasgow, 1988. Moody, G. J., and Thomas, J. D. R., in Selective ion-sensitive Electrodes, Merrow, Watford, 1971. Van der Linden, W. E., in Comprehensive Analytical Chemistry, ed. Svehla, G., Elsevier, Amsterdam, 1981, vol. XI.

ISSN:0144-557X    

DOI:10.1039/AP9912800293

出版商:RSC    

年代:1991

数据来源: RSC

摘要:

ANALYTICAL PROCEEDINGS, SEPTEMBER 1991, VOL 28 297 Equipment News Ion Source for Mass Spectrometers An electrospray ion source for the makers' Concept and Profile mass spec- trometers offers the advantage of being able to use the high resolution available with mass sector type instruments for the analysis of high relative molecular mass species. Electrospray has been developed as a powerful technique for the formation of intact ions from complex high relative molecular mass species in solution. The electrospray system is ideally suited to the can be assigned with a precision which is typically ~0.01%. Kratos Analytical Ltd. , Barton Dock Road, Urmston, Manchester M312LD. Mass Spectrometer Profile provides automation, ease of use and versatility with a performance pre- viously available only with complex, more expensive, research type instruments. It can cope equally well with simple GC-MS analyses, high relative molecular mass Kratos electrospray ion source for mass spectrometer mass spectrometric analysis of polar com- samples or with the provision of accurate pounds from a relative molecular mass information on elemental compositions.range in excess of 100 000 to below 100. The use of fully modular digital elec- Molecular masses, at least up to 40 000, tronics with distributed microprocessors provides maximum control and flexibility, all handled through a single, intuitive, graphics based user interface. The system also includes PROTUNE, an automatic instrument tuning program, and SYS- DOC, a comprehensive multi-level diag- nostic system.Kratos Analytical Ltd., Barton Dock Road, Urmston, Manchester M312LD. Spectrometer The FTS-7PC FTIR spectrometer com- plements the FTS-7 range of spec- trometers with the availability of IBM-PC compatible software. The FTS-7 optical bench has a 1 cm-' resolution over the complete spectral range of 4800- 400 cm-'. The addition of PC compatible software adds convenience to the high performance capability of the bench. The software extends to include data collec- tion and manipulation, library search and create capability and full quantitative packages. It can also collect data from an externally mounted microscope and from the FTS-7N near infrared optical bench. Bio-Rad Microscience Ltd. , Bio-Rad House, Maylands Avenue, Heme1 Hemp- stead, Hertfordshire HP2 7TD. Spectrophotometer Accessory The RSA-MR-30 colour measurement accessory has been developed in conjunc- tion with reflectance specialists Lab- sphere to replace the original illumination assembly of the Spectronic 3000 diode array spectrophotometer. It can be fitted in minutes and once installed integrates completely with the Rapid*Scan operat- ing software, allowing quick, efficient and accurate data acquisition for solid and liquid samples.Milton Roy European Laboratory Group, Fishponds Road, Wokingham, Berkshire RGll2FD. ICP Sequential Spectrometer The compact JY24 from ISA-Jobin Yvon offers the performance of a research quality ICP system at AA prices, provid- ing sensitivity at the sub-ppb level with a wide dynamic range, fast multi-element analysis with the ability to change analysis on demand, and aqueous, corrosive acid and oil sampling systems. A brochure is available.Instruments S.A. (UK) Ltd., 2 4 Wigton Gardens, Stanmore, Middlesex HA7 1BG. Spectrofluorimeter The Spex FluoroMax features an out- standing photon-counting detection system, a fast scanning system, ease of use298 ANALYTICAL PROCEEDINGS, SEPTEMBER 1991, VOL 28 and impressive sensitivity. It is controlled from an IBM PC equivalent computer, and the powerful DM3000 software sup- plied allows acquisition of data with maximum ease and efficiency. Fluorolog, a modular spectrofluorimeter system, is also available, as well as systems specifi- cally designed for dual wavelength exci- tation and emission applications. A bro- chure is available.Instruments S.A. (UK) Ltd., 2-4 Wigton Gardens, Stanmore, Middlesex HA7 1BG. Gas Chromatograph The GM 295 is finding applications in areas such as research, semiconductor production, manufacturing and gas purity analysis. Over 30 sales have been made worldwide and 100% customer satisfac- tion is being achieved. The GM 295 utilizes discharge ionization detection, which allows reliable detection in the ppb range. Gow-Mac Instrument Co. (UK) Ltd., Gow-Mac House, P.O. Box G13, Gillingham, Kent ME7 4HA. Column Cage The column cage which houses the makers’ 75 m DB-624 Megabore column has been redesigned, allowing easy access to injector and detector fittings for instal- lation or removal. Two 75 m DB-624 columns can be installed in a single oven. J and W Scientific, 91 Blue Ravine Road, Folsom, CA 95630-4714, USA.Gas Chromatography Column The 5 pm film thickness 30 m DB-5 Mega- bore GC column is specifically designed for the analysis of residual solvents com- monly used in various pharmaceutical manufacturing processes, as required by USP Method 467. Among the volatile impurities it can separate are solvents such as ethylene oxide, methylene chlor- ide, benzene, trichloroethylene and 1,4-dioxane. J and W Scientific, 91 Blue Ravine Road, Folsom, CA 95630-4714, USA. Multi-Vendor Instrument Control and Data Handling The first phase of LINK*GC is now available. This combination of software and hardware integrates the data handling and instrument control of multi-instru- ment, multi-vendor gas chromatography systems. It is available within the frame- work of the makers’ ACCESS*CHROM or Turbochrom 3 chromatography data systems and consists of the 600 Series LINK interface and an Instrument Per- sonality Module.Perkin-Elmer Ltd., Maxwell Road, Beaconsfield, Buckinghamshire HP9 1QA. Chromatography Data Handling System Turbochrom 3 is a PC based system providing simultaneous, single point instrument control and data handling for supported gas chromatographs of various manufacturers. By standardizing data acquisition, reduction and reporting through the new 600 Series Link digital- to-digital interface as well as the industry- standard Model 900 A/D interfaces, it can accommodate up to 15 instruments and is compatible with all commercially avail- able gas and liquid chromatographs. Perkin-Elmer Ltd., Maxwell Road, Beaconsfield, Buckinghamshire HP9 1QA.Continuous Chromatography Researched and developed by the French Institute of Petroleum in association with Separex, Liposep is a continuous sep- aration process using liquid chroma- tography. It offers continuous operation with little dilution. It uses the simulated counterflow technique and enables a mix- ture to be continuously separated into components not separable by distillation. Current systems consist of 24 columns along which the liquid or eluents are injected and the separated components extracted. The locations for injection and extraction constantly vary and are controlled by a central unit according to the parameters of the separation. Separex, Chemin de Blanches Terres, BP 9, 54250 Champigneulles, France.HPLC Columns REZEX columns are now available for analysis of carbohydrates, organic acids, alcohols and sugar alcohols in complex matrices such as soft drinks, juices, corn syrups, fermentation broths and many others. Major advances have been made with regard to column