ISSN:0144-557X    

DOI:10.1039/AP98926FX013

出版商:RSC    

年代:1989

数据来源: RSC

摘要:

ANPRDI 26(4) 121-148 (1989) Ana I yt ica I Proceedings Proceedings of the Analytical Division of The Royal Society of Chemistry CONTENTS 121 Reports of Meetings 122 Analytical Division Subject Groups 125 An a I ytica I Division Present at i o n s 125 Analytical Division Honours 126 SUMMARIES OF PAPERS 126 New Electrochemical Approaches to Clinical and Biochemical Analysis 'Evaluation of Ion-selective Field Effect Transistors for the Measurement of Ions in Whole Blood' by J. M. Thompson 126 128 Chemical Methods in Environmental and Clinical Analysis 128 130 'New Approaches to Reaction-rate Methods of Analysis' by Peter D. Wentzell 'Oxygen Radicals: Their Measurement In Vivo' by Joseph Lunec 'Carbohydrate and Protein Analysis of Plant Materials' by John F.Kennedy, Miss Z. S. 132 Rivera and C. A. White 133 'Progress in the Water Industry-Automation in a Water Company Laboratory' by Paul Hemmings 'Organolead Compounds in the Atmosphere' by P. J. Metcalfe 134 137 Equipment News 141 SAC 89: Update Courses 142 Recent IUPAC Recommendations 145 Conferences and Meetings 147 Courses 148 Analytical Division Diary Typeset and printed by Black Bear Press Limited, Cambridge, England April 1989 ... ANALYTICAL PROCEEDINGS. APRIL 1989, VOL 26 111 SERIES: RSC CHROMATOGRAPHY MONOGRAPHS SUPERCRITICAL FLUID CHROMATOGRAPHY Edited by Roger M. Smith Loughborough University of Technology SFC is the current focus of attention in the Chromatography world and Supercritical Fluid Chromatography is the first book devoted entirely to this rapidly expanding analytical technique. SFC promises to revolutionise analytical procedures in the petroleum, pharmaceutical, food, agrochemical and biotechnology industries, and this new publication will provide practising chromatographers in both industry and academia with a perspective on its principles, practice and potential applications. ISBN 0 85186 577 1 Hardcover 250pp. Price E27.50 ($55.00) For further information, please write to: Royal Society of Chemistry, Sales and Promotion Dept. Thomas Graham House, Science Park, Milton Road, Cambridge CB4 4WF, UK. RSC Members are entitled to a discount o:i most RSC publications and should write to the Membership Manager at the above address.

ISSN:0144-557X    

DOI:10.1039/AP98926BX015

出版商:RSC    

年代:1989

数据来源: RSC

摘要:

ANALYTICAL PROCEEDINGS, APRIL 1989, VOL 26 121 Scottish Region The fifty-fourth Annual General Meeting of the Region was held at 7.00 p.m. on Friday, November 4th, 1988, at the Uni- versity of Strathclyde, Glasgow. The Chair was taken by the Chairman of the Region, Mr. P. J. Stevens. The following office bearers were elected for the forth- coming year: Chairnian-Mr. P. J. Stevens. Vice-Chairman-Mr. A. D. Ruthven. Honorary Secretary-Mr. R. I. Aylott. United Distillers plc, Group Cen- tral Laboratory, Menstrie, Clackmannan- shire FKll 7ES. Honorary Treasurer- Dr. J. M. Warren. Honorary Assistant Secretary-Mr. E. C. Smith. Members of Covznzittee-Mr. M. J. Durey, Dr. J. Farmer, Mr. M. F. Godfray, Mr. P. Ms. Holroyd and Mr. A. B. MacKenzie. Dr. R. A. Chalmers and Dr. J. E. Whitley were re-appointed as Honorary Auditors.North East Region The twenty-third Annual General Meet- ing of the Region was held at 1.30 p.m. on Wednesday, November 16th, 1988, at Sheffield City Polytechnic. The Chair was taken by the Chairman of the Region, Mr. G. Penketh. The following office bearers were elected for the forthcoming year: Chairman-Mr. G. Penketh. Vice-Chair- man-Dr. P. J. Worsfold. Honorary Sec- retary-Dr. J. Marshall, ICI plc, Wilton Materials Research Centre, Materials Analysis and Testing Group, P.O. Box 90, Wilton, Middlesbrough, Cleveland TS6 8JE. Honorary Treasurer-Mr. M. Daniel. Honorary Assistant Secretary- Mr. J. Page-Gibson. Members of Corn- mittee-Dr. W. C. Campbell, Dr. D. J. Mowthorpe, Dr. J. D. Green, Dr. R. N. Reeve, Mr. S. Cave, Dr. J.R. Dean and Professor A. Townshend (ex officio). Mr. F. C. Shenton and Mr. J. Whitehead were re-appointed as Honorary Auditors. East Anglia Region The twenty-first Annual General Meeting of the Region was held at 2.15 p.m. on Tuesday, November 15th. 1988, at Uni- lever Research, Sharnbrook. The Chair was taken by the Chairman of the Region, Mr. A. M. C. Davies. The following office bearers were elected for the forth- coming year: Chairman-Mr. R. P. Mun- den. Vice-Chairrziaiz-Dr. C. Creaser. Honorary SecrerarylTreasurer-Mr. P. R. Brawn, Unilever Research, Colworth Laboratory, Sharnbrook, Bedfordshire MK44 ILQ. Honorary Assisrant Secre- tary-Mr. P. Snowdon. Members of Conz- mittee: Mr. A. M. C. Davies (immediate past Chairman), Mr. B. W. Woodget, Mr. A. Anderson, Mr.A. Henderson, Dr. M. S . Moss, Dr. M. G. Kibblewhite, Mrs. S. Dawes and Dr. A. Brown (co-opted). Mr. A. G. Croft and Mr. C. Waterhouse were re-appointed as Honorary Auditors. South East Region The fourteenth Annual General Meeting of the Region was held at 3.15 p.m. on Wednesday, December 7th, 1988, in the Geological Society Lecture Theatre, Burlington House, London. The Chair was taken by the Chairman of the Group, Mr. G. F. Phillips. The following office bearers were elected for the forthcoming year: Chairman-Mr. G. F. Phillips. Vice-Chairman-Mr. D. W. Houghton. Honorary Secretary-Dr. A. H. Andrews, Beecham Pharmaceuticals, Clarendon Road, Worthing, West Sussex BN14 8QH. Honorary Treasurer-Mr. D. Blair. Honorary Assistant Secretary-Mr. P. J. O’Neil.Honorary Youth Liaison Officer-Mr. D. W. Houghton. Members of Committee-Dr. R. M. Belchamber, Mr. R. Goulden, Dr. J. E. Newbery, Dr. J . E. Davies (co-opted), Mr. H. I. Shal- gosky (co-opted) and Dr. J. G . Firth (ex officio). Dr. J. E. Page and Mr. D. C. M. Squirrel1 were re-appointed as Honorary Auditors. Micro & Chemical Methods Group The forty-fifth Annual General Meeting of the Group was held at 1.30 p.m. on Wednesday, November 30th, 1988, in the Medical School, Birmingham University. The Chair was taken by the Chairman of the Group, Mr. C. A. Watson. The following office bearers were elected for the forthcoming year: Chairman-Mr. M. J. Graham. Vice-Chairman-Mr. C. A. Watson. Honorary Secretary-Mr. P. R. W. Baker, 55 Braemar Gardens, West Wickham, Kent BR4 OJN.Honor- ary Treasurer-Mr. M. R. Cottrell. Mem- bers of Committee-Mrs. D. E. Butter- worth, Miss L. Dixon, Dr. M. A. Russell, Dr. E. Vidgeon, Mr. M. J . West, Mr. A. Fassam and Dr. E. J. Newman (ex offi- cio). Mr. H. I. Shalgosky and Mr. B. T. Saunderson were re-appointed as Honor- ary Auditors. Atomic Spectroscopy Group The twenty-fourth Annual General Meet- ing of the Group was held at 6.00 p.m. on Wednesday, November 30th, 1988, at Imperial College, London. The Chair was taken by the Chairman of the Group, Dr. N. W. Barnett. The following office bearers were elected for the forthcoming year: Chairman-Dr. M. S. Cresser. Vice- Chairman-Dr. J. Marshall. Honorary Secretary-Dr. J. R. Dean, Department of Chemical and Life Sciences, Newcastle upon Tyne Polytechnic, Ellison Terrace, Ellison Place, Newcastle upon Tyne NE1 8ST.Honorary Treasurer-Dr. D. R. Hickman. Honorary Assistant Secretary-Mr. C. A. Watson. Members of Committee-Dr. N. W. Barnett, Dr. J. Carroll, Dr. S. Corr, Dr. A. T. Ellis, Dr. S. J. Hill, Dr. M. Thomsen and Dr. M. Thompson. Mr. T. Catterick and Mr. P. Sadler were appointed as Honorary Auditors. Chromatography and Electrophoresis Group The twenty-fourth Annual General Meet- ing of the Group was held at 2.30 p.m. on Thursday, December 8th, 1988, at King’s College, London. The Chair was taken by the Chairman of the Group, Dr. P. J. Houghton. The following office bearers were elected for the forthcoming year: Chairman-Dr. P. J. Houghton. Vice- Chairman-Dr. F. K. Butcher. Honorary Secretary1 Treasurer-Dr, D.Simpson, Analysis For Industry, Factories 213, Bos- worth House, High Street, Thorpe-Le- Soken, Essex C016 OEA. Members of Committee: Dr. R. G. Hopkins, Dr. J. Benner, Dr. C. Creaser, Dr. S . B. Laing, Dr. R. M. Smith and Mr. N. G. McTag- gart (co-opted). Mr. G. H. Mitchell and Mr. L. R. F. J . Ferandes were re-appoin- ted as Honorary Auditors. Thermal Methods Group The twenty-fourth Annual General Meet- ing of the Group was held at 12.30 p.m. on Thursday, November loth, 1988, at the Scientific Societies‘ Lecture Theatre. London. The Chair was taken by the Chairman of the Group, Mr. P. J . Haines. The following office bearers were elected for the forthcoming year: Chairman-Mr. P. J. Haines. Vice-Chairman-Mrs. J . A. Hider. Honorary Secretary-Dr . C. J . Keattch, Industrial and Laboratory Ser- vices, P.O. Box 9, Lyme Regis, Dorset DT7 3BT.Honorary Treasurer-Dr. R. H. Still. Members of Committee-Dr. J. M. Barton, Miss J. G. Griffiths, Mr. C. Jones, Dr. D. J. Morgan, Professor D. V. Nowell, Dr. F. R. Sale, Dr. A. Smith, Dr. G. M. Clark (co-opred). Dr. R. C. Mackenzie (co.opted) and Dr. F. W. Wilburn (co-opted). Dr. A. Dyer and Mr. D. Griffiths were re-appointed as Honorary Auditors. Automatic Methods Group The twenty-third Annual General Meet- ing of the Group was held at 1 .00 p.m. on Thursday, December 8th, 1988, at The Scientific Societies’ Lecture Theatre, Sav- ile Row, London. The Chair was taken by the Vice-chairman of the Group, Mr. R. Lidgett. The following office bearers were elected for the forthcoming year: Chair- man-Mr.K. J. Leiper. Vice-Chairman- Mr. R. Lidgett. Honorary Secretary-Dr.122 C. J. Jackson, Health and Safety Execu- tive, Steel City House, Broad Lane, Sheffield S3 7HQ. Honorary Treasurer- Dr. A. Braithwaite. Honorary Assistant Secretary-Dr. T. Lilley . Honorary Minutes Secretary-Mrs. E. Evans- Terlecki. Members of Committee-Mr. F. R. B. Fearn, Dr. M. A. Ford, Dr. M. Head, Dr. A. S. McLelland, Mr. D . G. Porter and Dr. K. J. Saunders. Dr. J. E. Page and Mr. R. Sawyer were re-ap- pointed as Honorary Auditors. Particle Characterisation Group The twenty-third Annual General Meet- ing of the Group was held at 2.00 p.m. on Tuesday, November 29th, 1988, at the Linnean Society, London. The Chair was taken by the Chairman of the Group, Mr. P. J. Lloyd.The following office bearers were elected for the forthcoming year: Chairman-Dr. M. I. Barnett. Vice- Chairman-Dr. J. P. K. Seville. Honor- ary Secretary-Dr. N. A. Orr, Research Division, Beecham Pharmaceuticals, Clarendon Road, Worthing, West Sussex BN14 8QH. Honorary Treasurer-Mr. R. W. Lines. Honorary Assistant TreasurerlSecretary-Mr. J. E. C. Harris. Members of Committee-Dr. K. Birch, Mr. C. J. Price, Dr. A. Rood, Mr. M. Till, Mr. P. J. Lloyd (ex officio), Dr. J. Mitchell (co-opted) and Dr. N. G. ANALYTICAL PROCEEDINGS, APRIL 1989. VOL 26 Stanley-Wood (co-opted). Mr. J. Spence was re-appointed as Honorary Auditor. Radiochemical Methods Group The twenty-second Annual General Meeting of the Group was held at 1.45 p.m. on Wednesday, November 9th, 1988, at MAFF, Weybridge.The Chair was taken by the Chairman of the Group, Dr. A. Ware. The following office bearers were elected for the forthcoming year: Chairman-Mr. A. Lally. Vice-Chair- man-Dr. J. Troke. Honorary Secretary -Mr. M. Crook, London School of Polymer Technology, Polytechnic of North London, Holloway Road, London N7 8DB. Honorary Treasurer-Dr. A. Palmer. Honorary Assistant Secretary- Dr. P. Warwick. Members of Committee -Mr. T. Bates, Mr. B. Lovett, Dr. J. Hislop, Dr. P. Robb, Dr. D. Tidy and Dr. A. Ware (ex officio). Mr. G. Farmer was re-appointed as Honorary Auditor. Electroanalytical Group The nineteenth Annual General Meeting of the Group was held at 2 p.m. on Friday, December 9th, 1988, at Canterbury Hall, London. The Chair was taken by the Chairman of the Group, Professor M.L. Hitchman. The following office bearers were elected for the forthcoming year: Chairman-Professor A. K. Covington. Vice-Chairman-Mr. D. Thomason. Honorary Secretary-Mr. A. E. Bottom, Kent Industrial Measurements Ltd., Oldends Lane, Stonehouse, Gloucester- shire GLlO 3TA. Honorary Treasurer- Dr. B. J. Birch. Honorary Assistant Secre- tary-Dr. J. P. Hart. Members of Com- mittee-Dr. P. N. Bartlett, Dr. E. A. H. Hall, Dr. K. Gibbs, Dr. J . Thompson, Dr. J. M. Slater, Dr. C. M. G. van den Berg, Dr. A. G. Fogg (co-opted) and Professor M. L. Hitchman (ex officio). Mr. J. D. Tillman and Dr. R. M. Smith were re-appointed as Honorary Auditors. Molecular Spectroscopy Group The second Annual General Meeting of the Group was held at 1.40 p.m. on Thursday, November 24th, 1988, at Birk- beck College, London. The Chair was taken by the Chairman of the Group, Professor A. Townshend. The following office bearers were elected for the forth- coming year: Chairman-Mr. A. M. C. Davies. Vice-Chairman-Dr. R. A. Spragg. Honorary Secretary-Dr. M. E. Rose, Department of Chemistry, The Open University, Walton Hall, Milton Keynes MK7 6AA. Honorary Treasurer -Dr. P. J. Worsfold. Members of Com- mittee-Dr. D. L. Andrews, Mr. J. M. Chalmers, Dr. A. D. H. Clague and Professor A. F. Fell. Dr. J. D. Green and Mr. G. F. Collier were re-appointed as Honorary Auditors.