efficiency, repro- ducibility and lifetime. Based on a rigid, sulphonated styrene-divinylbenzene copolymer matrix, REZEX columns offer outstanding separations by ion-exchange, ion-exclusion, partition and sizing mech- anisms. Five ionic forms are available, including calcium, hydrogen, silver, lead and sodium, as a series of ten columns, each with a unique selectivity. HPLC Technology Ltd., Wellington House, Waterloo Street West, Maccles- field, Cheshire SLll 6PJ. LC Columns Porozorb cartridges efficiently remove Triton X-100, sodium dodecyl sulphate and other detergents from protein sol- utions without loss of protein.Containing Amberlite XAD-4 or XAD-16 polymeric hydrophobic resins, these columns can also be used to isolate, purify or concen- trate pharmaceutical and biological com- pounds from aqueous streams. Porozorb low-pressure chromatography cartridges come in 250,500,1000 and 1500 ml sizes. Supelchem UK Ltd., Shire Hill, Saffron Walden, Essex CB11 3AZ. HPLC Column The Suplex pKb-100 column operates on a principle that virtually eliminates inter- actions between basic sample components and residual silanol groups on the packing surface. Even basic compounds can be analysed under mobile phase conditions of neutral pH and low ionic strength without amine modifiers.Supelchem UK Ltd., Shire Hill, Saffron Walden, Essex CB11 3AZ. Gas Tight Syringe The Hamilton 1701 ASRN removable needle syringe for use with 23s or 26s gauge needles offers many advantages compared with some liquid-tight syringes: lower cross-contamination, less metal residue caused by plunger abrasion, the possibility to change plungers and better results with volatile liquids. V. A. Howe and Co. Ltd., Beaumont Close, Banbury, Oxfordshire OX16 7RG. UV Detector for HPLC The Model 7215 UV detector features a motor driven monochromator to enable wavelength change at the touch of a button. The excellent sensitivity is based on the low baseline noise level of less than 5 X u h-’ (at 250nm). The 7215 incorporates an autozero, switchable con- stants and variable outputs for any recorder or integration system.Applied Chromatography Systems Ltd., The Arsenal, Heapy Street, Macclesfield, Cheshire SK11 7JB. Capillary Electrophoresis Columns Three CELect columns with novel, bonded phases offer a stable interior surface superior to bare silica tubing for many protein and polymer separations. The three phases, a moderately hydro- phobic phase, a highly hydrophobic phase and a hydrophilic phase, alter electro- osmotic flow in the columns in unique ways that affect the separation mech- anisms. The hydrophobic columns are recommended for increased selectivity in micellar separation experiments. All three columns are available in 50 and 75 pm i d . and can be prepared as custom products in 25 or 100 pm i.d.Also avail- able are kits that include one 50 or 75 pm i.d. column of each phase, plus an untreated silica column and a test standard. Supelchem UK Ltd., Shire Hill, Saffron Walden, Essex CBll3AZ. Autosampler Spares A range of spares for Waters WISP autosamplers is announced. HPLC Technology Ltd., Wellington House, Waterloo Street West, Maccles- field, Cheshire SKll 6PJ.ANALYTICAL PROCEEDINGS, SEPTEMBER 1991, VOL 28 299 Etching Bath Analysed by Ion Chromatography After dilution to the mg 1-I range the sample is filtered through a 0.45 pm membrane and injected into the Metrohm 690 ion chromatograph. The following approximate retention times hold: acetate 1.81 min, fluoride 2.36 min and nitrate 7.26 min. The eluent is benzoic acid at a concentration of 3 mmol 1-1 in ultra-pure water-acetonitrile (98 + 2) (pH value adjusted to 4.65 with TRIS).V. A. Howe and Co. Ltd., Beaumont Close, Banbury, Oxfordshire OX16 7RG. Capillary Electrophoresis System The P/ACE System 2050 features computer control, a flexible autosampler and effective capillary cartridge cooling, for a variety of applications, including automated methods development and fraction collection. Powerful PC (Inter- national Business Machines Corporation) control allows the user to vary parameters within methods and link those methods for extended automated operation. P/ACE permits the user automatically to change rinse sequences, inlet and outlet buffers, samples and sample volumes, temperature, voltage and detection wave- length. The flexible autosampler enables the instrument to collect peaks automati- cally after separation, a useful feature for confirmation of identity and micropre- parative applications.Beckman, Progress Road, Sands Indus- trial Estate, High Wycombe, Buckinghamshire . Demonstration Disk A demonstration disk for the Pyramid chromatography manager offers a com- plete review of how Pyramid is pro- grammed and operated and an explana- tion of most of its features, including totally graphic programming in Windows 3.0. A PC-AT with at least 4Mbyte of hard disk memory is required to run the demonstration. Pyramid is a user-con- figurable data acquisition and analysis system providing true applications multi- tasking, full GLP compliance and direct control of most HPLC and GC com- ponents or systems.Axxiom Chromatography Inc., 11988 Challenger Court, Moorpark, CA 93021- 7122, USA. Headspace Sampler The Model HS 40 automatic headspace sampler is a stand-alone unit with a storage capacity of 40 samples. It can be interfaced to a number of gas chromato- graphs in addition to the makers’ Auto- System and 8000 Series. Its constant mode maximizes sample throughput by allowing each sample of a series to be thermostated for the same time. By overlapping con- stant thermostated periods the sample throughput is dependent only upon the GC analysis time, sample degradation due to extended heating is avoided and no stirring or vibration is required. Perkin-Elmer Ltd., Maxwell Road, Beaconsfield, Buckinghamshire HP9 1QA. Headspace Oxygen Analyser The Ingold InPack 507 analyser for moni- toring trace oxygen levels in packaged products uses a polarographic oxygen sensor with a read-out to display pack oxygen levels to as low as 0.1%, giving accurate results in under 30 s.A recharge- able battery gives maximum portability for use on the factory floor in the QA laboratory. Ingold, Mettler-Toledo Ltd., 64 Boston Road, Beaumont Leys, Leicester LE4 1AW. Sampling Tubes for Air Monitoring The ORB0 range of air sampling tubes for phenols and cresols, organophos- phorus pesticides, acetone and vinyl acetate are an addition to the makers’ range of specialized air sampling tubes and ancillary equipment such as pumps, impingers, gas sampling bulbs and thermal desorption units. Catalogues are available. Supelchem UK Ltd., Shire Hill, Saffron Walden, Essex CBl1 3AZ.Trace Oxygen Analyser The Model 306WAM on-line trace oxy- gen (02) analyser guards against oxygen contamination in hydrogen, nitrogen, argon and other ultra-pure gases used in the manufacture of high density VLSI, VHSIC and other semiconductor devices. It offers full-scale analysis as low as 0- 500 ppb with outstanding accuracy (+lo/,) and exceptional low range sensi- tivity (1%). Teledyne Analytical Instruments, The Harlequin Centre, Southall Lane, South- all, Middlesex UB2 5NH. Exhaust Gas Monitor The Model 9150 carbon monoxide and oxygen on-line analysis system monitors exhaust gas from combustion processes that burn clean fuels such as natural gas and light, low-sulphur fuel oils. It is compact and is equipped with an air aspirated sampling system.It comes standard with three oxygen ranges (0-5, 0-10 and @-25y0) and two carbon monox- ide ranges (0-500 and 0-1000 