ISSN:0144-557X    

DOI:10.1039/AP9892600121

出版商:RSC    

年代:1989

数据来源: RSC

摘要:

122 ANALYTICAL PROCEEDINGS, APRIL 1989. VOL 26 Analytical Division Subject Groups Many of the activities of the Analytical Division are organised by “Subject Groups” which currently are: Atomic Spectroscopy Automatic Methods Biological Methods Chemometrics Chromatography and Electrophoresis Electroanalytical Micro and Chemical Methods Molecular Spectroscopy Particle Characterisation Radiochemical Methods Thermal Methods Pharmaceutical Analysis (joint with the Pharmaceutical Society) These Groups arrange meetings, which are “technique orientated” and therefore complement meetings organised by Regions, which are mainly “applications” based. Following a report to Council by a Working Party on Group activities,’ it was decided to hold a review of the activities of about three Groups each year, so that each Group would be able to demonstrate its progress in meeting its remit about once every 4 years.The first of these reviews took place at the January meeting of the GLPC and summaries of the presentations made by the Groups appear below. I would also like to remind members of the excellent value of Group(s) member- ship for RSC members and that all the Groups are very pleased to receive sug- gestions for meeting subjects and venues. New members are particularly welcome; it is often they who bring new ideas to the attention of the Group Committees and ensure the continuing development of their activities and thus the best possible service to all the members. Reference 1. Watson, C. A . , A n d . Proc., 1987, 24, 161. COLIN WATSON Biological Methods Group The Biological Methods Group of the Analytical Division, Royal Society of Chemistry, is composed primarily of people interested in using biological systems as analytical tools, in particular techniques based on the specific biochem- ical interactions occurring in living systems.The Group was inaugurated in October, 1945, as a Group of the Society of Public Analysts and other Analytical Chemists, and was concerned principally with methods for the bioassay of anti- biotics, antiviral agents, hormones, etc. Nowadays, with the advent of biotechnol- ogy, the Group is interested in: Biosensor Technology; Immuno-Diagnostics and Other Receptor-based Assays; Nucleic Acid Probe Technology and Applica- tions; Biospecific Affinity Chromato- graphy, etc.Recent meetings of the Group have included the following titles: Principles and Problems in Testing for AIDS; State of the Art and Future Potential of Nucleic Acid Probes; Analy- tical Applications of Lectins; Automated Microbiological Analysis; New Fields for Drug and Antigen Targetting; Analysis of Foodstuffs. Many of these meetings are held jointly with other Groups and Regions of the Analytical Division, with other RSC Divisions and, more rarely, with other Scientific Societies. Extended summaries of papers presen- ted at Group meetings are generally published in the RSC journal Analytical Proceedings. The AGM of the Group is generallyDate May 1985 Sep 1985 Oct 1985 Nov 1985 Dec 1985 Feb 1986 Mar 1986 Oct 1986 Oct 1986 Nov 1986 Nov 1986 Jan 1987 Feb 1987 Apr 1987 Oct 1987 Nov 1987 Dec 1987 Jan 1988 Feb 1988 May 1988 Oct 1988 Nov 1988 Nov 1988 Nov 1988 ANALYTICAL PROCEEDINGS.APRIL 1989. VOL 26 Table 1. Micro and Chemical Methods Group. Programmes for 1985-1988 123 Subject Standardisation and Certification of Reference Materials Whats New in CHN (User Forum) Spectroscopy of Small Samples Forensic Application of Enzyme-linked Assay (Disc) Karl Fischer Determination of Water (Disc) Recent Developments in FIA (Disc) Determination of Oxygen and Sulphur (User Forum) Analysis of Asbestos Ion Chromatography (Disc) Role of Classical Analysis in Present Day Analytical Chemistry Quality Assurance (Disc) Optical Microscopy (Disc) Modern Titrimetry How to Get the Best from Your Analyser (User Forum) Small Scale Manipulation (Disc) Practical Chemical and Biological Sensors Hot Stage Microscopy (Disc) Sample Preparation in Food Analysis (Disc) Physical Characterisation of Medical Substances Whats New?/Low Levels of NitrogeniLists of Spares (User Forum) Chemiluminescence Microwave Sample Digestion Handling Hazardous Substances ICP-MS Length f day f day I day 2 h 2; h 2 h 1 day day 1 day 2+h + day 2 h 2 h 2 days 1 day 2 h 2 h 24 h 1 day 1 day 2 h 4 day 1 day 2 days No.45 60 3 0 20 22 17 35 50 67 35 60 17 17 37 60 12 150 17 21 110 62 19 10s 32 Joint - - ST BM - - AS - - - E&T - - Mid - - AD PC JPAG MS AS - - - held in November of each year in Lon- don, and includes a “lay-talk” of scientific interest together with a buffet and wine, to which Members are encouraged to bring family guests.Membership of the Group currently stands at about 400, and consists of scientists from academia, industry, the Scientific Civil Service and the Health Services. Approximately 11% of the membership is from outside the UK. Persons with expertise in the Group’s fields of interest are always welcome to enquire about vacancies on the BMG Committee. Prospective meet- ings include the following titles: May l l t h , 1989, “QA of Biologicals: Analy- tical Implications”; June 28th, 1989, “New Applications for Antibodies ’‘ ; October 24th, 1989, “Consumer - D.I.Y. Diagnostics”; November 16th, 1989, AGM and “Drugs in Sport.” For further information please contact the Group Secretary: Alan Crooks, Mole- cular Virology Group, Biologics Division, PHLS CAMR, Porton Down, Salisbury, Wiltshire SP1 3PH.(Tel: 0980-610391, Ex. 382). Micro and Chemical Methods Group The Micro and Chemical Methods Group is the oldest subject Group in the Analy- tical Division and was formed in 1944. It was known then as the Microchemistry Group and was founded to cater for the needs of the considerable body of analysts using the microchemical techniques pioneered by Pregl, Emich and others. In 1964 the name was modified to the “Microchemical Methods Group” and again in 1986 to the “Micro and Chemical Methods Group”, to take into account changes in emphasis and future require- ments. The group remit early in this review period was updated and its terms of reference are now: “The analysis of small samples, including elemental and func- tional group analysis, relevant techniques involving microscopy, chemical methods including sample preparation, chemical standards, chemical separations, classical analysis and chemistry as applied to other techniques.” This broad and all encom- passing remit is deemed useful as it serves to cover aspects of the chemistry and methods that are generally applicable to other analytical techniques, e.g., sample preparation.For this reason, some of our meetings are organised jointly with other Groups. The more specific parts of the remit, Elemental and Functional Group Analysis, are covered by our Elemental Analysis User Forum. Meetings range from informal discus- sions of about 2-h duration to traditional scientific meetings of 1-2 days. Our User Forum combines two approaches, where users are given the opportunity to share their experience and manufacturers are given the opportunity to present details of their latest developments, sometimes dis- playing equipment and giving demonstra- tions. (The Group always takes great care to ensure that no bias can be inferred from the choice of speakers.) Through the user Forum we canvass members’ opinions and organise collaborative practical work, for example the performances of micro- balances and carbon, hydrogen and nitrogen analysers.During the past four years, all aspects of our remit have been covered. We try to cater for small minority interests as well as major topics of interest. This is illustrated in the past diary of events in Table 1. Financially, the Group aims to provide a programme of meetings at reasonable cost and prudent planning ensures that we do not generate an unnecessarily large surplus in our account.We believe that the financial support provided by the Society should be invested in the educa- tion of chemists (in the broadest sense) and the furtherance of chemistry. Clearly, the profit or loss on any meeting is very dependent on the attendance and it is not possible to predict this with any accuracy. Table 1 shows the considerable variation in numbers attending the various meet- ings, many of which were fairly accurately predicted. It is our policy to encourage the attendance of students whenever pos- sible and they are normally admitted either free or at minimal charge, as are our retired members. Our future pro- grammes are already being planned and we would encourage members to read the bulletin and non-members who have an interest in our activities to become members.Forthcoming meetings include “Small Scale Sample Handling” and “Trace Ele- ments Analysis,” as well as a one-day symposium on “Chemical Methods of Analysis” at SAC 89. For further details of Group activities and any suggestion for meetings (or a venue for a meeting) please contact the Honorary Secretary of the Group, P. R. W. Baker, 55 Braemar Gardens, West Wickham, Kent, BR4 OJN. (Tel. 0 1-777- 1225). Atomic Spectroscopy Group The remit of the Atomic Spectroscopy Group (ASG) is to cover all aspects of analytical atomic spectroscopy including relevant techniques of surface analysis. The officers and committee members of the ASG responsible for the organisation of the scientific programme for 1988189 are: Chairman, Dr.M. S. Cresser (Uni- versity of Aberdeen); Vice-chairman, Dr. J. Marshall (ICI Wilton Materials Research Centre); Honorary Secretary, Dr. J. R. Dean (Newcastle upon Tyne Polytechnic) ; Honorary Assistant Secre- tary, Mr. C. A. Watson (Consultant),124 ANALYTICAL PROCEEDINGS. APRIL 1989, VOL 26 Table 1. Topics of Atomic Spectroscopy Group meetings held over the period 1984-1988 Topic Inductively coupled plasma atomic emission spectrometry X-ray analysis Atomic absorption spectroscopy Inductively coupled plasma mass spectrometry Inorganic trace analysis Microwave digestion Training requirements Hyphenated techniques, e.g., coupled chromatography - atomic spectroscopy General atomic spectroscopy, e.g..BNASS, ASU Number of meetings 2 2 2 3 1 1 1 1 11 Honorary Treasurer, Dr. D. A. Hickman (Metropolitan Police Forensic Science Laboratory). The committee members are: Dr. J. Carroll (ICI Chemicals and Polymers), Dr. S. J. Hill (Plymouth Poly- technic), Dr. M. Thompson (Birkbeck College), Dr. A. T. Ellis (Link Analy- tical) and three co-opted members, J. Egan (RSC), Dr. M. Thomsen (Perkin- Elmer) and Dr. S. Corr (ICI). The immediate Past-Chairman is Dr. N. W. Barnett (ICI Chemicals and Polymers). Meetings A summary of the topics of ASG meetings held over the period 1984-1988 is shown in Table 1. Table 2 lists the venues and co-sponsors of ASG meetings over the same time period. Included in these lists are two meetings which are held annually and biennially, respectively.The first is the Atomic Spec- trometry Updates meeting, prior to 1986 the Annual Reports on Analytical Atomic Spectroscopy Symposium, covering aspects of analytical atomic spectroscopy. In 1989 the meeting was held at Strathclyde University on March 29th- 30th, the theme being “Analytical Atomic Spectroscopy in the Environment.” July 18th-20th, 1990, will see the fifth in the series of meetings Biennial National Atomic Spectroscopy symposium (BNASS), when the venue will be Lough- borough University . The ASG will again participate in SAC ’89, (SAC ’86 being held in conjunction Table 2. List of Atomic Spectroscopy Group Meeting venues and co-sponsors 1984-1988 Year 1984 1984 1984 1984 1984 1984 1985 1985 1985 1986 1986 1985 1986 1986 1987 1987 1987 1987 1988 1988 1988 1988 Venue Sheffield City Polytechnic University of Strathclyde University of Leeds (2nd BNASS) Stockton-on-Tees (Ti oxide Cent r a I Labor at o r i e s ) Norwich (Food Research Institute) London (AGM) (Geological Society) London (Savoy Tavern) Sheffield City Polytechnic Bristol University Sheffield City Polytechnic (AGM) London (Geological Society) Sheffield City Polytechnic Bristol University (3rd BNASS) Imperial College (AGM) Thames Polytechnic University of East Anglia Plymouth Polytechnic UMIST (AGM) University of Hull University of York (4th BNASS) Thames Polytechnic Imperial College (AGM) Co-sponsor(s) of meetings Annual Reports on Analytical Atomic Spectroscopy Symposium and Sheffield Metallurgical and Engineering Association Scottish Region Spectroscopy Group of the Institute of Physics North East Region- East Anglia Region Education and Training Group? Microchemical Methods Group+ Annual Reports on Analytical Atomic Spectroscopy Symposium and Sheffield Metallurgical and Engineering Association Western Region North East Region Microchemical Methods Group- Atomic Spectrometry Updates and Sheffield Metallurgical and Engineering Association Spectroscopy Group of the Institute of Physics Atomic Spectrometry Updates Automatic Methods Group and East Anglia Region Western Region and Peninsula Section Atomic Spectrometry Updates, Molecular Spectroscopy Group, North East Region and UV Spectrometry Group Spectroscopy Group of the Institute of Physics Micro and Chemical Methods Group and South East Region ’ Meeting on inductively coupled plasma atomic emission spectrometry and X-ray analysis.f Defunct Group. Re-named Micro and Chemical Methods Group.ANALYTICAL PROCEEDIXGS. APRIL 1989. VOL 36 with the 3rd BNASS). to be held at Cambridge University between July 30th and August 5th. 1989. An ASG session will incorporate a meeting on Inductively Coupled Plasma Mass Spectrometry. a Memorial to the late Dr. A. R. Date. Future meetings for 1989 include a meet- ing on "Chemometrics in Atomic Spectro- scopy." to be held jointly with the Chemometrics Group, at Thames Poly- technic on November 1st and a meeting on "X-ray Methods," jointly with the .Midlands Region. in Hereford on Novem- ber 22nd. 1989. Conclusions Reference to Tables 1 and 2 demonstrates how the ASG has complied with its remit.The recent introduction into the remit of relevant areas of surface analysis is emerging in the scientific programme. for example, the scanning electron micro- scope. January IXth, 1989. The atten- dance at meetings is usually good. Excel- lent attendances (200-250 delegates) are regularly achieved at the BNASS meet- ings. Other well attended meetings include the ASU meetings and state of the art meetings. such as Sample Jntroduction Into the Inductively Coupled Plasma, Bristol. 1985. Throughout the ASG programme regular joint meetings are held with other Groups and Regions of the RSCiAD. The following Groups and Regions have been involved with the ASG since 1984/85: North East Region, East Anglia Region.Scottish Region. South East Region, Mid- lands Region. Western Region and the Peninsula Section of the RSC, Education and Training Group. Automatic Methods Group, Micro and Chemical Methods Group and the Chemometrics Group. We would therefore like to take this I25 opportunity t o express our thanks to the above mentioned Regions and Groups for their co-operation and hope that future meetings can be organised equally effi- ciently and in a scientifically stimulating manner. It is also hoped that our pro- gramme will enable us to combine with all of the Regions and most of the other Groups in the foreseeable future. Finally. if any members of the ASG would like t o suggest topics and/or venues for future scientific meetings. please contact the Honorary Secretary at the address given below.For further information contact Dr. J. R. Dean. Department of Chemical and Life Sciences, Newcastle upon Tyne Poly- technic, Ellison Terrace. Ellison Place. Newcastle upon Tyne YE1 8ST. (Tel. 06 1-232-6002. EX. 35 17). Analytical Division Presentations During the lunch break of the Analytical Division Council Meeting held on Febru- ary 22nd. 1989. presentations were made to two long serving RSC employees who were about to take early retirement as an alternative to moving to the new RSC office at Cambridge. The President of the Division. Professor D. Thorburn Burns. first presented Mr. P. W. Shallis with a of an ornithologist's telescope to Mrs. number of Edinburgh Crystal glasses. Mr R. L. Jordan, the Product Manager of Shallis. who had completed 32 years' Anulyticcll Absrrcicts, who had completed service. had been the Assistant Editor of 25 years' service to the SAC and RSC. The Ancilysr. the Secretary of the Analy- The presentations were made in the Hin- tical Methods Committee and. more shelwood Room of Burlington House. recently, the Editor of Analytical Books. The President next made a presentation Analytical Division Honours The Council of the Analytical Division. at fessor J. H. Purnell (University of Swan- Awards have been awarded to Dr. G . B. its meeting on December 12th. approved sea). The 1989/90 Schools Lecturer will be Marshall (Central Electricity Generating the following recommendations from it\ Professor D. Littlejohn (Strathclyde Uni- Board. Leatherhead) and Dr. J. F. Tyson Honours Committee. The 1990 Theo- versity). The seventeenth and eighteenth (Loughborough Univer\ity of Technol- philus Redwood Lecturer will be Pro- Analytical Division Distinguished Service ogy).