ppm). The system is housed in an enclosure rated NEMA 4, 12 and 13. Teledyne Analytical Instruments, The Harlequin Centre, Southall Lane, South- all, Middlesex UB2 5NH. Dew Point Sensor The Series 3000-80 cooled-mirror dew point meter provides continuous, on-line measurement to an absolute precision of +0.2”C dew point in a multitude of industrial, research and calibration ap- plications. The new ‘80’ sensor offers greatly improved measurement range capability, which is extended by at least 15°C over the older type ‘60’, which it replaces. It has an operating range from -40 to +90 “C with a dew point measure- ment span of between 40 and 80°C, depending on operating temperature. Michell Instruments Ltd., Unit 9, Nuf- field Close, Nuffield Road, Cambridge CB4 1SS.Probes for pH Measurement A complete range of electrochemical probes for pH, redox and conductivity measurement in the laboratory, field or industrial plant has been introduced. The range of pH electrodes includes models suitable for all makes of pH meter and all applications. Also available is a wide range of buffer solutions, pH standards, in solution or capsule forms, reference electrolyte solutions and ion solutions, reagents and standards. ChemTech Analytical Ltd., Alpha- Line Division, 4 Railton Road, Wolsley Business Park, Kempston, Bedford MK42 7PN. Determination of Low Water Con tents Metrohm’s 701 KF Titrino offers out- standing indication and control features allowing great precision and reproduci- bility with small sample additions.V. A. Howe and Co. Ltd., Beaumont Close, Banbury, Oxfordshire OX16 7RG. Titrator Metrohm’s 702SM Titrino features four titration modes, method storage, built-in interface for printer, balance, PC or robot, full two-way communication with PC or LIMS, extensive calculation facility and compatibility with existing Metrohm accessories and automation ranges. V. A. Howe and Co. Ltd., Beaumont Close, Banbury, Oxfordshire OX16 7RG. Titrator The DL70 with multi-burette system and optimized software is used in central and routine laboratories where automation is in great demand. Simple preparation, method database with proven functions, Karl Fischer applications, a learn titration program, etc., are featured.Greifensee, Switzerland. Mettler-Toledo AG, CH-8606 Water Analysis Service A complete water quality analysis service for measurements in rivers, estuaries, coastal regions and offshore includes chemical, microbiological, bacteriological300 ANALYTICAL PROCEEDINGS, SEPTEMBER 1991, VOL 28 and virological tests carried out from a fully equipped survey launch, the Searcher. The data can be specially for- mated to suit specific mathematical models for the management of water quality and discharges into rivers and estuaries. Andrews Hydrographics Ltd., Marine Environmental Division, 1 Victoria Place, The Promenade, Kingsbridge, Devon TQ7 1JG. Drying Oven for Karl Fischer Titration The DO302 drying oven provides a solu- tion to determination of water in samples such as plastics that release water slowly or in substances such as ascorbic acid which react with the Karl Fischer reagent.The water in the sample is driven off in the DO302 and transferred by means of a dry inert gas to the titration beaker of a Mettler KF titrator. The oven has variable heating up to 300 “C. Greifensee, Switzerland. Mettler-Toledo AG, CH-8606 Filter Funnel Reservoir A 400 ml reservoir has been introduced for the 7cm size of the makers’ three- piece filter funnel. Designed with glass microfibre filters particularly in mind, the three-piece funnel will hold a filter in the correct position for optimum filtration, its positive edge clamping preventing any liquid from flowing around, rather than through, the filter circle.Whatman Scientific Ltd., Whatman House, St. Leonard’s Road, 20/20 Maid- stone, Kent ME16 OLS. Microfiltration Devices Puradisc 25 AS is a device with low hold- up volumes and Luer lock connections for sample preparation and filtration of volumes up to 50 ml. The polysulphone membrane selected for low protein bind- ing makes the unit ideal for biological applications. Devices with larger pore sizes make useful pre-filters prior to reverse osmosis or ultrafiltration. Polydisc AS and Polycap AS are intended for sterilizing and filtering larger aqueous volumes such as tissue culture media, antibody and enzyme solutions and lab- oratory water supplies. Both feature a low-binding membrane made of asym- metric esters of cellulose and a glass microfibre pre-filter.Whatman Scientific Ltd., Whatman House, St. Leonard’s Road, 20/20 Maid- stone, Kent ME16 OLS. Balances The BDH DElOOA is compact, light- weight and uncomplicated. It is accurate down to 0.1 mg with a maximum capacity of 100 g. One key operates all facilities including tare and automatic calibration, while an easy to read, non-glare liquid crystal display provides fast response results with excellent visibility. A %door, glass draught shield is provided and there is an RS232C interface. Merck Ltd., Broom Road, Poole BH12 4”. Isocyanate Analysis Kits are available for isocyanate sampling and analysis using the HSE’s guideline method MDHS 25 and the modern auto- mated instrumentation used provides a rapid results service. Active participation in the recognized external QA scheme for isocyanate analysis (AQUA) guarantees accurate measurement and the whole package is available for less than 545 per sample.The National Occupational Hygiene Service Ltd., Skelton House, Manchester Science Park, Lloyd Street North, Man- Chester M15 4SH. Hydrogen Bromide MEGA-CLASS hydrogen bromide offers typical purity levels of 99.995% and water contamination reduced from the 1000 ppm of previously available product to between 10 and 30 ppm. Air Products plc, Hersham Place, Molesey Road, Walton-on-Thames, Surrey KT12 4RZ. Nitrogen Trifluoride A new grade of nitrogen trifluoride, MEGA-CLASS NF3, offers 99.995+% purity, with tetrafluoromethane levels at less than 10ppm. Air Products plc, Hersham Place, Molesey Road, Walton-on-Thames, Surrey KT12 4RZ.Mercury Concentration System The PU9365 mercury concentration system allows the detection of mercury at the 20 ng 1-I level. In conjunction with an atomic absorption spectrometer it is ideal for the detection of trace levels of mer- cury in environmental samples. The new system is readily linked to the makers’ continuous flow vapour system and atomic absorption spectrometer. It is suitable for PU91OOX, PU92OOX and PU94OOX users wishing to upgrade their equipment. A large number of samples can be handled automatically if the spec- trometer is fitted with an autosampler. Philips Analytical, York Street, Cam- bridge CB12PX. Thermal Analysis Software A three-dimensional data plotting and manipulation capability is available as an advanced option for the PL-Plus V soft- ware package, which can control up to seven thermal analysis instruments, including DMTA, DSC, TGA, TMA and STA.PL Thermal Sciences, Polymer Labora- tories Ltd., The Technology Centre, Epinal Way, Loughborough, Leicester- shire LEll OQE. Thermal Analysis Products The Hi-Res TGA 2950 thermogravi- metric analyser is the first module to use the makers’ new Hi-Res thermal analysis technology. It offers accurate, reproduc- ible weight change values, high sensitivity (0.1 pg) and weight capacity (1.5 g), and automated ease-of-use features. Also announced is an automated differential scanning calorimetry system that analyses up to 62 samples unattended and offers the choice of up to 15 different exper- imental methods