ISSN:0144-557X    

DOI:10.1039/AP9892600122

出版商:RSC    

年代:1989

数据来源: RSC

摘要:

126 ANALYTICAL PROCEEDINGS, APRIL 1989, VOL 26 New Electrochemical Approaches to Clinical and Biochemical Analysis The following is a summary of one of the papers presented a t a Joint Meeting of the Scottish Region and the Association of Clinical Biochemists held on June 8th, 1988, in the University of Stirling. ~ ~ ~~ Evaluation of Ion-selective Field Effect Transistors for the Measurement of Ions in Whole Blood J. M. Thompson University of Birmingham, Anaesthetics Department, Clinical Research Block, Queen Elizabeth Hospital, Birmingham B75 2TH and Thorn €MI Central Research Laboratories, Dawley Road, Hayes, Middlesex UB3 - 7 HH Although ion-selective field effect transistors (ISFETs) have been used experimentally for cation measurement in whole blood by various groups,*-j both in vitro and in vivo, such devices have previously not been suitable for large-scale manufacturing (in the range of hundreds of thousands or of millions of devices per year).This can readily be inferred from the absence of any commercially available instruments using ISFETs. However, recent developments at THORN EMI, in the automated deposition and patterning of electroactive films and in encapsulation techniques suitable for large volume production, together with other advances in the formulation of stable electroactive films and in composite gate construction, have enabled useful devices to be manufactured (D. Pedley and P. Whalley, personal communication).j These devices have been undergoing detailed clinical evaluation and trialling in order to determine their suitability for use in “near the patient” clinical measurement systems. In designing suitable approaches to the evaluation and trialling, account must be taken of the different modes of use of “near the patient” systems compared with standard clinical chemistry equipment.Nonetheless, performance comparisons must be made against such equipment, in order that the new equipment might gain acceptance by both clinical chemists and by the various clinicians who may be the ultimate users. Examples of the various types of trialling are presented, along with a brief discussion of some of their advantages and disadvantages. Evaluating Reproducibility Tests can be performed with a wide variety of materials ranging from single substance calibrant solutions to whole blood. The “matrix” effects of these different media produce different patterns of reproducibility. For example, the ISFET5 were compared with two conventional ISE based potassiumisodium analysers, commonly used in clinical chemistry laboratories (the Radiometer KNAl and the Corning 902), and a “coated wire” type of single use ISE card system (the Chempro 500) recently introduced to the clinical market.In one test, pre-packaged liquid quality control materials (suitable for use with ISE analysers) were used which were designed to mimic the properties of human serum in respect of the assayed constituents. The results are shown in Table 1. In another test, heparinised whole arterial blood was used as the test material and the results are shown in Table 2. It is immediately apparent that for the coated wire ISE cards there is a vast difference in behaviour between the q.c.materials and whole blood. There are also considerable differences for the Corning 902 but much less marked differences for the Radiometer KNAl and the ISFET. In terms of the needs of clinicians, the tests with whole blood are much more relevant because this is the medium being tested by them in a “near the patient” scenario. This sort of comparison raises questions not only about instrument evaluation but also about local and external quality assurance and the value of synthetic quality assurance materials other than for diagnosis of instru- ment behaviour for maintenance purposes. Comparisons Between Instruments by Regression Analysis Comparisons were made by measuring the same sample with Table 1.Reproducibility tests using NOVA q.c. materials for potassium ion measurements ([K+] in mmol 1-I). The number of replicates at each level for each instrument tested was 12 THORN EM1 Microsensors Level NOVA Radiometer Corning Chempro no. value KNAl 902 500 ISFET 1 ISFET 2 1 Mean 2.3 2.54 2.26 2.03 2.97 3.03 S.d. 0.116 0.026 0.123 0.094 0.092 C . V . 4.6% 1.2”/” 6.1% 3.2% 3 . 0 ”% 2 Mean 3.9 4.07 3.72 3.47 3.12 3.22 s.d. 0.065 0.035 0.089 0.12 0.16 C.V. 1.6% 1 .O% 2.6% 3.W” 3.9% 3 Mean 6.5 6.32 6.43 5.95 6.30 6.32 S.d. 0.072 0.058 0.25 0.18 0.15 C.V. 1 . 1 % 0.9”/0 4.3% 2.9% 2.5%ANALYTICAL PROCEEDINGS, APRIL 1989. VOL 26 127 Table 2. Reproducibility tests of potassium ion measurement in whole blood samples ([K+] mmol 1 - 1 ) THORN EM1 Radiometer Corning Chempro Microsensors KNAl 902 500 ISFET Combined 5.d.of all sets of replicates 0.0677 0.162 0.433 0.164 Over-all sample mean 3.28 4.28 4.05 4.10 Combined coefficient of variation. ’% 1.58 3.79 10.7 4.00 Number of sets of replicates 34 33 34 34 Total number of replicates 89 88 89 89 each instrument being evaluated. Two standard laboratory ISE analysers were tested as a means of checking on sample handling. In assessing the relative performance of one system compared with another, the regression of the measurements with the ISFET or the coated wire ISE systems (as the y variable) against measurements with the standard ISE instru- ment (as the x variable) were calculated to determine whether there was significant constant or proportional bias between 6.6 1 5.6 z 5 4.6 Y t I Ii LL 3.6 2.6 1.6 I ’ I 2.1 3.1 4.1 5.1 6.1 [ K + ] i m ~ (Radiometer KNAI) Fig.1. Regression of TEM K + ISFET whole blood potassium ion measurement against Radiometer KNAl measurements. Regression equation, Y = -0.08 + 0.96 X: correlation coefficient, 0.94: coefficient of determination, 88.6% : number of measurements. 132 them. The correlation coefficient was also calculated and used as an indicator of the degree of agreement between measure- ments on the various systems. An example of the regression analysis is shown in Fig. 1 for the comparison of the ISFET with the Radiometer KNAl and in Fig. 2 for comparison of the Corning 902 with the Radiometer KNAl for potassium ion measurements in whole blood. The plot in Fig. 1 suggests a strong relationship between the measurements with the ISFET and the Radiometer, which is very similar to that between the Corning and the Radiometer. Along with the results of the reproducibility tests, this suggests that ISFETs that are suitable for incorporation in commercial “near the patient” analysers can now be manufactured reliably. 7 L 2.1 3.1 4.1 5.1 6.1 [ K + ] / ~ M (Radiometer KNA1) Fig. 2. Regression of Corning 902 K i ion measurements in whole blood on Radiometer KNAl measurements. Regression equation. Y = -0.14 + 1.03 X; correlation coefficient, 0.96: coefficient of determina- tion, 92.5% : number of measurements. 140 References 1. 2. 3. 4. Janata, J . , and Huber, R. J.. “Ion-sensitive Field-effect Transis- tors,” Ion Sel. Electrode Rev. 1980. 1 . 31. Hirst, A. D., and Stevens. J . F.. Ann. Clirz. Biochem., 1985.22. 460. Sibbald. A . , J. Mol. ElcctronicJ. 1986. 2, 51. Pedley. D., and Whalley. P., Personal Communication.

ISSN:0144-557X    

DOI:10.1039/AP9892600126

出版商:RSC    

年代:1989

数据来源: RSC

摘要:

128 ANALYTICAL PROCEEDINGS. APRIL 1989. VOL 36 Chemical Methods in Environmental and Clinical Analysis ~~ The following are summaries of five of the papers presented at the Analytical Symposium of the RSC's Autumn Meeting, held on September 20th-21st, 1988, in the University of Birmingham. New Approaches to Reaction-rate Methods of Analysis Peter D. Wentzell Department of Chemistry, University of British Columbia, Vancouver, British Columbia, Canada, V6T I Y6 Reaction-rate methods of analysis, those analytical methods based on the direct or indirect measurement of reaction rate. have been used for many years.1 A number of books and frequent review articles have appeared on the subject. Areas of application vary widely and the types of reactions commonly employed include complexation reactions, functional group specific reactions.enzyme reactions. chemiluminescent reac- tions and catalytic methods. Reaction-rate methods play an especially important role in clinical chemistry, where many techniques involve the use of enzymes. Advantages of reaction-rate methods include their speed and potential for kinetic selectivity. An important disadvan- tage is the inherently lower precision arising from the fact that the reactions do not go to completion as with equilibrium methods. Variations in the rate constant due to changes in experimental conditions can also degrade precision. Today. however, the routine availability of laboratory computers can substantially extend the capabilities of these methods through more sophisticated data processing. This article addresses some of these improvements.Minimising the Effect of Rate Constant Variations Many reaction-rate methods are based on first- or pseudo-first- order kinetics. a consequence of employing excess reagent concentrations. With traditional reaction-rate methods. such a s fixed-time. variable-time and derivatiire methods. precision is eroded by between-sample variations in the pseudo-first- order rate constant caused by changes in pH. temperature and other experimental variables. As even small changes in these variables can dramatically affect the rate constant.' this source of error is significant. Several "optimised" methods have been developed over the years that attempt to alle\hte the problem. The susceptibility of traditional and optimised approaches to the problem of between-sample rate constant variations has been reviewed elsewhere.2 I n this section.two approaches that we have used to address this problem are discussed. The Two-rate Method One of the ways we have developed to solve the problem of between-sample rate constant variations is the two-rate method. This is a relatively simple approach which requires that the rate be measured at two points on the reaction curve. These meawrements are then used to calculate the two-rate parameter (TRP) ;is given in equation ( 1 ) . RIA[ TRP( ti .f') = (R1/R2)'i A' . . . . (1) In( R IIR:) Here. R I and R, are the rates at times f I and f2. respecti\,elv. and At = f2 - 1,. The calculated value is an estimate of absorbance (or some other measured parameter) at I = x .and so should be largely independent of the rate constant. This simple approach has been found to be effective in reducing the effect of temperature variations in the molybdo- phosphate reaction for the determination of phosphate. and for pH effects in the determination of calcium by a complexation reaction.j Table 1 compares the results obtained for calcium b!. the two-rate method to those obtained with the initial rate method. Table 1. Effect of pH variations on the initial rate method (IRM) and the two-rate method (TRM) determination of calcium. Calibration ~ v a s performed at pH 6.0. Actual [Ca' ' ] = 1 .OO !IM. Pseudo-first-order rate constants \{'ere determined b!, non-linear regression [ Ca'- ] rnca~urcd. y X I Error. '7, pH k:s I IRM TRM IRM TRM 6.0 0.305 1.11x 1.044 I' 4.4 5.8 0.476 1.681 0.962 6s -3,s 6.2 0.191 O.hO2 0.98s -41 - 1.2 The precision of this method in the absence of rate constant variations was shown experimentally and theoretically t o he comparable to similar derivative methods. proliding measure- ment times are correctly chosen.Optimum measurement times have been reported.-' The Extended Kalman Filter While the two-rate method is a simple and effecti\fe means of addressing the problem of bet\veen-sample rate constant variations. its potential is limited by the fact that it is ;I two-point method. Better precision should be realised \\,ith use of a method which takes account of all of the data. Perhaps the best multi-point method is one that employs non-linear regression to fit an appropriate model to the data.Unfortu- nately, most of these methods are still cumbersome batch procedures which are not easily implemented in real-time applications. An id e a1 ii I t e r n a t ive to ba t c h - m ode n o n- I i n e a r regression would be a recursive algorithm for non-linear modelling. One way of obtaining this is through the extended Kalman filter. The Kalman filter is an algorithm for the recursive estimation of linear model parameters from noisy measurements and has become an increasingl>r popular tool in anall.ticril chemistry in recent years.' Most applications ha\.t: employed the filter ;IS ;I means of performing linear least squares fitting." Strictly speaking. the Kalman filter is no! intended for non-linearANALYTICAL PROCEEDINGS.APRIL IYXY. VOL. 26 129 applications. but an adaptation of the basic algorithm. the extended Kalman filter. can be used. While results with this approach are not guaranteed to be optimal in the least squares sense. it is often k'ery effective. In an attempt to compensate for the effect of betuwn- sample rate constant variations. ~ v e employed the extended Kalman filter with the simple first-order model where A, is the absorbance at any time f , A , the final equilibrium absorbance. k the pseudo-first-order rate constant and B a constant background absorbance. The parameters estimated with the filter were A , . k and B. By generating an estimate of the equilibrium absorbance in this manner. result5 should be largely independent of between-sample changes in the rate constant.Because the non-linear form of the Kalnian filter is sensitive to initial parameter estimates. reasonable starting \.dues had to be provided. The estimate of k was its nominal value. while A , and B were estimated from the initial data points. Results were generated with a single pass of the filter. Other workers have employed multiple passes.' but this defeats the real-time nature of the filter. Good results were obtained with the extended Kalman filter. as is shown in Fig. 1 for the determination of phosphate by the molybdophosphate reaction. Calibration graphs were gener- ated at three different temperatures for the study. The slopes of the calibration graphs obtained with the extended Kalman filter are much less sensitive to temperature variations than those obtained with the initial rate method.While this method should improve precision. the relative complexity of the extended Kalman filter will probably act as a barrier to its implementation. 0.5 EKF 0.4 I - T = 31.2"C 0.3 + 0.2 0.1 0 - I Initial rates 1 0.3 1 m n I 4 0 2.0 4.0 6.0 8.0 10.0 Concentration of P, p.p.m. Fig. 1. Comparison o f phosphate calibration cun'es at three diflcrcnt temperatures. ;is obtained t y thc cstcndcd Kalman filter and the initial rate method Differential Kinetic Methods One of the advantages of reaction-rate methods is their potential for kinetic selectivity. Not only can the rate of the reaction be used to minimise interferences. but differing reaction rates for parallel reactions also permits the simul- taneous determination of more than one analyte.Such multi-component analysis techniques are called differential kinetic methods. While these methods can be used to analyse related classes of analytes (e.g., phosphate and silicate). their potential has been restricted by the data analysis methods available. Traditional techniques. such a s graphical extrapola- tion or the solution of simultaneous equations. have imposed restrictions on the relative rates of the reactions involved or limited the precision and accuracy of the results. The ideal data processing approach to differential kinetic analysis would involve a reliable multi-point method which could be conveniently implemented in real-time. I t has long been recognised that linear least squares fitting exploits the data most effectively, but this solution has not been amenable to real-time applications.The Kalman filter, however. can be used to implement linear least squares recursively. While traditional approaches often require a rate constant ratio of 1 0 to determine two components reliably. studies with synthetic and experimental data have shown the Kalman filter to provide accurate results with rate constant ratios of less than three. In contrast to the extended Kalman filter, the linear Kalman filter is very stable, simpler to implement, faster and insensitive to initial parameter estimates. Such qualities make it a desirable data analysis tool. Experimental studies of this approach involved the determination of the amino acids glycine and asparagine by reaction with trinitrobenzenesul- phonic acid.s The model employed two first-order eyuations similar to equation 2.and the results for the analysis of two mixtures are given in Table 2. Although the errors may at first appear large, the data analysis method was pushed close to its limits in this application. The ratio of the rate constants was only 2.5 and the between sample standard deviation in the pseudo-first-order rate constants was about 6%. No better results were obtained with non-linear least squares. Table 2. Rcxults of differential kinetic analysis of amino acid mixtures Lvith the Kalinan filter A mi n o Concentration Concentration Mixture acid taken, y~ foundiuxi Error. 1 Glycine 11.3 17.8 - 10 Asparaginc 5.7 5.0 - 1' - Glycine 12.0 10.3 - 14 Asparagine 21.0 24.0 0 7 Additionally, data processing can easily be carried out on a personal computer in real time.Computation times typically run from 20 points s-1 to 800 points s-1, depending on the model used and the computation power employed. Conclusions It is clear from the results presented here that the use of new data analysis methods can substantially improve the quality of results available from reaction-rate methods of analysis. Two methods have been shown to be effective in minimising the problem of between-sample rate constant variations. and the Kalman filter has been shown to enhance the capabilities of d i ff e rent i a I k i net i c methods significant I y . These i m prove me n t s can be accomplished without loss of speed o r reliability. important practical considerations in the implementation of any new data processing method.The author gratefully acknowledges the contributions of Drs. S. R. Crouch. M. I. Karayannis and A. P. Wade. and the Editors of Tulutiru for making it possible to present this work in Britain through the Ronald Belcher Memorial Award. References 1 . Mottola. H. A . . -'Kinetic Aspects o f Anal!,tical C'hcmistr! ..' u'iley. New Yorli. I W X .130 ANALYTICAL PROCEEDINGS. APRIL 1989. VOL 26 2. 3 . 4. 5 . Carr. P. W.. Anal. Cheni., 1978. 50. 1602. Wentzell. P. D.. and Crouch. S. R.. Anal. Chem., 1986. 58. 2855. Wentzell. P. D.. and Crouch. S. R.. A i d . Chem., 1986. 58. 2x5 1 . Brown. S. D.. AnriI. C'him. Acfa, 1986, 181. 1 . 6. Wentzell. P. D.. Wade. A. P.. and Crouch. S. R.. And. Chem., 1988.60. 905. 7. Rutan. S. C . . and Brown. S . D.. Aiiril. Chirn. A m , 1985. 167. 23. 8. Wentzell, P. D., Karayannis. M. I.. Lopez-Nieves. M.. and Crouch, S. R.. And. Chirn. Actri, in the press. Oxygen Radicals: Their Measurement ln Vivo Joseph Lunec Department of Biochemistry, SeIly Oak Hospital, Raddlebarn Road, Birmingham B29 6JD It is now almost 50 years since Michaelis' first predicted the ubiquitous nature of one electron reduction reactions in enzymic processes which regulate human metabolism. Although the importance of such free radical reactions cannot be questioned, their role in the development of disease is controversial. Without doubt, one of the major reasons for this apparent impasse in the field of free radical pathology is the absence of adequate measurement of in vivo free radical activity.The following review attempts to focus on this problem by describing both the direct and indirect techniques employed to measure oxygen radical activity in vivo. The Source of Free Radical Activity In Vivo The biochemistry of radical reactions in human metabolism is inextricably linked to oxygen and the term oxygen radical is commonly used to describe intermediates of the four one- electron reduction steps converting oxygen to water. Superoxide (0:- ) is the first one electron reduction product of oxygen.? Hydrogen peroxide and the highly reactive hydroxyl radical (OH.) are the other two species which are commonly referred to, collectively, as reactive oxygen species (ROS). with hydrogen peroxide the non-radical species of the three.One of the most important agents of oxygen toxicity is the superoxide radical. At physiological pHs it is a fairly strong reducing agent and a weak oxidising agent. It dismutates spontaneously into hydrogen peroxide, and also by virtue of its reducing properties can dissociate protein-bound iron. parti- cularly from iron storage molecules such as ferritin.3.4 Once iron in its protein bound iron(II1) form is reduced to iron(I1) by superoxide, the Fez+ can then interreact with hydrogen peroxide via a Fenton reaction to produce the highly destructive hydroxyl radical (OH.). Hydroxyl radicals that are believed to be formed in vivo are thought to have a steady-state concentration of between l!-j and 10-9 M. This means that they can travel barely a few Angstroms in any direction before reacting with another biomolecule.Understandably, this accounts for why this radical is very difficult to detect under complex biological conditions, and particularly in vivo. So how do we measure such activity in vivo and decide with both confidence and accuracy that oxygen radical species are produced in certain disease processes? There are essentially two ways to do this: either by direct procedures, which are dependent on the physico-chemical properties of the radical species. or by indirect methods. which are dependent on the measurement of the products of radical reaction with certain biomolecules. Direct Methods There are two main procedures for measuring radical events directly in tiivo: both are controversial. The first is electron spin resonance spectroscopy (ESR).This method has developed into a powerful technique for measuring radical reactions. The technique is dependent on the paramagnetic properties of the unpaired electron. When a radical of interest is placed in a strong magnetic field. the unpaired electron aligns into one of two quantised energy states with respect to the orientation of the electronic magnetic moment to the field. parallel or antiparallel. The application of a resonant high frequency electromagnetic field (usually in the microwave range) excites spin flips between the two states. The absorption of the incident radiation causing such a change is detected electronic- ally, the pattern of the second derivative signal being a characteristic profile of the radical detected.5.h Even with such powerful instrumentation the hydroxyl radical, because of its high reactivity.is extemely difficult to detect. In an effort to extend the lifetime of free radicals such as the hydroxyl radical, one of two alternative procedures are usually carried out. Measurements in biological material are made either on lyophilised samples at low temperatures. or. alternatively, by "spin trapping" procedure~.