and more than 100 data analysis routines.Autoanalysis software programs are also available for thermo- gravimetric analysis and differential scan- ning calorimetry. TA Instruments, Eckenheimer Land- strasse 60a, D-6000 Frankfurt am Main 1. Software for Thermal Analysis The 7 Series/UNIX software system is designed to run on industry-standard DEC 325 workstations. It allows com- plete automation and control of the 7 Series thermal analysis instruments, the DSC 7 differential scanning analyser, theANALYTICAL PROCEEDINGS, SEPTEMBER 1991, VOL 28 301 TGA 7 thermogravimetric analyser, the DMA 7 dynamic mechanical analyser and the TMA 7 thermomechanical analyser. The system permits multi-tasking so that multiple thermal analysis modules can be run simultaneously. The 'DOS task' feature allows simultaneous operation of thermal analysis software libraries and DOS software programmes for maximum flexibility. Perkin-Elmer Ltd., Maxwell Road, Beaconsfield, Buckinghamshire HP9 1QA. Sample Changer The Metrohm 676 sample changer is ideal for applications that require a digestion stage prior to analysis, e.g., chemical oxygen demand in waste water and hy- droxyl and saponification numbers in oils and fats.V. A. Howe and Co. Ltd., Beaumont Close, Banbury, Oxfordshire OX16 7RG. Sample Changer The cost of a sample changer for Metrohm equipment is often repaid within short periods of time, based on operator time savings during the normal working day alone. Even greater savings can be achieved by unattended overnight operation. V. A. Howe and Co. Ltd., Beaumont Close, Banbury, Oxfordshire OX16 7RG. Centrifuges The complete range of Eppendorf centri- fuges runs from the microcentrifuge 5413, 5415C and the refrigerated 5402 up to the ZK 630 high capacity refrigerated model, capable of handling 6 1 of material.All models have lid locks and comply with European safety standards including BS 4402, and all Z-series centrifuges except the 2230 have imbalance indicators and variable braking; the larger models have sensors to protect samples from over- temperature and freezing. BDH Laboratory Supplies, Broom Road, Poole, Dorset BH12 4". Ultracentrifuge The Optima XL-A provides a convenient instrument for evaluating shape, size, density and interaction of molecules. Applications include binding studies, sedimentation coefficient determination and research on association-dissociation behaviour.The Optima XL-A features a high intensity xenon light source, a patented diffraction grating monochro- mator, a light detector and a software package that controls the system and compiles data. Beckman, Progress Road, Sands Indus- trial Estate, High Wycombe, Buckinghamshire . Pumps Mark IV pumps are quiet versions of the makers' laboratory chemical vacuum pumps. They use a silicone fluid which resists oxidation and attack by acid and because the pumps continuously purge the oil of any solvent it does not need to be changed. The pumps are fitted with a remote control socket which can be inter- faced with the Vac Stop version of the SF50 combined centrifugal concentrator and freeze dryer.The Mark I CVP50, launched in 1987, achieved a vacuum of 10 mbar with a 50 1 min-l flow rate. The CVP100, launched in 1989, with an ulti- mate vacuum of 0.15 mbar and a flow rate of 1001 min-', is also suitable for cen- trifugal concentration. Genevac Sales Development Ltd., 9 Farthing Road, Sproughton, Ipswich IP15AP. Dispenser The 665 Dosimat allows accurate dispens- ing, free from pulsation, of small or large amounts of liquids. The resolution of the contents of a burette comprises 10000 steps and allows precise dispensing with rates adjustable from 0.001 ml min-' to 9 1 h-l. For continuous, uninterrupted dispensing two 665 Dosimats can be linked. V. A. Howe and Co. Ltd., Beaumont Close, Banbury, Oxfordshire OX16 7RG. Rotary Shaker The totally re-designed Maxi Mix I11 Type 65800 is even more versatile than its predecessor.Its four distinct, inter- changeable accessory holders handle a complete range of laboratory shaking and mixing needs. A soft rubber plate for mixing tubes or flasks is supplied free with the base unit. The Maxi Mix I11 also comes complete with an ordoff switch, rubber feet, power cord and plug. An optional tray for petri dishes is available. The flask holder can accommodate up to four 250 ml flasks and the universal holder will hold racks of all kinds. Radleys, Shire Hill, Saffron Walden, Essex CBll3AZ. Safety Labelled Wash Bottles An additional 12 varieties of 500 ml wash bottles are announced and the 1000ml range is also extended to include other more popular names. They offer the convenience of having wash bottle solu- tions spelt out in bold, eye-catching letters and graphics.The bottles have wide mouths for easy filling. Radleys, Shire Hill, Saffron Walden, Essex CBll3AZ. LIMS ACCOMPLIS LIMS features a flexible, non-hierarchical security system specifi- cally designed for laboratory applications. Data are completely protected against unauthorized access, and in multi-labora- tory installations users can be assigned different levels of access in each laboratory. ICI Chemicals and Polymers Ltd., P.O. Box No. 1, Billingham, Cleveland TS23 1LB. Photomultiplier Tubes The PMT Series of highly sensitive, wide- band photomultiplier tubes achieves sig- nificantly increased performance for pho- tochemical, photobiological and photon counting applications in which conven- tional tubes cannot provide sufficiently high performance.The PMT Series con- sists of two proximity-focus, micro-chan- nel plate photomultiplier tubes featuring a spectral response of 200-800 nm and an extremely low background count rate. They offer a choice of input window and the option of a double or triple micro- channel plate. Instrument Technology Ltd., 29 Castle- ham Road, St. Leonards-on-Sea, East Sussex TN38 9NS. Molecular Modelling Software Previously available only on Digital Equipment VAXNMS systems, COBRA conformational analysis software is now available to users of Silicon Graphics workstations. Silicon Graphics is the first in a series of ports into the standard UNIX environment. COBRA is also available on other UNIX platforms, such as the new Series 700 from Hewlett- Packard and the Sun SPARCstation.It will shortly be available on the IBM RS/6000. Oxford Molecular Ltd., Terrapin House, South Parks Road, Oxford OX1 3UB. Control System for Electron Microscopes With the WINSEM control system users can operate the microscope with extreme ease and speed using the system's mouse control, or by using the more familiar analogue controls. The WINSEM presents the user with information clearly and concisely using the Windows graphi- cal interface. Jeol microscopes fitted with the new system have a third screen dedicated to the Windows display. Jeol (UK) Ltd., Jeol House, Silver Court, Watchmead, Welwyn Garden City, Hertfordshire AL7 1LT. Thermal Arraycorder The WR7400 is a portable, compact, two- channel, realtime recorder with a dual a.c./d.c.power supply. It offers a fre- quency response of 200 Hz (-3 dB) and measuring ranges from 50mV to 200V (fsd). There are two chart speed ranges: a fixed ran e from 1 to 50mms-I or mm min-F, or a variable range from 0.1 to 60 mm s-' or mm min-' in 1 mm s-' or mm min-' increments. The chart speed can be synchronized with an external pulse up to a maximum of 60 mm s-'.302 ANALYTICAL PROCEEDINGS, SEPTEMBER 1991, VOL 28 Graphtec (UK) Ltd., Welshman’s Lane, off Welsh Row, Nantwich, Cheshire CW5 6AB. Lettering System The P-touch PT-2000 electronic lettering system is a fast, easy means of producing instant, self-adhesive, laminated labels. Just Plastics Ltd., Cromwell House, Staffa Road, London El0 7PY. Non-slip Pads Dycem non-slip pads, mats, reels and self- adhesive pads have many applications in the laboratory, hospital, office, home and industry.Dycem Non-Slip is manufac- tured from a specially developed polymer compound with an exceptionally high coefficient of friction. Radleys, Shire Hill, Saffron Walden, Essex CBll3AZ. Baffled Flasks Break-resistant , re-usable, polycarbonate baffled flasks are available in 250 and 500 ml sizes. The baffles increase mixing when trypsinizing, aeration or gas exchange is conducted in a variety of processes such as fermentation, cell cul- ture growth and cultivation or genetic engineering procedures. Nalge Co., Sevenoaks, Kent TN14 5BQ. Spill Containment Pack Independent tests carried out by an estab- lished contract testing laboratory have officially confirmed the effectiveness of the Whatman Spill Containment Pack in dealing with accidental chemical spillages within laboratories.Whatman Scientific Ltd., Whatman House, St. Leonard’s Road, 20/20 Maid- stone, Kent ME16 OLS. Disinfectant Wipes Cide-Swipes are powerful, high-level pre- saturated disinfectant wipes. Freshly scented and easy to use, they are available in pad form or as a cloth to suit specific applications. Radleys, Shire Hill, Saffron Walden, Essex CBll3AZ. Laboratory Chair The new Lab-Seat laboratory chair was designed especially for use in the labora- tory and industry where raised benches and worktops require seating with added height facilities. The Lab-Seat features a ‘waterfall’ front to alleviate pressure behind the knee and a top release gas operated height adjustment with a maxi- mum seat height of 85 cm when fully extended and a minimum of 60 cm.Radleys, Shire Hill, Saffron Walden, Essex CBll3AZ. Portable Containment Station The Fumebubble FX1 provides a personal space where the operator can work with hazardous materials or substances in safe, uncontaminated conditions. Compact and economic, it can be used to replace existing, more expensive and less flexible stationary facilities such as fume hoods. Air is drawn through the hand ports (away from the operator) and is dis- charged at the back of the unit through the specially designed extraction-filt- ration outlet. Radleys, Shire Hill, Saffron Walden, Essex CBll3AZ. Literature A 2-page flyer describes instrument tech- nology, possible applications and techni- cal data for the Spectroflame-ICP D sequential ICP spectrometer.Spectro Analytical Instruments, Bosch- strasse 10, D-4190 Kleve, Germany. Literature is available on the Senator range of quadrupoles for residual gas analysis, leak detection, gas analysis and process monitoring for vacuum, semi- conductor, biotechnology, chemical, metallurgy, pharmaceutical and food pro- cessing industries. Spectramass Ltd., Radnor Park Indus- trial Estate, Congleton, Cheshire CW12 4XR. A book provides a timely review of the various analytical methods currently available for determining trace amounts of pollutants: ‘Environmental Analysis - Instrumental Techniques’. Hewlett-Packard S.A., 150 route du Nant-d’Avril, CH-1217 Meyrin 2, Geneva, Switzerland.Application notes describe the advan- tages of novel sample handling techniques for routine GC analysis. Methods include determination of water in solvents by capillary chromatography, rapid detec- tion of volatile compounds in crude ben- zole, detection of residual methyl bro- mide fumigant in natural products, and flavour and fragrance profiling. Tech- niques include fully automatic heart-cut- ting, backflushing, thermal desorption and headspace procedures. More than 200 GC-related application notes are available. Perkin-Elmer Ltd., Maxwell Road, Beaconsfield, Buckinghamshire HP9 1QA. A brochure gives details of the Model 116 isocratic and Model 126 gradient solvent delivery modules for chromatography. Beckman Instruments (United King- dom) Ltd., Progress Road, Sands Indus- trial Estate, High Wycombe, Buck- inghamshire HP12 4JL.The 1991 Chromatography Users’ Cata- logue is now available for scientists seek- ing a single source for laboratory supplies, consumables and accessories. Hewlett-Packard S.A., 150 route du Nant-d’Avril, CH-1217 Meyrin 2, Switzerland. An Application Brief describes the com- bined use of GC-MS and GC-IR detec- tors for the analysis of hazardous wastes. Hewlett-Packard S.A., 150 route du Nant-d’Avril, CH-1217 Meyrin 2, Switzerland. Volume 5 , Number 1, of ‘The Separation Times’, a quarterly chromatography newsletter, discusses government meth- ods for residual solvents in pharma- ceutical manufacture with analysis requirements for the USP Method 467 and simulated distillation of petroleum products for ASTM Method D2887.Other articles include information on capillary electrophoresis, sample prep- aration and conditioning solid phase extraction cartridges. J and W Scientific, 91 Blue Ravine Road, Folsom, CA 95630-4714, USA. A complete range of HPLC systems and components is described in a catalogue, ‘HPLC- Systems for Solutions’. Perkin-Elmer Ltd., Maxwell Road, Beaconsfield, Buckinghamshire HP9 1QA. A guide to pH measurement in process and laboratory, ‘Practice and Theory of pH Measurement’, is now available. Ingold, Mettler-Toledo Ltd., 64 Boston Road, Beaumont L W , Leicester LE4 1AW. A thermal analysis supplies catalogue gives details of the full range of acces- sories and consumables available. Perkin-Elmer Ltd., Maxwell Road, Beaconsfield, Buckinghamshire HP9 1QA. Literature describes the 615 mains distri- bution system, which allows five or six different instruments to be run from a single mains socket, isolating them from mains-borne interferences. V. A. Howe and Co. Ltd., Beaumont Lane, Banbury, Oxfordshire OX16 7RG. The 1991 Nalgene laboratory ware cata- logue gives details of a range of products for filtration, cryopreservation, centri- fugation and ultracentrifugation, as well as bottles, carboys and benchware. Merck’ Ltd., Broom Road, Poole BH12 4”. The 1991 BDH Laboratory Supplies chemicals and apparatus catalogues give a comprehensive guide to the complete range of products available. Merck Ltd., Broom Road, Poole BH12 4”. A brochure describes the Model MAS- 300 microwave muffle furnace.ANALYTICAL PROCEEDINGS, SEPTEMBER 1991, VOL 28 303 CEM Corporation, P.O. Box 200, Matthews, NC 28106, USA. Following the introduction of the Electro- nic Catalogue on disk, featuring over 1700 product types, the ‘Rental Decision Maker’, which calculates whether pur- chase or rental is the more cost effective from figures input by the user, is offered as standard on the catalogue disk, avail- able in 34 and 54 in floppy disk versions. Also available is a brochure describing an environmental monitoring service. Livingston Hire, Livingston House, 2-6 Queens Road, Teddington, Middlesex TWll OLB. The Winter 1990-91 issue of Chemical Design News gives details on the choice of Chem-X to build a 3-D database of the Chapman and Hall Dictionary of Drugs. It also includes other items on software and workstations. Chemical Design Ltd., Unit 12,7 West Way, Oxford OX2 OJB. Two brochures are available, one giving information on a range of glassware, the other giving details of a range of computer software. Aldrich Chemical Co. Ltd., The Old Brickyard, New Road, Gillingham, Dor- set SP8 4JL. Death We regret to announce the death of Dr. Lewis Edwin Coles, the former Public Analyst of Mid-Glamorgan and West Glamorgan.