~.S In principle. the spin trap is used to react with radicals to form more persistent radicals or spin adducts, which are easily detectable by ESR. The most commonly used spin traps are nitrones and nitroso compounds, which yield nitroxide spin adducts. By using this technique Hearse et ul. have identified hydroxyl radicals generated in rat hearts during the induction of cardiac arrhythmias.9 One other way in which specific radicals can be measured is by light emission or chemiluminescence.This technique can be applied to identification of a range of radical species by selective use of interference filters. Characteristic emissions can be measured."' For instance, singlet oxygen has two types of luminescence, one at 1.27 um and dimol luminescence at 631 and 704 nm. Excited carbonyls denoted as RO" emit between 380 and 460 nm. Luminol (S-amino-2.3-dihydrophthalazine- 1,4-dione) can be used to amplify chemiluminescent signals. Luminol is oxidised by several oxidant intermediates, e.g., superoxide, hydrogen peroxide, hydroxyl radical and singlet oxygen to an electronically excited aminophthalate anion that, when relaxed to the singlet ground state, emits photons.Emission is at around 450 nm, so that liquid scintillation counting is possible. The particular advantage of chemilu- minescent assays is that analysis of whole. intact organs is possible." This technique may well become one of the major methods for measuring free radical activity itz viiw. Indirect Procedures Lipid Peroxidation By virtue of their inherent reactivity. oxygen derived free radicals are reactive with all manner of biomolecules. This property can be put to our advantage in terms of assay development. The chemistry of the reaction of radicals with polyunsaturated lipids (PUFA), proteins and DNA is well documented (for reviews see references 12 and 13). PUFA are, by far, the most reactive of oxygen radical substrates.and if we wish to determine whether radicals are produced in viiw then identification of oxidation products of lipids would logically be our procedure of choice. However, with lipid peroxidation, because of the complexity of the reaction, the number of products is considerable. Crude measures, such as dime conjugate (DC) formation. which detects the rearrangement ofANALYTICAL PROCEEDINGS. APRIL I9X9. VOL 26 131 methylene interrupted double bonds to alternate single and double bonds. are poor measures of peroxidation itz i-iiw, where other ultraviolet absorbing. lipid soluble materials may interfere. Measurement of end products of peroxidation. often referred to as thiobarbituric acid reactive substances (TBARS). is by far the most popular measure.and many variations of this method have been described in the literature in an attempt to increase its specificity.14.15 TBARS are thought to reflect a whole range of peroxides and aldehydes. including malondialdehyde (MDA). generated as a result of ongoing peroxidation. Tappel and co-workerslo.li have. however. pointed out that if aldehydes, and particularly MDA. are produced in r-ilvo, they are unlikely to be detected there in their free form. MDA crosslinks primary amino groups of amino acids. DNA. proteins and phospholipids to form conjugated 1.3-iminopropene structures (Schiff bases). which are autofluorescent. This reaction has been made the basis of an in ~jivo assay of free radical activity but has not proved popular. probably because of interference (from other fluoro- phores) and the unavailability of standardising reference material.However. these somewhat crude. non-specific methods of measuring peroxidation are now being superseded by more specific procedures. These are generally of three types: measurement of alkanes by gas chromatography in the expired breath of animals and humans's; measurement of aldehyde and peroxide products by high-performance liquid chromato- graphy (HPLC)I'): measurement of peroxides by enzymic methods.") Although more specific than either TBA reactivity or d.c. methods, these procedures are far from perfect and suffer considerably from interference from extraneous sources. Protein Oxidation Monitoring PUFA oxidation is a popular way of measuring free radical activity. probably because our understanding of the chemistry of lipid peroxidation has been so well developed over the last 40 years.Very recently. however, the oxidation of proteins, which has in the past been of almost exclusive interest to radiation biologists, is coming to the fore a s a marker of free radical activity in Ltivo.2' Proteins oxidise in a similar manner t o PUFA; however. unlike PUFA, protein oxidation products can be identified and measured much more specifically. Obviously, the way in which they oxidise depends to a great extent on the way in which their constituent amino acids react with oxygen radicals. Aromatic amino acids are particularly prone to radical attack. Tyrosine undergoes dimerisation to dityrosine. tryptophan undergoes pyrrole-ring cleavage o r hydroxylation of the aromatic ring to yield several fluorescent derivatives, such as kynurenine, N-formylkynurenine and 5-hydroxytryptophan." Tyrosine dimers and the above named derivatives of tryptophan all possess a characteristic auto- fluorescence in the region of 420-480 nm when excited between 320 and 380 nm.This autofluorescence is of analytical importance because it can be used to detect oxidative alterations to proteins such as immunoglobulin G and albumin in human serum.'l.z' Other denaturative changes occurring to proteins have also been recorded by using this type of technique: for instance. the oxidation of cysteine to cysteic acid and methionine to methionine sulphoxide. Proline residues are also susceptible to damage and are converted to glutamic acid (for review see reference 23).Oxidised products of amino acids can be measured by reversed phase. high-performance liquid chromatography (HPLC). Colorimetric procedures are avail- able for the general measurement of carbonyls generated from the oxidation of amino acids within proteins. These are usually non-specific and suffer from similar pitfalls to those found for the measurement of oxidised lipid.?' DNA Oxidation DNA is highly susceptible t o attack by oxygen radicals. Thymine and guanine are the bases which appear to be most susceptible to oxidation. Thymine glycol or 5-(hydroxy- methyl)-uracil are formed from thymine. although guanine is most readily oxidised by gamma radiation or photo-oxidation. Monoclonal antibody technology has been applied to the measurement of thymine glycol production.A major product of guanine oxidation which can be identified (by HPLC') ensuing from direct oxygen radical attack on DNA is 8-hydroxy-deoxyguanosine (8 OH-dG) .25 It is most conce- niently detected in the urine of animals and human subjects.'" This represents perhaps the most optimistic note in the field o f free radical biochemistry applied to pathology a s it provides us with a very specific measure of free radical activity irz \,ii,o. It is reasonable to predict that in the next 5-10 years these new methods of measuring free radical activity will undoub- tedly be applied. more and more. to the study of disease processes. Only at the end of this period will we be able to identify whether oxygen radicals cause.or promote. disease, o r whether their production in r>iiw is just another interesting epiphenomenon. References 1. 7 -. 3 . 4. 5 . 6 . 7 . x. 9. 0. 1 . 7 -. 13. 14. IS. 16. 17. 18. 10. 20. 21. 37 --. 23. 24. 25. 26. Michaelis, L.. Cold Spring Harhoiir SFtnp. Qriurir. Biol., 1039. 7 . 33. Habcr. F.. and Willstattcr. R.. Brr. Derrr.\(h C ' h e t i i . , 1939. 64. 2844. Bicrnond. P.. Van Eyk. H. G . . S\vaak. A. J . G . . and Kostcr. J. F.. J . C h . Iiz\.esr.. 1984. 73. 1576. Gutteridge, J. M. C.. Ro\vley. D. A , . and Halliu,cII. €3.. Biodzmz. J . . 19x1. 199. 263. Borg. D. C.. iti Swartz. H. M . . Boston. J . R.. and Borg. D. C.. Ed; r o rs , *. B i ol og i c a I A ppl i c;i t i o ns of E 1 e c t ron S pi n R e so- nance." Wilcy Interscience.New York. 1072. p. 265. Ingrarn. D. J . E.. "Free Radicals a s Studied by Electron Spin Resonance." Academic Press. New York. 1958. Janzcn. E. G.. Free Rrid. Biol., 1080. 4. 155. Borg. D. C.. Free Rad. Biol.. 1976. 1. 49. Hearse. D. J.. in Rice Evans. C.. Editor, "Free Radical\. Oxidant Stress and Drug Action." Richelieu Press. London. 1087. p. 13. Cadenas. E., and Sies. H . . i r i Packer. L.. Editor, '.Oxygen Radicals in Biological Systems Methods in Enzymology." 1984. 105. '21. Boveris. A , . Cadenas. E.. Reiter. R.. Filipkoivski. M.. Nakase. Y.. and Chance. B.. Proc. ,C'cirl. Acud. S c i . , 1980. 77. 347. Lunec. J.. Anti. Cliti. Riodzetiz., 19x0. in thc press. Sies. H., A i i g h - d i e C'herizie. 19x6. 25. IOCX. Gutteridge. J . M. C.. Free Rtrd. Rc.\.< ~ o t ? i n i . , 1986. 1. 173. Guttcridge. J . M. C.. and Quinlan. G . J . . J . AppI. RiocAcw.. 19x3. 5 . 293. Tappel, A . L.. ;ti Trump. B. F.. and Antilla. A , . .&litor\. "Pathological Aspects of Cell Membrane\." Academic Pre\s. New York. 1975. p. 145. Fletcher. B. L.. Dillard. L. J . . ; i d Toppcl. A. L.. A t i ( i 1 . Bioc/zc>ni., 1973. 52. 1 . Rcily. C. A , . Cohen. G.. and Liehermann. M.. .I'cietzcc. 1974. 183. 208. Slater. T. F.. itz Packer. L.. Etliror, "Oxygen Radical\ in Biological Systems." Academic Prcs\. NCM, York. 1984. pp. 105. 2x3. Heath. R. L.. and Tappel. A . L.. Arzul. Rioc/ir>tiz.. 1976. 76. 184. Jones. A. F.. and Luncc. J . . Rrir. J . ( ' ( i t i c . , 1987. 55. S ~ p p l . VIII. 60. Griffiths. H. R.. Unsworth. J . . Blake.D. R.. and Lunec. J . . it1 Rice Evans. C.. and Dormandy. T. L . . Editors. "Frcc Radicals. Chemical Pathology and Medicine." Richelicu P r w . London. 1988. p. 439. Wolff. S . P.. Garner. A , . and Dean. R . . Tretztl\ Biol. S c i . , 1986. 11. 27. Stadtman. E. R.. Twtids Riol. Sci.. 1986. 11. 1 1 . Floyd. R. A , . Watson. J . J . . Wong. P. K.. Altmillcr. D. 11.. and Rickard. R. C.. Frw Rtitl. Re\. <hmni., 1986. 1. 163. Cundy. K . C.. Kohen. R.. and Ames. B. N . . ill Simic. 31. (3.. Erliror. "4th International Congre\\ on Oxygen Radicals." 1988, in the press.132 ANALYTICAL PROCEEDINGS. APRIL 1989. VOL 26 Carbohydrate and Protein Analysis of Plant Materials John F. Kennedy and Miss 2. S. Rivera Research Laboratory for the Chemistry of Bioactive Carbohydrates and Proteins, Department of Chemistry, University of Birmingham, Birmingham B 75 2TT C.A. White Chembiotech Limited, Institute of Research and Development, University of Birmingham Research Park, Vincent Drive, Edgbaston, Birmingham B 75 2SQ Carbohydrates and proteins are the two most widely occurring macromolecules in the plant kingdom. They may be present on their own. or as compounds involving proteins, carbohydrates, lipids, etc. (i.4.. glycoproteins. glycolipids) or with incorpora- tion of groups such as phosphates and sulphates. In such combinations they become essential to many biological reac- tions. Recent interest in biotechnology and renewable sources of raw materials has boosted interest in the analysis of these two important biomolecules. A great number of chemical and physico-chemical techniques have been developed and improved.However, present discussion will place emphasis on the chemical methods. Carbohydrates Isolation and Purification The identification and structural analysis of carbohydrates necessitates an initial isolation of the material in a pure form with no degradation or loss of structural features. Thus, the use of acids, alkalis or enzymes is eliminated. After solubilisation in an appropriate solvent the carbohydrate can be isolated by ul tracen trifugation, membrane ul trafil tration , electrophoresis. gel filtration. chromatography. etc. Identification and Quantitation of the Monosaccharide Residues These can be achieved by total or partial acid hydrolysis but this should be performed without degradation of the monosac- charide units.Direct hydrolysis utilising mineral acids fre- quently results in degradation. Thus. alternative methods using trifluoroacetic acid, methanolysis or more specific methods using enzymes have been employed. These hydrolysis procedures liberate a mixture of monosac- charides which are separated, identified and quantified by chemical methods (see Table l ) , various chromatographic techniques, electrophoresis and mass spectrometry. Determination of Configurations The proper D- or L- configurations of the pure monosaccharides are measured by their specific rotation. circular dichroism Table I . Chemical methods for the anal~sis o f the main classes of car bo h 4; drat e s Class Hexose Reducing sugar Pentose Ketostt Hexohami ne Uronic acid Sialic acid Assay L.- C y s t e i n c s u I p h u r i c iic i d Phenol - sulphuric acid Neocuproine Dinitrosalicylic acid Iron(II1) - orcinol Phenol - boric acid - sulphuric acid Elson - Morgan assay Ninhydrin Orcinol - sulphuric acid Carbazole Warren assay absorption or enzymic susceptibility. Values obtained are compared with known monosaccharides or with literature values.The anomeric configuration of a glycosidic linkage is best determined by enzymatic hydrolysis o r chromium( VI) oxide oxidation. I n the latter an initial acetylation of the carbohy- drate is performed. After treatment with chromium( VI) oxide in acetic acid, acetylated aldopyranosides with equatorially attached aglycons are oxidised to 5-aldulosonates. whilst those with axially attached aglycons show very minimal reaction.Sequencing and Determination of Linkage Points These are commonly performed by methylation processes either by the Purdie (methyl iodide in silver oxide or carbonate) or by the Haworth (dimethyl sulphate in aqueous alkali) procedures. Methylation on its own will not give structural sequence data but it will identify the monosaccharide components and determine their linkage points and their ring structure. Other methods utilised are periodate oxidation. Smith degradation, acetolysis, enzymic hydrolysis and alkaline degra- dation. Unlike methods such as enzyme hydrolysis. alkaline degradation degrades from the non-reducing end and is therefore more definitive in the analysis of branched structure owing t o there being only one reducing end to the molecule.Characterisation of Polymeric Carbohydrates 0 1 i gosacc h a r i de s an d po I y s a cc h a r i de s a re c h a r ac t e r i \e d b > their monosaccharide repeating units and their relative mole- cular mass distribution. The number of repeating unit5 pre\ent is determined from the relative molecular mass distribution of the polymeric carbohydrate. which is obtained b> gel-permea- tion chromatography. Proteins Proteins, of any origin. are classified according to their function, which in turn is determined by their structure. The sequential arrangement of the constituent amino acids and the covalent cross-linkages between residues in the polypeptide chain form the protein's primary structure. Knowledge of the primary structure is of fundamental importance and the strategy for a complete sequence determination is presented.Purification and Preliminary Characterisation For sequence analysis of proteins. the retention of secondary and tertiary structures is not required, so purification in denaturing media such as 8 M urea or sodium dodecylsulphate is possible. However, conditions deleterious to the co\.alent structure should be avoided. The preliminary characterisation of proteins involves the determination of relative molecular mass, usually by gel permeation chromatography. the complete analysis of amino acids. the determination of molar absorptivity by the ultra- violet absorbance at 280 nm and the identification of the am i no- t e r m i n al and car box y - t e r m i n a I residues .An accurate amino acid analysis serves as the basis against which the information derived from the sequence determina-I!NALI'?'ICAI_ PROCEEDINGS. APRIL I9S9. VOL 26 I33 tion is compared. Various chemical methods. usually emplo!r- ing derivatising reagents such as ninhydrin. fluorescaniine. p h e n y I i so t h i oc y an ate . or t hop h t h a 1 a I de h y de an d others . h a\.e been d e ~ ~ l o p e d for amino acid analysis. some of which can be used in con j u n c t ion w i t h c h ro m ii t o g r a p h y . A preliminary chemical modification of the protein f o r sequence analysis should be performed. particularly the conversion of cysteine residues into stable derivathres to prei'ent the formation of disulphide linkages during peptide isolation.The determination of amino-terminal residues is performed by reactions with reagents such as dansyl chloride, phenyliso- t h ioc y a n a t e . 4-d i me t h y 1 am i n oazo be nze n e -4 ' - i sot h i oc y a n ;it e and some amino peptidases. among others. chemical methods employed to identify the carboxy-terminal residues include car b o x y pe p t i d a s e digest ion . h y d r az i no 1 y s i s . t r i t i ii t i o n ;I 11 d h y da n t oi n form a t io n . Specific Cleavage of the Protein and Determination of the Peptide Sequence For typical protein chains (200-500 amino acid residues), clea\.age at specific points and purification of the resulting peptides are required. The amino acid composition will sen'e a s a guide as to which chemical methods can be used.Peptide mapping is usually performed by the Edman degradation using phenylisothiocyanate. The process involves the reaction between the amino-terminal residue and phenyl- iso t hi oc y a n a t e to form it p he n y l t h io h y d ii n t oi n de r i va t i \,e . w h i c h can be id e n t i fied c h ro m a t ogr a p h ical 1 y . Deduction of the Total Primary Structure The final step is to deduce the total primary \tructure o f the protein from the different peptide sequences. From (hi\. the position of the disulphide cross-linkages and the over-all three di me nsi on a I structure cii 11 be es t a b 1 i shed . Post-translational hlodification of Carbohydrates and Proteins in Plants C h e mica 1 mod i f i cii t i o n s of car b o h y d r a t e s and pro t e i n s occ u r ir 1 \-i\w and such modifications significantly affect their biological functions.Two main classes of these glycoconjugates are the g I y co p r o t e i n s and g I y co 1 i pi ds . Glycoproteins At present. characterisation of plant glycoproteins has on11 in\x)l\,ed the glycoprotein lectins as distinct from protein lectins to elucidate the structure of the carbohydrate moieties. Their isolation makes use of lectins Lvhich bear specific sugar-binding sites. Glycans are conjugated to glycopeptide chains through N-glycosyl o r 0-glycosyl primary covalent linkages. Their c h e mica 1 cl e ii \,:I ge can be pe r fo r m e d by red u c t i 1.e 13 - e 1 i mi n a t i o n reactions. alkaline cleavage or hydrazinolysis. or a combina- tion of these methods.The composition of the cleaved glycan in terms of the monosaccharide residues is determined by the chemical methods discussed earlier. Glycolipids Glycolipids are compounds wherein the lipid is combined with ca r bo h y d r a t e s . us u a I I y bran c h e d o 1 i go sii cc h ;i r i d e s an d n on - carbohydrate groups such as acetyl and sulphate. Glycolipids are commonly extracted using chloroform - methanol mixtures. Their separation and purification are usually performed by phase separation or chromatographic techniques. The composition of glycolipids in terms of car- bohydrates. fatty acids. sphingosine bases and glycerol is then de t e rniined . The limitations of these chemical methods should be continually borne in mind. A combination of these is necessary for a complete structural determination to understand fully the activity and function of these macromolecules.Technological Aspects, Current Uses and Future Trends The use and importance of carbohydrates and protein\ derived from plants in various technologic\ and industries is unque\- tionably increasing. Continuous research in biotechnolog!. and Table 2. Technological aspects. current uses and futurc trends Current use4 Fu t u re t re n d 4 Carbohydrates Food and bren ing Oil industry Pharmaceutical and cosmetic4 Chemicals from Construction and packaring biomass Tcx t ilt: Chromatographic supports Organic acid production Modification of carbohydrate4 t o irnpr0i.c. alter pro pe r t i e 4 bled i ci n e Fe r me n t a t io n su h4 t r;i t c Proteins Food.hreiving and dair). Genetic engineering Medicine Plant ccll Chemical and pharmaceuticill biotechnolosy Cosmetics Bi oca t al p i s I m m u no logy Enzyme i mmo bil isat ion Enzyme biolucl and bioclect rochernical cell the on-going search for source\ of raw materials ha\e. no doubt, enhanced the application o f these materials. Example5 of their incaluable use are summarised in Table 