ISSN:0144-557X    

DOI:10.1039/AP9912800297

出版商:RSC    

年代:1991

数据来源: RSC

摘要:

304 ANALYTICAL PROCEEDINGS, SEPTEMBER 1991, VOL 28 Conferences and Meetings Medical Diagnostics in Japan October 4, 1991, London GAMBICA (the association for the in- strumentation, control and automation indus- try in the UK), in collaboration with the Department of Trade and Industry (DTI) is organizing a one-day seminar to report the findings of the recent high-level mission to Japan on in vitro diagnostics. The seminar will take place at the Grosvenor House in London. In April of this year Dr. Ron Cole- man, Chief Engineer and Scientist at the DTI, led a high-level mission to study the structure of the diagnostics market in Japan and likely developments to the year 2000, to identify opportunities for collaboration and to discuss, with Japanese Government officials, their regulatory system for diagnostic reagents and the effect on foreign suppliers. The seminar will report on the Mission's findings, high- lighting the strengths and weaknesses of both UK and Japanese companies, discuss the op- portunities for collaboration and any steps UK companies can take to capitalize on these opportunities.It is anticipated that delegates will also be able to talk in detail with various Mission Members. A written report contain- ing details of the Mission's findings will be launched at the seminar. The fee for attendance, to include refresh- ments and a copy of the Mission Report, will be El65 inclusive of VAT. Further details and an application form are available from Janice Kew or Colin An- drews at GAMBICA, 8 Leicester Street, Lon- don WC2H 7BN.Reliable Sampling Conference December 4-5, 1991, London Reliable sampling for chemical analysis is an important technical subject which can become of public concern when it is related to the legal and moral implications of the work. Recent examples relate to the contami- nation of water supplies and to forensic evi- dence used in criminal prosecutions. The importance of reliable sampling procedures for liquid and gaseous streams and solid masses cannot be over-emphasized. Only if the sample is reliably taken can subsequent analyses have validity. The Laboratory of the Government Chemist and the Association of Public Analysts are co-sponsoring, and pro- viding speakers for, this important and timely Sira Communications conference, which will be held in the Scientific Societies Lecture Theatre, new Burlington Place, London W 1.The emphasis of the conference will be on environmental sampling and process quality assurance covering food, brewing, agricultu- ral feeds and fertilizer industries. There will also be presentations on standards, accredita- sampling. Annual Meeting and Exposition For further information contact Peter Rus- sell, Sira Communications Ltd., South Hill, May 1992* Chislehurst. Kent BR7 5EH. This will be a joint meeting of the Interna- tional Society for Fat Research and the American Oil Chemists' Society. The Shera- Oil and Gas Thailand/Chemical Thai- ton Centre Hotel and Towers will Serve as headquarters for the meeting. The pro- landnnstrument Thailand Febuary 27-March 1, 1993, Bangkok, Thai- gramme will feature speakers from around Lana' the world, allowing an opportunity for inter- national interaction among professionals has confirmed that it will organize an official try.ISF adds a special feature to this United Kingdom participation at Oil and Gas meeting, the Kaufman Memorial Lecture, ThailandIChemical Thailand/Instrument which will be held Tuesday, May 12. Four Thailand. This exhibition covers all aspects days of technical sessions are planned for this duction of oil and gas, through chemical and planned in the following petrochemical processing to instrumentation, equipment. The Department Of Trade and Industry (DT1) working in all areas of the fats and oils indus- Of Petrochemicals, from and Pro- meeting. At this time technical sessions are areas: Biology and Nutrition, Plant Lipids, Bioengineering, Flavour Quality and Sta- Exhibitors who form part Of the UK bility, Environmental, Edible Uses of Fats cal, Safety and Engineering, Oilseed Proteins mately 50% off participation cost plus a travel allowance of over E600 per person for and Chemicals and Fatty Acids.2 people. Companies interested in joining the UK Group should contact the following Further information is available from Meetings Department, AOCS, PO Box 3489, Champaign, Illinois, 61 826-3489, USA. to register their interest: Patrick Hamgan, Overseas Exhibition Services Ltd., 1 1 Man- Chester Square, London W1M 5AB. Fourteenth International Symposium on Europt(r)rode 1: First European Con- ference on optical Chemical Sensors and May 25-29,1992, Baltimore, Maryland, USA Biosensors This symposium will be held in the Stouffer April 12-16, 1992, Graz, Austria Harborplace Hotel.Review papers, invited process and laboratory and Surfactants and Detergents, Biotechnology- Group benefit from a subsidy Of approxi- and Oils, Fats and Oils Production, Analyti- Chromatography Among the numerous Sensor types, those and submitted papers, poster sessions and based on optical methods have received par- plenary and parallel discussion sessions on titular attention in the past 10 years. Numer- the latest ous sensing schemes have been developed, Of, chromatography~ microcolumn and and instruments are being marketed or and microseparation techniques will be are close to. Apart from commercial in- presented. Also presented will be a vendor SOr types have been installed for use in sion sessions encompassing the latest devel- Qc/QA.In new fibre op- to be covered include: capillary GC, capillary tics, planar waveguides, new opto-electronic GC-MS9 GC-mR7 GC- the optical sensor technology has grown very matography (SF')* 'One fast and is likely to play a major role in mod- electrophoresis (CZE), micellar electrokinetic continuous monitoring purposes, in particular covered include environmental