2 and inve\tigations are carried out to explore fully the potential\ of plant materials in terms of their \pecific carbohydrate and protein contents. Progress in the Water Industry-Automation in a Water Company Laboratory Paul Hemmings South Staffordshire Waterworks Company, Green Lane, Walsall, West Midlands WS2 7PD I n recent years. the grwvth in regulatory standards for potablc water supplies has led to a rapid expansion in both sample numbers and particularly in the range o f anal>'tical methodolo- gies required by the routine D.ater quality control laborator!..Thih growth in analytical requirements has been requireci without increases in staffing levels. and has only been possible by a concerted drive towards automation where methods and sample numbers permit. Accordingly. the trend mithin the industry is towards feu.er. larger laboratories (e.g., the Regional Centres being set up by many Lvater Authorities) o r increasing collahorati\fe ventures between laboratories.134 ANALYTICAL PROCEEDINGS, APRIL 1989. VOL 26 Within the laboratory. the trend is towards larger, stand- alone, fully automatic instrumentation requiring minimal operator involvement, often operating around the clock.Add i ti on a 11 y . Labor at o r y I n fo r m a t i o n M an age me n t System s (LIMS) are increasingly used to enable rapid access to and manipulation of analytical information for a range of uses. Automation of Colorimetric Methods Options for automation of the many colorimetric or turbidi- metric methods used in water analysis include both continuous flow and discrete analysis. Continuous flow analysis is well established and includes both convention a I1 y air -se g m e n t e d '' Auto Analysis " and the more recent non-segmented "Flow Injection Analysis" types. Both have found wide usage and may be considered to be complementary. Discrete analysis has found steadily increasing application within water laboratories as the available equip- ment has become more versatile and sophisticated.Instru- ments based upon this principle are now replacing continuous flow equipment in many laboratories. This trend towards discrete analysis is not due to any inherent advantage of the technique over continuous flow: indeed in many ways discrete analysers are limited by their inability to perform separation methods. etc. It is the random access nature of the available equipment that makes its use preferable to that of continuous flow. the majority of which is batch in nature. In this way, only those tests which are actually required are carried out, with consequent savings in time, sample and reagent consumption. Additionally, further sam- ples can be added whilst the instrument is in operation which, in t u r n .further improves the efficiency and flexibility of the I a b o r a t o r y . The Kone Progress Analyser This is a computer controlled random access discrete analyser which has been in routine use within the Company's laboratory for two years. typically handling 20-60 samples per day for up to nine determinands. Samples. standards and reagents are stored in cooled trays within the instrumentation and are transferred to the disposable reaction cuvettes by a robotic transfer arm using precision syringes. Up to four reagent additions per test may be programmed. with a minimum final volume of 100 yl being required for measurement. Unlike with early instruments of this type, the ratio of sample to reagent volume is not limited and hence limits of detection are similar to those possible with manual methods.Between every dispensing operation the arm is rinsed and dried to minimise any carryover and hence prevent cross- contaminations. The order of analysis is optimised every minute by the instrument processor with recalibration on a time basis: hence. the instrument may be carrying out several methods simultaneously. The on-board photometer is of a single-channel dual-beam design, using optical fibres in con- junction with narrow band-width interference filters through which the 7mm path-length cuvette (containing 12 tests) is stepped in 2.7 s. In a typical analysis the cuvette transfer arm takes a cuvette from the magazine, checks it for optical cleanliness and places it in an available slot in the incubator.Once in position. the robot arm dispenses appropriate volumes of sample and reagents, mixing where required. Finally. the cuvette arm is used to step the cuvette through the photometer for measure- ment and to discard the cuvette into the waste compartment. Out of range samples are automatically diluted and re-analysed by the instrument. The instrument computer is used for programming test requests (via keyboard, bar-code reader or directly from the LIMS using an appropriate interface), validation of results and production of final reports of both test and quality control data. Currently, nine tests are carried out on the instrument (based on DOE standard methods) at rates of 80-100 tests h-1. Method performance is summarised in Table 1 .Table 1. Current method performance o n PROGRESS analyser Determinand/ Expectcd Mean Standard mgl concentration reported dciiation Alkalinity 0.0 1 .o 1 .X8 100.0 101 .o 1.78 Aluminium 0.00 0.01 0.01 1 0.20 0.19 0.01 1 Chloride 0.0 0.0 0.81 50.0 50.0 0.98 Arnmonia- 0.00 0.01 0.OOY nitrogen 0. SO 0.49 0.013 Nitrite-nitrogen 0 .oo 0.00 0.004 Total organic 0.00 0. 1 0.096 nitrogen 10.0 9.9 0.184 Phosphate 0.00 0.04 0.033 Sulphate 0.0 1 .o 0.35, Silica 0.0 0 . 2 O.OY9 5.0 5.0 0. 100 0.20 0.20 0.007 1 .oo 0.97 0.072 45.0 44.0 1.06 Discussion The performance shown in Table 1 demonstrates the PRO- GRESS analyser to be highly suitable for water analysis in a medium-sized laboratory. The extreme flexibility of the instrument leads to performance approaching the best of manual methods with no loss in sensitivity.Operator involve- ment is minimal and reliability has been excellent to date with less than 1% downtime recorded. Cross-contamination effects and carryover may still lead to problems, particularly where extremely low concentrations of determinand are present. Careful fine tuning of methods is required to reduce or eliminate these effects. Additionally. calibration requirements have been proved to be far more rigorous than those suggested by the manufacturer to eliminate errors caused by small drifts in instrument response. Organolead Compounds in the Atmosphere P. J. Metcalfe Department of Environmental Science, University of Lancaster, Bailrigg, Lancaster LA 1 4YL There is a wide range of organolead compounds which can be the type (R3Pb): are also known, but these are derivatives of best summarised as being either divalent ( R2Pb) o r tetravalent RIPb with a lead to lead double bond.The tetravalent (R4Pb). where R is an organic group. Ditneric compounds of compounds are slowly oxidised in air. and ;ire liable toANALYTICAL PROCEEDINGS. APRIL 1989. VOL 26 1.33 photochemical decomposition \*ice a free radical mechanism. The divalent compounds are more stable. both thermodynam- ically and hydrolytically. and readily decompose ~ . i a dispropor- tionation to RjPb + Pb. The synthesis of organolead compounds is easily accomp- ished by reaction of a divalent inorganic salt (usually a halide) with either organolithium or a Grignard reagent. EtTO 2 PbX2 + 4 R-MgX 2 RjPb + Pb + MgXZ Compounds of Environmental Interest Despite the huge diversity of compounds.the environmental chemistry of organolead is dominated by a small number o f tetraalkyl lead compounds. their salts and decomposition products. The reason for this is seen in the two possible sources of environmental organolead. Atirlzropogetzic. This is solely caused by the manufacture and use of tetraalkyl lead compounds as gasoline additives. i.0.. Eni~iront7ietirnl alkylnrion. If environmental a1 kylation occurs, it will almost certainly be methylation. Thus. the compounds of environmental interest are the fi\.e tetraalkyl compounds. M4Pb, M,EtPb. M2Et2Pb. MEt,Pb and EtjPb. and the corresponding halide salts. R3Pb+ and R2Pb‘+. giving a total of 13 compounds. The tetraalkyl compounds are dense.moderately volatile liquids. sensitive to heat and light. The salts are highly crystalline ionic compounds with high melting-points. which are soluble in water. and relatively stable in solution. The tetraalkyl compounds are manufactured from a mixture of molten lead and sodium (ratio 9 : 1). which after solidifica- tion is flaked and reacted with alkyl chloride at 75 “C and 400 kPa using an acetone catalyst. The products are collected and purified via steam distillation. MjPb, EtjPb. Ant hropogenic Sources The anthropogenic emissions to the atmosphere are Lia: man u fac t u re and transport 1 o sse s ; evaporation d u r i n g trans fe r : evaporation from vehicles; and vehicle exhaust pipes. Of these the most important pathway is the emission from vehicle exhausts.Within our research group we have recently studied this process. Our findings show that with increasing engine efficiency. there is an increase in the total of lead emitted. This is mostly inorganic lead. but if we consider only total alkyl lead we find that the amount emitted as aerosol remains constant, and for vapour phase alkyl lead the amount emitted decreases with increasing engine efficiency. This is explained by the fact that with more efficient engine perfor- mance, less fuel is emitted unburnt. In addition, we have investigated the speciation of the vapour phase alkyl lead emitted. We have found that with increasing engine efficiency we have a shift from tetraalkyl lead to ionic alkyl lead compounds being predominant. i. e . , R4Pb compounds are more effectively serving their purpose (as free radical scavan- gers) and are being broken down to the ionic alkyl derivatitzes.Atmospheric Chemistry On leaving the exhaust pipe. m., these organolead compounds enter into the environmental cycle. Their atmospheric chem- istry is best summarised by the scheme Decomposition half-life (f!), and although shown to exist in laboratory studies is not detectable in environmental samples. If environmental alkylation does occur, it is not thought to involve methylation of inorganic lead. but the re-alkylation of the ionic interme- diates. Although a minor role is thought to be played by het- erogeneous reactions on the surface of atmospheric particu- lates, the major decomposition pathways are due to homogeneous gas phase reactions, involving ozone.triplet atomic oxygen, photolysis and hydroxyl radicals (OH. ), of which the last two are considered most important. In a photochemically active atmosphere the f t values f o r MJPb and Et,Pb are 0.6-2 h and 5-10 h , respectively. A proposed scheme for the decomposition via (OH-) is given below: (CH+Pb + CH3‘ I The kinetics of these reactions are second order. and assuming a mean annual ambient (OH.) concentration of 1 x 106 cm- 3 . we can calculate the 1; of MejPb as 41 h , of Et,Pb 8 h . of Me3Pb+ 126 h and of Et,Pb+ 34 h . An interesting point is that f i for an ionic species is longer than that for the corresponding tetraalkyl compounds. Taking into account these half-lives. it can be seen that these compounds may be transported considerable distances from their anthropogenic sources.and thus may play an important role in the biogeochemical cycling of lead in the environment. Hence the need to in\,estigate the levels of these species in not only urban and rural areas, but also in remote areas (e.g., marine air). Sampling Methods The sampling methods used for this include adsorption on to porous polymer (R,Pb). adsorption into water (R3Pb+/ R2PW+) and cryogenic trapping (R,Pb + R3Pb+/R2Pb’+). In addition u’e have also been investigating the adsorption of vapour phase ionic compounds on to ion-exchange resin. However. we have concentrated on the use of cryogenic trapping using liquid nitrogen as a coolant (-130 “C) The advantage of this sampling technique is the simulta KOUS collection of both tetraalkyl and ionic species, and wbse- quently simultaneous analysis.Following the collection of a sample. the extraction procedure given below is carried out. (i). Add 5% sodium chloride solution. hexane and sodium diethyldithiocarbamate (NaDDC). 0.5 M: (ii). shake for 30 min and separate the hexane layer; (iii). add Grignard reagent (Pr-MgCl/Et,O) under a nitrogen atmosphere and shake the solution gently for 10 min; ( ; I , ) . add 0.5 M sulphuric acid and then shake (to destroy excess Pr-MgCI): and (i!), the solution is concentrated by evaporation. The principles involLred are that RjPb is extracted directly into the hexane fraction. and R3Pb+iR2Pb’+ form a complex with NaDDC/NaCI which is hexane soluble. after which they are propylated i-irr R,Pb+ + Pr-MgCI - R3Pb-Pr + Mg:+ + C1- I hexane dil.14iSOj The tetraalkyl lead decomposes \ria stages to inorganic lead. The intermediate (RPb.;+) is very unstable with ;I very short136 ANALYTICAL PROCEEDINGS. APRIL IY89. VOL 26 The propylation of the ionic compounds to fully alkylated species produces volatile compounds that are now suitable for separation by gas chromatography. We have also used butyla- tion, but propylation gives shorter retention times and hence easier analysis. Some people have also used an in sitii ethylation technique. Analytical Technique The technique used for the speciation and quantification of alkyl lead compounds makes use of a gas chromatograph (GC) connected via a PTFE transfer line to an atomic absorption spectrometer (AA).In place of the usual atomisation devices the AA has been fitted with a custom built furnace mounted on the burner head. This consists of a ceramic tube around which is wound Ni - Cr wire. By passing 120-130V through the wire the furnace can be heated to -1000 "C. By using the appropriate wavelength (A = 283.3 nm) this modified AA provides an element specific detector for the output from the GC, which has been fitted with a 1 m glass column packed with 3% OV-101 on Gaschrom-Q. The carrier gas used is helium, which is mixed with hydrogen prior to entering the furnace. These two gas flows and the oven temperature program have been optimised to produce good chromatographic separation, and optimum peak heights. The detection limits possible using this method are 6.G18.0 x 10-3 ng for RjPb and 19.C34.0 x 10k-7 ng for R3Pb+/R2Pb'+.Environmental Sampling Our objective was to investigate the alkyl lead content of remote o r marine air. As the levels were considered to be around 1 pg m-3. we needed to be able to sample >25 m3 of air. One problem associated with cryogenic trapping is that water ROYAL SOCIETY OF C HE MI ST Rlf lnformatm Services vapour will be also condensed out. forming ice which will eventually block the trap. Therefore, we needed a trap of sufficiently large size to allow sampling of the desired air volume. This was developed using a 6-1 PTFE screw cap bottle and stainless steel Swagelok fittings. This device was used for sampling marine air on field trips to the Isle of Harris (Outer Hebrides) and Bantry Bay (Co.Cork. S.W. Ireland). The effective detection limits that we were able to achieve were in the range 0.02 to 0.06 ng m-3 for R4Pb and 0.06 to 0.11 ng m-3 for R3Pb+ and R2Pb'+. I n the samples fron.1 the Isle of Harris we found detectable levels o f M4Pb and M2Pb2+ in the range of up to 2.4 ng m-3 for M4Pb and 1.7 ng m-3 M2Pb2+. As yet we are unable to comment on the origin of these compounds, as we have not at present calculated the air mass back trajectories. This also applies to the Irish samples. the results of which were not available when this paper was presented. Bibliography Allen. E. G., Radojevic. M.. and Harrison. R. M.. €riivirori. Sci. Tecknol.. 1988. 22. 517. Hewitt, C . N.. Harrison. R. M.. and Radojevic. M.. Arid. Uiini. Acta., 1986, 188. 229. Hewitt, C. N.. and Rashed, M. B . , Appl. OrpiriotnPt. Cheni., 1988. 2. 95. Hewitt, C. N . . and Harrison, R. M.. in Craig. P. J.. Editor, "Organometallic Compounds in the Environment . * * Longman. London. 1986. p. 160. Radojevic. M.. and Harrison. R. M.. Sci. Total €uiiirou.. 1YX7. 59. 157. Shapiro, H.. and Frey. F. W.. "The Organic Compounds o f Lead." Wiley, New York. 1968. AN INTRODUCTION TO APPLICATIONS OF LIGHT MICROSCOPY IN ANALYSIS By D. Simpson and W. G. Simpson, Analysis for Industry, Thorpe-le-Soken This new book reviews recent experience of the application of the light microscope in its various forms to a range of analytical applications. Light microscopy is one of the oldest basic techniques at the disposal of the analyst and is greatly undervalued and under used in the analytical laboratory. It remains a convenient, economical technique which should not be overlooked and can be of great value in the analysis of foods, pharmaceuticals, metals, plastics, water, agrochemicals, waste management, bacteriology and much more. The authors aim to encourage wide use of microscopy in actual practice and to remind analysts of its qualities and applications. Microscopists, analysts and students alike will gain much from the authors' enthusiasm and this book should assist in extending the utility of the instrument in the future. Brief Contents: Petrology and Mineralogy; Metals and Alloys; Plastics and Polymers; Surface Properties and Faults in Materials; Fibres, Paper and Textiles; Clinical and Biological Materials; Pharmaceuticals; Bacteriology and Microbiology; Moulds, Yeasts, Brewing and Distilling; Water Quality and Water Supplies; Foods and Spices; Health and Safety; Microscopy and Forensic Science. The book includes a bibliography, a listing of microscopy journals and an index. ISBN 0 85186 987 4 Hardcover 225pp Published 1988 Price f29.50 ($63.00) For further information, please write to: Royal Society of Chemistry, Sales and Promotion department, Thomas Graham House, Science Park, Milton Road, Cambridge CB4 4WF. U.K. To Order, please write to: Royal Society of Chemistry, Distribution Centre, Blackhorse Road, Letchworth, Herts SG6 1HN. U.K. or telephone (0462) 672555 quoting your credit card details. We can now accept AccesslVisal MasterCard/Eurocard. RSC Members are entitled to a discount on most RSC publications and should write to: The Membership Manager, Royal Society of Chemistry, Thomas Graham House, Science Park, Milton Road, Cambridge CB4 4WF. U.K.

ISSN:0144-557X    

DOI:10.1039/AP9892600128

出版商:RSC    

年代:1989

数据来源: RSC

摘要:

ANALYTICAL PROCEEDINGS. APRIL 1989. VOL 26 137 Equipment News Ultrasonic Nebuliser The ARL ultrasonic nebuliser (USN) is an alternative sample introduction acces- sory for both ICP and DCP instruments. It is applicable to samples which occur naturally as solutions or can be put into solution. Its primary advantage over con- ventional sample introduction systems is the improved detection limits which result from enhanced sample transport efficiency. Fisons Instruments, Applied Research Laboratories, Sussex Manor Park, Gatwick Road, Crawley, West Sussex RHlO 2QQ. Spectrophotometer The DU-68, a new addition to the DU-60 Series spectrophotometers, combines optimised wavelength scanning with step- programmable capabilities. It offers simultaneous data acquisition and real- time viewing facilities.For quantitative analysis the DU-68 displays calibration curves for reviewing and editing, then produces final results calculations which can be printed out or stored. In qualita- tive analysis it simplifies the development of absorption spectra by monitoring the spectra while in progress. Kinetic analysis of six different samples can be performed simultaneously. For gel and film scanning the user can pick peaks or set base lines on the CRT screen or control other parameters. Beckman, Progress Road, Sands Indus- trial Estate, High Wycombe, Bucking- hamshire. partial pressures is always equal to that of the total pressure measurement. This improves accuracy and eliminates non- linearity errors at high pressures and loss of sensitivity caused by contamination. Spectramass Ltd., Radnor Park Indus- trial Estate, Congleton, Cheshire CW12 4XR.De-gas System for Mass Spectrometers A high-performance de-gas system, de- signed to accept NBS and Cathodeon, or all-metal type filament beads, ensures efficient, contaminant-free filament con- ditioning with the minimum of operator involvement. Up to 16 beads of either single or triple filament configuration may be inserted for sequential de-gassing in sets of 4. Subsequently these may be stored, ready for sample loading when desired. Contamination of the sample turret is avoided, as it is not involved in the de-gassing procedure. VG Isotopes Ltd., Ion Path, Road Three, Winsford, Cheshire CW7 3BX. Vapour System for Atomic Absorption Spectrometers Designed specifically for use with the makers’ atomic absorption spectromet- Spectrophotometer By coupling a spectrophotometer to an IBM compatible PC and a high-resolution colour monitor a powerful tool has been created for analysing and comparing col- ours.The system’s software makes it specifically useful for solving manufactur- ing problems in the ink and paint indus- tries as well as in other fields, such as plastics and textiles. There is a basic colorimetry module with an integrated sorting facility; this allows the measure- ment, comparison and sorting of colour samples in a range 40&710 nm. There is a module for characterising the pigment or colour base; it calculates K-absorption and S-diffusion every 20 nm according to the degree of concentration. Also featured is the ability to derive formulae for colour shades by conbining pigments in different concentrations, either manu- ally or automatically.MTS Colorimetrie, Immeuble Jules Cesar, 12 chaussee Jules Cesar, F-95520 Osny, France. Electrochemical Detector The M400 electrochemical detector offers the liquid chromatographer a novel analy- tical technique. Compounds such as car- bohydrates, amino acids and non-aro- matic alcohols can be satisfactorily detec- Mass Spectrometer The PC 2000 Series of quadrupole gas analysers features a new ion source which has a built-in independent total pressure collector. Rapid switching between par- tial and total pressure measurement allows software normalisation of the spec- trum by ensuring that the sum of the Philips Scientific PU9360 vapour system ers, the PU9360 vapour system offers the ted by using a pulsed potential waveform.benefit of continuous, rather than tran- The electrode is sequentially subjected to sient, signals during the trace determina- three distinct potentials which, respec- tion of hydride-forming elements and tively, prime the electrode, perform the mercury. oxidation and clean the electrode. A Philips Scientific, York Street, Cam- current is measured only during the inter- bridge CB1 2PX. mediate oxidation stage.138 ANALYTICAL PROCEEDINGS, APRIL 1989, VOL 24 Jones Chromatography Ltd., New Road, Hengoed, Mid-Glamorgan CF8 8AU. Reverse-phase Silica Gel The Colpak range of flash chromato- graphy media has been extended by the addition of a reverse-phase CI8 silica gel suitable for biomolecule separations. Sorbsil C200 RP18 is based on bonded silica gel with a 20 nm mean pore diameter, which allows ready access for peptide and proteins of relative molecular mass up to 100000 Daltons.May and Baker Ltd., Liverpool Road, Eccles, Manchester M16 9HF. HPLC Columns The Supelcogel C-610H column is a resin- based HPLC column for analysing organic acids found in food and bever- ages, or used as monomeric and poly- meric additives. Specifically prepared for ion-exchange analyses, it requires little sample preparation, and although analy- ses are best performed at low pH, the column is stable over a wide (1-13) pH range. The Supelcogel C-611 column pro- vides fast, efficient ion exchange analyses of mono- and disaccharides and sugar alcohols.It can be used at flow-rates up to 1.5 ml min-1. It requires little sample preparation, is compatible with many inorganic salts and has a high capacity. It is stable over the pH range 1-13 and at temperatures up to 70 "C. Supelco Inc., Supelco Park, Bellefonte, PA 16823-0048, USA. Packed Column Supercritical Fluid Chromatography After successful evaluation the modular JASCO SFE and SFC systems are now available. The chromatographic system, based on existing JASCO LC-800 HPLC modules, has resolved customer samples as well as SFC standard mixtures. The JASCO LC-800 modules are easily upgraded for supercritical use. The main hardware feature is the fully electronic back pressure regulator which provides extremely stable system pressures that are flow independent.Ciba Corning Diagnostics Ltd., Hal- stead, Essex C 0 9 2DX. High Performance Spherical Silica Kromasil is now, on special request, available in packed columns. A re-pack- ing service of preparative columns is also offered. The columns are high pressure slurry packed. Typical plate numbers for preparative columns are 50 000 per metre on 10 pm Kromasil. The columns are available in sizes from analytical to prepa- rative 5-cm diameter. Kromasil is made in large scale and in 5 , 7, 10, 13 and 16 pm particle sizes, all with the same chemical properties. It is available as plain silica or derivatised with C1, C4, Cx or Clx. Eka Nobel AB, Nobel Industries Sweden, S-445 01 Surte, Sweden. Software for Chromatography Version 3.10 software adds useful capabil- ities to the makers' System Gold personal chromatography system. With the new software users can translate chromato- graphic data points and results into ASCII or Data Interchange formats for use in popular data base and spreadsheet pro- grams.These can be utilised to develop and maintain chromatographic data bases, make special calculations and create graphics using a variety of X-Y plotters and laser printers. Data files can be formatted according to individual requirements and stored automatically on disk. The files can also be transmitted to other computers. Beckman, Progress Road, Sands Indus- trial Estate, High Wycombe, Bucking- hamshire. Standards for Contract Laboratory Programme All of the volatile organic compounds on the US EPA Target Compound List (TCL) are included in a series of five new calibration standards.Highly concen- trated components (2000 yg ml-1) make these standards suitable for purge and trap analyses, multi-point calibrations or use in combinations of two or more mixtures. Supelco Inc., Supelco Park, Bellefonte, PA 16823-0048, USA. Hop Acid Analyser The Shimadzu SN-1 hop acid analyser is built on the LC-6A HPLC system and includes the latest switching technique. The method including sample preparation is completely automatic and saves more than an hour on manual analysis. The SN-1 provides reliable analysis of nine bitter taste substances including a-acids, iso-a-acids and P-acids contained in beer or wort. Dyson Instruments Ltd., Hetton Lyons Industrial Estate, Hetton, Houghton-le- Spring, Tyne and Wear DHS ORH.Ion Chromatography System The Metrohm IC690 ion chromatograph and its auxiliary components, the 697 IC pump and the 698 autosampler, offer ease of use. The system can, for example, provide routine determination of sodium, potassium, lithium, ammonium, magne- sium, calcium, barium and strontium using a single column and a single eluent with electronic suppression, where previ- ously only the use of a gradient elution format with chemical suppression of the eluent could achieve the same results. Two IC690 systems can be combined using a single autosampler 698 with two IC pumps 697 to provide a total ion station, which will give routine separation of. typically, chloride, nitrate, phosphate, sulphate, sodium, ammonium, potas- sium, magnesium and calcium in around 15 min.Also available are Super-sep anion and cation columns. V. A. Howe and Co. Ltd., 12-14 St. Ann's Crescent, London SW18 2LS. Phenol Determination System Aimed at the water supply analyst who has to monitor on a routine basis the concentration of phenol in water, a new automated phenol determination system is capable of monitoring the phenol con- centration to levels some 14 times lower than the current EEC regulations stipu- late, and there is no requirement for sample preparation. Severn Analytical Ltd., Unit 2B, St. Francis Way, Shefford Industrial Park, Shefford, Bedfordshire SG17 5DZ. Automated Thermal Desorber The Model ATD.50 automated thermal desorber and the single shot unit, the Model TD4, were designed to transfer adsorbed atmospheric pollutants quanti- tatively on to a gas chromatograph from adsorption tubes which are compatible with both pumped and diffusive air sam- pling.Specifications for the adsorption tubes and for the ATD50 were set by the UK Health and Safety Executive. Perkin-Elmer Ltd., Post Office Lane, Beaconsfield, Buckinghamshire HP9 1QA. Dust Monitor A new HAM gravimetric dust monitor with a detachable sensor head measures dust, mist, fumes and smoke. The detach- able sensor is attached by a flexible coil. The instrument gives a direct readout in mg m-3 and it has a selectable measuring range from 0-2, 0-20 and 0-200 mg m-3. An optional field gravimetric calibration kit, which can be used with any type of air sampling pump, is available. Environmental Monitoring Systems Ltd., Kingswick House, Kingswick Drive, Sunninghill, Berkshire SLS 7BH.Carbon Dioxide Removal Drier This instrument offers a dewpoint of -70 "C and delivers 2.5 1 min-1 with a remaining carbon dioxide content of less than 2 p.p.m. It requires no electrical connections and it has won a British Design Award. Jun-Air (UK) Ltd., Bridge Street, Lin- wood, Paisley PA3 3DG. pH Meters Three new benchtop pH meters are announced: the pHI32, a standard instru- ment for use in education, the pH1 34, a universal instrument for use in quality control, and the pH1 50, which is opti- mised for bio-research and bio-industrial applications requiring precise readings (its measurements are to 0.001 pH unit).ANALYTICAL PROCEEDINGS. APRIL 1989, VOL 26 139 Beckman. Progress Road, Sands Indus- trial Estate, High Wycombe, Bucking- hamshire.Oxygen Analyser The Model 316R trace oxygen analyser monitors O2 contamination in nitrogen, argon, helium and many other pure gases and gas mixtures. It accurately monitors oxygen from p.p.m. to p.p.b. levels. It features four full-scale switch-selectable ranges: &lo, 0-100, 0-1000 and 0-10 000 p.p.m. of 02. Also available are optional ranges as low as &1 p.p.m. A brochure describes the Series 300 trace and per cent. oxygen analysers, the 317 EXIC, 317 RAC.317 RBC,318 RC,327 RAC, 327 RBC and 328 RC, all CENELEC approved. Teledyne Analytical Instruments, The Harlequin Centre, Southall Lane, South- all, Middlesex UB2 5NH. Microplate Washer The Wellwash-4 is a programmable, auto- matic microplate washing system in which wash procedures are controlled by stan- dard plug-in program cards covering from 1 to 4 wash cycles with either an 8-way or 12-way dispense head.Cards for non- standard routines can be rapidly supplied, and an optional master programmable card is available allowing the user to perform practical wash sequences for most modern plate-based assays. Denley Instruments Ltd., Natts Lane, Billingshurst, West Sussex RH14 9EY. Autosampler The SP3 autosampler complements the recently introduced DMA 48 micro- processor controlled digital density meter. When linked the SP3 and DMA 48 provide a completely automatic system for measurement of density and specific gravity of liquids, gases and concentra- tions of solids. Paar Scientific Ltd., 594 Kingston Road, Raynes Park, London S.W.20.Pressure Gauges and Calibrators The Thommen HM18 provides the means of measuring in the range 0.2-10 bar. Operating on a disposable battery with a life of 200 h, this hand-held. digital instrument is used for tracing faults in pneumatic systems. Valor Flow Control, 475 Foleshill Road. Coventry CV6 5AP. Analytical Balances The new Mettler AT balances feature functionally divided panes which can be displaced automatically by keystroke or manually. They also have sensor and microprocessor circuits which provide full automatic balance calibration. The AT balances include a CL line-current inter- face as well as an RS232C voltage inter- face. There are 3 models: the AT100 with a range of 0-100 g and a readability of 0.1 mg, the AT200 (0-250 g, 0.1 mg) and the AT250 (0-52 g, 0.01 mg and 0-205 g, 0.1 Mettler Instrumente AG, CH-8606 mg).Greifensee. Switzerland. Rheometry Instruments The Rheomat 120 is a new universal system, of modular construction, with three expansion stages allowing reliable and fast evaluation of viscous and elastic characteristics for simple and complex applications. The Covimat 101/105 series instruments are rotational viscometers with concentric cylinder measuring systems to determine the dynamic viscos- ity of liquids. Contraves Industrial Products Ltd., Times House, Station Approach, Ruislip, Middlesex HA4 8LH. Reactor Contalab is a computer controlled labora- tory reactor which can operate 24 h per day. It features a heat balance calorimetry facility . Contraves Industrial Products Ltd., Times House, Station Approach, Ruislip, Middlesex HA4 8LH.Furnaces The Ultraspeed 1800 is designed to meet demands for firing temperatures of 1800 "C. It features a specially developed chamber of graded low thermal mass insulation material. The door opens with the heated area away from the operator and it incorporates electrical interlocks which de-energise the heating elements. The Ultraspeed is currently available with a chamber capacity of 3 1, though it may be supplied in other optional chamber sizes as user needs demand. Lenton Thermal Designs Ltd., 12-14 Fairfield Road, Market Harborough, Leicestershire LE16 9QQ. Autoclaves The PBI autoclaves are available in differ- ent volumes ranging from 17 to 140 1. The automatic models need only initial pro- gramming by the operator, after which the complete cycle is automatic.The combined use of recorder and sterilisation indicator simplifies the validation control. A brochure is available. Pool Bioanalysis Italiana, Via Novara 89, 20153 Milano, Italy. Automation for Microplate Assays The Biomek SL is a labware loading option for the Biomek 1000 automated laboratory workstation. It is capable of transferring labware and pipette tips to and from the Biomek 1000 tablet without operator intervention. Beckman, Progress Road, Sands Indus- trial Estate, High Wycombe, Bucking- hamshire. Lenton Thermal Designs Ultraspeed 1800 fiirtiuce140 ANALYTICAL PROCEEDINGS, APRIL 1989, VOL 26 Scintillation Medium Ready Cap is a solvent-free scintillation medium for counting radiolabelled mi- crosamples.It is ideal for the measure- ment of non-volatile radiolabelled sub- strates in a volatile liquid carrier and it can be used in the makers’ or other LS counters. Beckman, Progress Road, Sands Indus- trial Estate, High Wycombe, Bucking- hamshire. Liquid Scintillation Counters The Series LS 5000 benchtop liquid scin- tillation counters feature the makers’ H-number quench monitor, which assures accurate DPM results for single or dual labelled samples, regardless of the type of cocktail or vial, volume of sample or isotope ratio. Three models are available in the series: the LS 5000 CE, the LS 5000 TD and the LS 5000 TA. Beckman, Progress Road, Sands Indus- trial Estate, High Wycombe, Bucking- hamshire. Non-isotopic Library Screening Systems No isotopes are needed for the Screen-A- Gene library screening systems.The Bio- tin-Blot Clone detection kits use biotin- ylated DNA probes to screen phage or colony libraries and offer high signal-to- noise ratio. Lambda g t l l libraries can be screened for expressed proteins with the Lambda-Lift expression detection kit. Bio-Rad Laboratories S.A., 19 Dreve De Senkchal, B1180 Brussels, Belgium. Petroleum Sulphonates The Focus range of petroleum sulphon- ates, with their excellent corrosion protection and emulsifying qualities, are ideal for the soluble oils market. De- watering fluids, dry cleaning aids, lubri- cant additives, dispersants, flotation and stabilising agents and aircraft de-icers are among the variety of end uses. Carless Refining and Marketing Ltd., St.James’s House, Eastern Road, Rom- ford, Essex RM1 3NL. Water Filtration System Timesander water filters, based on Man- ganese Greensand, are used for removing soluble iron, manganese and hydrogen sulphide from well waters. Manganese Greensand, a purple - black filter medium processed from glauconitic greensand, will perform over a pH range of 6.2 to 8.8 and it is easily regenerated with a weak solution of permanganate. United Engineering Ltd., Charterland House, 225 1 Coventry Road, Sheldon, Birmingham B26 3NX. Cleaning Agents Neodisher GK and Deodisher MA are powdery mild-alkaline cleaning agents without surfactants for special laboratory equipment washing machines. Neodisher GK will remove residual media, cell-cul- ture and tissue remnants, radioactive contaminations, organic dye and pigment impurities and has uses in laboratory equipment washing machines in all med- ical, industrial and food laboratories. Neodisher MA gently removes residual media, blood, proteins, baby foods and chemicals.The Scientific Instrument Centre Ltd., Unit 34D, Parham Drive, Boyatt Wood, Eastleigh, Hampshire SO5 4NU. Software Package for Scientific Authors The Reference Manager scientific soft- ware program retrieves full references from 20 000 entries in less than 5 s and allows a scientific or medical author to store up to 32000 bibliographic refer- ences. It can be used with TBM PC/XT/ AT and PS/2 personal computers and microcomputers that support MS/PC- DOS operating systems. Beckman, Progress Road, Sands Indus- trial Estate, High Wycombe, Bucking- hamshire.Literature GammaBind G high performance affinity chromatography (HiPAC) columns are the subject of a new data sheet. This shows how HiPAC silica support linked with a GammaBind G affinity probe binds IgG sub-class antibodies from human, mouse (including IGgl) and rat serum in under 10 min. The new product line carries the advantages of not binding IgM, IgE, IgA, IgD or serum albumin. ChromatoChem Inc., 2837 Fort Mis- soula Road, Missoula, MT 59801, USA. An application data sheet gives full details of the determination of the concentration of certain inorganic ions in tap water using the Shimadzu HIC-6A ion chromato- graph. The HIC-6A separates ions on an ion-exchange column and detects them by means of a conductivity detector.Dyson Instruments Ltd., Hetton Lyons Industrial Estate, Hetton, Houghton-le- Spring, Tyne and Wear DH5 ORH. FLEC (fluorenyl ethyl chloroformate) is described in a new brochure. Application sheets are submitted with the brochure. Available in 1 ml and 10 ml bottles, either in the [ +] form or as its [ -1 isomer, FLEC quickly derivatises primary and secondary amines, amino acids and alcohols to diastereoisomers, which are then sepa- rated by ordinary reverse phase chromato- graphy. Eka Nobel AB, Nobel Industries Sweden, S-445 01 Surte, Sweden. Chromatography Update, Autumn 1988, includes items on NuGel Affinity-Pacs, solid phase extraction columns, Nucleogen HPLC columns, NuGel P-AC for adsorption chromatography, new reversedhormal phase TLC plate and silica gel plates for TLC.Camlab Ltd., Nuffield Road, Cam- bridge CB4 1TH. A brochure describes Chromafil dispos- able filters and Chromabond columns for selective sample preparation for GC, HPLC, TLC, spectroscopy, ion chromat- ography, etc. Camlab Ltd., Nuffield Road, Cam- bridge CB4 1TH. Sigma ImmuNotes number 1, 1988, gives details of ExtraAvidin staining kits, new antibodies to cytoskeletal proteins and new monoclonal antibodies. Sigma Chemical Co. Ltd., Fancy Road, Poole, Dorset BH17 7NH. A brochure introduces the RABIT rapid automated bacterial impedance tech- nique. The equipment described can be expanded to a maximum of 512 channels and each 32-channel block can run at a different temperature. Temperature con- trol is better than k0.005 “C. Don Whitley Scientific Ltd., 14 Otley Road, Shipley, West Yorkshire BD17 7SE.Literature gives details of the Labshield fume removal safety system, with separ- ate sections on the fume cupboard, the gas scrubbers and the flanged ducting. Labshield (UK) Ltd., 51-59 Bancrofts Road, Eastern Industrial Estate, South Woodham Ferrers, Chelmsford, Essex CM3 5UG. The Serva 1989 Fine Biochemical Cata- logue deals with 800 new products and includes special sections on electrophor- esis, gas chromatography, liquid chromat- ography, peptides, ion exchangers, mol- ecular biology, tissue culture and immu- nology. Uniscience Ltd., 12-14 St. Ann’s Cres- cent, London SW18 2LS. A brochure describes the new GenELISA software available for the Beckman Biomek automated laboratory worksta- tion, providing a capability for fast rou- tine ELISA work. The brochure illus- trates the single computer screen which helps users to enter assay parameters easily. Beckman, Progress Road, Sands Indus- trial Estate, High Wycombe, Bucking- hamshire. Nalgene Products News, Vol. 7, No. 1, features the latest Nalgene labware pro- ducts, including the newest members of the Nalgene square bottle family, the award-winning PETG square media bot- tles. Also featured are Media-Plus and serum filter units, the 4-1 heavy-dutyANALYTICAL PROCEEDINGS. APRIL 1989. VOL 26 141 bottle, the new desiccator cabinet, affinity tional information on gel separations and chromatography units and matrix, vac- Nalgene Company, 75 Panorama measurement by scanning spectropho- uum manifold break-resistant filter fun- Creek Drive, Box 20365, Rochester, New tometry, optimising information from nels with clamp, dilution bottle and multi- macromolecules. bottle racks, microcentrifuge tube box Beckman, Progress Road, Sands Indus- and storage box, fillinghenting closure, trial Estate, High Wycombe, Bucking- barbed bulkhead fitting and new animal hamshire. science products. York 14602-0365, USA. Beckman technical and support staff will be pleased to offer guidelines and addi-