analysis, or- flavours and fragrances, food and beverages, strumentation, a number of tailor-made sen- exhibition as process control, or are applied routinely in opments in instrumentation. The techniques as workshop type discus- analytical components and microprocessors, AES7 micro-HPLC, su~rcritical fluid chrO- ern analytical sciences. Given the real-time chromatography (MEKC), and new nature of sensors, they are ideally suited for and instrumentation.The to be for chemical and biotechnological processes, ganic water quality, the air we breathe and in clini- drug testing, petroleum and petrochemica's, Pharmaceutical analY cal analysis. In the Congress, which will be held in the Proteins and Peptides, trace and preparation techniques. Persons submit a Congress Centre, Graz, it is intended to Cover all aspects of optical chemical sensing and wishing to Present Papers 300 word abstract before November 30, For further information contact Professor 1991, to Dr. Pat Sandra at the following ad- Krijgslaan 281 (S4), B-9000 Ghent, Belgium. optical biosensing.Otto s. wolfbeis, Institute for Optical Sen- dress: Professor SOTS, Steyrer-Gasse 17, A-8010 G r z , Austria. for Organic Pat Sandra, Laborato~ Of Ghent, Further information on all aspects of the 20th ISF World Coneress: 83rd AOCS meeting. as well as registration materials. can tion, economics, legislation and medical ~- ~~ ~-~ n "I "ANALYTICAL PROCEEDINGS, SEPTEMBER 1991. VOL 28 305 be obtained from Dr. Leonard Schronk, Foundation for the ISCC, PO Box 663, Ken- nett Square, PA I9348 USA. The Fifth International Symposium on Polymer Analysis and Characterization June 1 4 , 1992, Inuyama City, Japan This three day Symposium will consist of poster sessions, invited lectures, round-table discussions and information exchange on re- cent advances in polymer characterization ap- proaches, techniques and applications. The topics discussed will include chromato- graphy, infrared, NMR, mass spectrometry, chemical characterization, light scattering, rheology, microscopy, viscometry, surface analysis, thermal analysis, thermodynamics and solution properties of polymers, as well as general contributions on polymer analysis and characterization.Further information can be obtained from Dr. Sadao Mori, Department of Industrial Chemistry, Faculty of Engineering, Mie University, Tsu, Mie, 514, Japan, or Dr. Ho- ward Barth, Du Pont Company, Experimental Station, PO Box 80228, Wilmington, DE 19880-0228, USA. Australian and New Zealand International Forensic Science Symposium August 17-21, Hobart, Tasmania, Australia The 11 th symposium of the Australian and New Zealand Forensic Science Society is to be held in Hobart, Tasmania.Further details may be obtained from The Conference Manager, 1992 ANZFSS, Banks Paton Conference Management, GPO Box 558F, Hobart, Tasmania, Australia, 7001. EUCMOS XXI August 23-28, 1992, Vienna, Austria EUCMOS XXI will be held in the Technical University of Vienna and will feature 8 main topics in 8 plenary, 24 keynote and a great number of contributed oral or poster papers. The main topics to be considered will be: molecular structure and interactions; surface analysis-methods and applications; hyphe- nated techniques (chromatography-spectros- copy); optical sensors; computer aided molecular spectroscopy; theoretical aspects; biological pathways; and phase transition and order phenomena.Further information is available from Pro- fessor Dr. R. Kellner, Congress Chairman, c/o Interconvention, Austria Centre, Vienna, A- 1450 Vienna, Austria. Fifth International Conference on Nickel Metabolism and Toxicology September 7-12, 1992, Sudbury, Ontario, Canada The Sudbury Conference, which will be held in the Holiday Inn, continues the tradition of the International Conferences on Nickel Me- tabolism and Toxicology. The hosts will be Inco Limited and Falconbridge Limited, Sud- bury, Canada. The conference will provide a forum for the exchange of information on recent advan- ces in nickel biochemistry, metabolism, geno- toxicity, carcinogenicity, immunotoxicity, reproductive toxicity, environmental toxicity and related ecological issues, as well as epi- demiological studies of nickel workers and biological monitoring of nickel exposures in the workplace.Regulatory aspects of nickel exposure will also be considered. For details contact the Fifth International Conference on Nickel Metabolism and Toxi- cology, c/o Falconbridge Limited, Ms. Mar- garet Koski, Falconbridge, Ontario, Canada POM 1SO. The 1992 International Symposium on Radon and Radon Reduction Technology September 22-25, 1992, Minneapolis, Min- nesota, USA The purpose of the Symposium is to provide a forum for the exchange of technical infor- mation on radon and radon reduction tech- nology in the indoor environment. It will be held in the Sheraton Park Hotel. Papers will address all facets of radon and radon reduction technology for residential and large buildings and the sciences on which this technology is based. Topics of greatest interest include the following. Health issues: Epidemiological and Inhalation Toxicology; Studies; Radon and Radon Progeny Studies; Risk Assessment; Worker Health Protection and Exposure; Public Information and Educa- tion. Government Policy: International; Federal; State; Local. Measurement Meth- ods: Techniques; Quality Assurance; Short- t e d o n g term Measurements. Surveys and Geological Data: Residential Surveys; Soil Characteristics; Geological Parameters; Map- ping. Radon Dynamics Modelling: Transport; Entry; Building Dynamics. Radon Control in Residential, School, and Large Buildings; Mitigation Methods; Barrier Technologies; HVAC Effects and Interactions; Radon Resis- tant New Construction; Costs and Cost Effec- tiveness; Effectiveness of Hardware and Sealants; Optimization and System Perfor- mance. To obtain a registration form write to Radon Symposium, c/o CRCPD, 205 Capital Avenue, Frankfort, KY 40601, USA.

ISSN:0144-557X    

DOI:10.1039/AP9912800304

出版商:RSC    

年代:1991

数据来源: RSC

摘要:

ANALYTICAL PROCEEDINGS, SEPTEMBER 1991. VOL 28 305 Courses Loughborough Short Courses Autumn, 1991, Loughborough The following courses will be held in the De- partment of Chemistry. ‘Separations for Bio- technology and Biochemistry’, September 23-27, 1991; ‘Modern Techniques in Immu- noassay’, October 24-25, 199 1 ; ‘Atomic Ab- sorption Spectrometry’, December 16-20, 1991; and ‘Statistics for Analytical Chem- istry’, December 17-20, 199 1. Further details are available from Mrs. S. Maddison, Department of Chemistry, Lough- borough University of Technology, Lmghbo- rough, Leicestershire LEI 1 3TU. Chemical Engineering for Scientists September 30-October 4, Bradford This will be a five day intensive course de- signed for chemists and other scientists work- ing in the chemical and process industries as an introduction to the basic concepts and general philosophy of chemical engineering.Chemical engineering is a broad techno- logical discipline that is essentially concerned with the application of scientific and engin- eering principles, both theoretical and empiri- cal, to the design, development and operation of industrial processes. Chemical engineers have made a substantial contribution to the development of the chemical, petroleum and petroleum industries. For detailed information and a registration form contact Conferences and Courses, In- stitution of Chemical Engineers, Davis Build- ing, 165-1 7 1 Railway Terrace, Rugby CV21 3HQ. Applications of Microwave Techniques in Analytical Sample Preparation October 1-2, 1991, Hull In recent years there has been a rapid growth in the use of microwave heating for the wet and dry ashing of samples.The attractions of this approach to sample preparation are well documentated and include rapid digestion times, minimization of contamination, loss of volatiles and more effective use of reagents. This short course will introduce current and potential uses to a range of application areas, including fusion techniques and automation. In addition, as we become more dependent on these techniques, a better understanding of the chemical and physical mechanisms in- volved in digestion will be required and this aspect of the subject will be addressed at the meeting. The course will be of interest to analysts involved in the preparation of sam- ples for both organic and inorganic analysis,306 and for those who wish to improve their methodology in this important growing area of sample preparation.The course will take place at the Univer- sity of Hull, Cottingham Road, Hull. The registration fee will be f129 plus VAT. This includes the conference dinner, accommoda- tion, breakfast and lunch on October 2. Reg- istration without accommodation is &99 plus VAT. For Eurther details contact Sandie McCol- lin, The Short Course Office, School of Chemistry, The University, Hull HU6 7RX. Analytical Science and the Environment Autumn, 1991, Ascot and Milton Keynes The organizers have designed the courses for anyone concerned with environmental prob- lems. They are suitable for consultants, re- searchers, analysts and managers who want an update on current methods.Whether you are particularly interested in water, soil, vege- tation or air samples, the courses will give a good basis for deciding how to tackle the problem. They will be held at Silwood Park, near Ascot, except for the XRF course which will be held at the Open University. The ANALYTICAL PROCEEDINGS, SEPTEMBER 1991, VOL 28 courses will be: October 22-24, 199 I, ‘Prob- lem solving in environmental science: samp- ling, analytical techniques and data interpretation’ (Dr. M.H. Ramsey and Dr. P.J. Potts); November 5-7, 199 1, ‘Inductively coupled plasma atomic emission spectro- metry: sample preparation techniques, ana- lysis and interpretation’ (Dr. J.N. Walsh and Dr. I. Jarvis); November 19-21, 1991, ‘In- ductively coupled plasma mass spectrometry: a powerful analytical tool for the environ- mental scientist’ (Dr.K.E. Jarvis and Dr. J.G. Williams); December 3-5, 199 1, ‘X-ray fluo- rescence: analytical practice in the fields of environmental, industrial and research scien- ces’ (Dr. P.J. Potts and Dr. P.C. Webb); De- cember 10-12, 1991, ‘Activation spectrometry: the role of neutron activation and gamma ray spectrometry in environmen- tal analysis (Dr. S.J. Parry). For further information contact Pamela Manser, Continuing Education Centre, Im- perial College, London SW7 2AZ. Laboratory Waste Disposal and Environ- mental Compliance November 6 7 , 1991, San Diego, CA, and December 2 4 1991, Durham, NC, USA Hazardous waste disposal is of more concern than ever. Laboratories face a cradle-to- grave liability for proper waste disposal and the US Justice department is increasing criminal enforcement actions against indis- criminate hazardous waste disposal practices, including indictments returned against labor- atories.This course is designed to save the often overworked laboratory scientist from having to sift through and make sense of ever-changing legislation and research. The information is presented in a condensed, di- gestible format so that participants will be able to return to their laboratories and put into practice what they have learned. The course outline includes basic toxicology, la- boratory hygiene, regulatory compliance, and related topics such as hazard communication. The last is especially important as labora- tories often mistakenly assume that their em- ployees know the hazards of the chemicals they handle. As the close of the course, at- tendees receive a certificate of completion. For space availability or more informa- tion, please contact Carol Rouse at +1 (703) 522-3032, or write to AOAC, 2200 Wilson Boulevard, Suite 400, Arlington, VA 22201- 3301, USA.

ISSN:0144-557X    

DOI:10.1039/AP9912800305

出版商:RSC    

年代:1991

数据来源: RSC

摘要:

306 ANALYTICAL PROCEEDINGS, SEPTEMBER 1991, VOL 28 Publications Received Pharmaceutical Drugs International Agency for Cancer. ZARC Monographs on the Evaluation of Carci- nogenic Risks to Humans. Volume 50. Pp. 41 5. World Health Organization. 199 1. Price SwFr65.00. ISBN 92-832- 1240-9. ces. Volume 47. Pp. viii + 309. Marcel Dek- Advances in BioSensors ker. 199 1. Price $99.75 (US and Canada); Edited by Anthony P.F. Turner. Volume 1. Pp. $1 14.50 (all other countries). ISBN 0-8247- xii + 299. JAI Press. 1991. Price E54.00; US 8499-5. $92.50. ISBN 1-559382-40-6. Report of the Proceedings of the 20th Ses- sion, Colorado Springs, June 3-8 1990 International Commission for Uniform Meth- ods of Sugar Analysis. Pp. xxxvi + 410. ICUMSA. 1991. Price E40.00. ISBN 0- 905003 - 1 2-8.Iron Oxides in the Laboratory. Preparation and Characterization U. Schwtermann and R.M. Cornell. Pp. xiv + 137. VCH. 1991. Price DM118.00; E45.00. ISBN 3-527-26001-6: 0-89573-858-9. HPLC in the Pharmaceutical Industry Edited by Godwin W. Fong and Stanley K. Lam. Drugs and the Pharmaceutical Scien- Applications Of Plasma Source Mass spec- Catalytic Antibodies Ciba Foundation Symposium 159. Pp. ix + trometry Edited by Grenville '''land and Andrew N* 259. Wiley-Interscience. 199 1. Price E39.50. Eaton. Royal Society of Chemistry. 1991. Pp. ISBN 0-471 -92962-X. viii + 222. Price E37.50. ISBN 0-85 186-566- 6. Calixarenes Factor Analysis in Chemistry C. David Gutsche. Monographs in Supra- xii + 350. wiley. 1991. price ~43.70. ISBN Society of Chemistry. 1991. Price E39.50. Edmund R.Malinowski. Second Edition. pp. tdecular Chemistry* Pp. xii + 224. 0-47 1-53009-3. ISBN 0-85 186-9 16-5. C ylcophanes Gas-Liquid-Solid Chromatography V.G. Berezkin. Chromatographic Science Francois Diederich. Monographs in Supra- Series. Volume 56. Pp. viii + 231. Price US molecular Chemistry. Pp. xv + 313. Royal $99.75 (US and Canada); US$14.50 (all other Society of Chemistry. 1991. Price E55.00. countries). ISBN 0-8247-845-1. ISBN 0-85 1 86-966- 1.EIGHT PEAK INDEX OF MASS SPECTRA 4th Edition The essential tool r mass spectrometrists! Available soon - the latest edition of the highly regarded Eight Peak Index of Mass Spectra. In the last 21 years this compilation has become the definitive printed aid for the identification of unknown mass spectra. KEY FEATURES OF THE EXPERT’S CHOICE OF INDEX INCLUDE: easy access to over 80,000 mass spectra via versatile indexing rapid identification of unknowns by simple intensity matching no difficulty identifying statistically important peaks spectra not currently available in any other commercial collections 15,000 new mass spectra and 25% more compounds over previous edition instant access without a computer Probably the best printed index of mass spectra in the world! ROYAL SOCIEJYOF CHEMISTRY For more information about the NEW edition and the pre-publication discount, simply contact us for a copy of our detailed leaflet. Write to: Kirsteen Ferguson, Sales and Promotion Department, Royal Society of Chemistry, Thomas Graham House, Science Park, Milton Road, Cambridge CB4 4WF, United Kingdom. Tel: 4 4 (0) 223 420066. Fax: +44 (0) 223 423623 Telex: 818293 ROYAL Information Services

ISSN:0144-557X    

DOI:10.1039/AP9912800306

出版商:RSC    

年代:1991

数据来源: RSC