ISSN:0144-557X    

DOI:10.1039/AP9892600137

出版商:RSC    

年代:1989

数据来源: RSC

摘要:

ANALYTICAL PROCEEDINGS. APRIL 1989. VOL 26 141 SAC 89 Update Courses The two previous SAC conferences have featured a set of intensive one-day courses on the Wednesday which have proved very popular with delegates. These Update Courses are designed to survey developments in analytical techniques and methodology of topical importance. The emphasis is on topics for which commercial instrumentation or facilities are available or are emerging, and thus the courses are designed very much for the practising analytical chemist. Aims and Structure The courses will provide a rapid, econom- ical introduction to the basic concepts of each topic, together with a survey of applications and likely future trends. I n general, the courses will mix lectures, tutorials and discussion sessions with hands-on practical work and demonstra- tions.Several manufacturers and organ- isations will be providing “state of the art” equipment or facilities. The courses are designed to take advan- tage of the international nature of the SAC Conference and not only are the course leaders well-known in their re- spective fields both as researchers and teachers, but many of the contributors to the courses are internationally known experts. Each course represents a unique opportunity to meet some of the world’s leading analytical scientists. Numbers on the courses will be restricted to allow the most effective use of resources and main- tain the high-quality reputation that these courses have developed. Topics The topics for the courses are: Chiral Separations, led by Dr.David Taylor of UMIST; Chemiluminescence and Biolu- minescence, led by Dr. Paul Worsfold of Hull University; Near Infrared Spectro- scopy, led by Mr. Tony Davies of Oxford Analytical Instruments Ltd. ; Laser-Based Analytical Mass Spectrometry, led by Professor Robert Donovan of the Univer- sity of Edinburgh; and Information Tech- nologies for Analytical Chemists led by Mrs. Cheryl Teague of the Royal Society of Chemistry Information Services. Chiral Separations Since the withdrawal of thalidomide because of the notorious side effects of the unwanted enantiomer in this racemic drug, international regulatory bodies have become ever more reluctant to permit the registration of racemic sub- stances. The target requirement is that new formulations and the supporting analytical procedures are based on accu- rately known levels of each enantiomeric substance.This has placed an additional and onerous responsibility upon indus- trial analysts who support not only the development and process chemists, aim- ing at bulk manufacture of pure enan- tiomers, but also the pharmacologists assessing the metabolism and biological effects of each enantiomer. As a direct result, a large number of new chromatographic column packings have been developed for both HPLC and GC, capable of separating enantiomers as well as diasterioisomers. This profusion of column packings, although offering a useful range of selectivities, has led to a demand for training opportunities in which chromatographic analysts can fam- iliarise themselves with such new pro- cedures. The Update will address this need by providing opportunities in which partici- pants can work out appropriate condi- tions for typical chiral separations on a variety of recently developed commercial column packings.In addition to the Course leader, Dr. David Taylor, one of the UK’s leading researchers in this area, contributors to the Update will include Professor Bill Pirkle (inventor of the well-known Pirkle columns and one of the four plenary lecturers at SAC 89), who will cover HPLC column selection, Dr. Gerald Gubitz (University of Graz, an expert on chiral ligand-exchange LC), Professor Konig (University of Hamburg, inventor of the perpentylcyclodextrin phase for chiral LC) who will deal with GC separa- tions, Dr. David Lloyd (University of York, involved in the development of a recently launched chiral detector for HPLC) and Dr.Irving Wainer (St. Jude Children’s Hospital, Memphis, an expert on the HPLC of chiral drugs) who will cover optimisation in HPLC. There will also be sessions on the industrial analysts requirements and an introductory overview of strategies for chiral separations. Chemiluminescence and Bioluminescence The emission of light from chemical reac- tions at room temperature by the radi- ative decay of an excited state species formed in the chemical reaction provides exceptionally low limits of detection owing to the absence of any other source of photons in the system. Selectivity can be conferred by the judicious choice of primary reaction and reaction conditions. The Update will provide a comprehen- sive treatment of chemiluminescent reac- tions and their analytical applications and will cover the following topics: Introduc- tion (theoretical aspects, kinetics, instrumentation, solid, liquid and gas- phase reactions); Classical Liquid-phase Reactions (peroxyoxalate, luminol, lugigenin); Post-column Detection; Gas- phase Reactions (ozone, sulphur, phos- phorus); Bioluminescence (firefly and bacterial luciferase, coupled reactions, clinical and biotechnology reactions); Chemiluminescent Immunoassays (isolu- minol, acridinium ester and peroxidase labels).The practical session will include demonstrations of chemiluminescence reactions and hands-on experience of chemical instrumentation for gas-phase and liquid-phase reactions and in-house flow-injection techniques.The course tutors will be drawn mostly from the members of the Analytical Science Group staff of the Chemistry Department at Hull University, which has an international reputation for research in this area, parti- cularly in the use of flow-injection and flame techniques, and will include Profes- sor Alan Townshend (one of the four Plenary Lecturers at SAC 89). Near Infrared Spectroscopy Near infrared (NIR) spectroscopic analy- sis is well known as a rapid method of analysis for the constituents of crops and foodstuffs, The use of NIR for the analy- sis of the protein content of wheat is in142 ANALYTICAL PROCEEDINGS. APRIL 1989, VOL 26 world-wide use and has had a major impact on the international wheat trade. NIR analyses are also used in the chemical, mining, petrochemical, plastic, pharmaceutical and textile industries.Few chemists have received any educa- tion about absorptions in the NIR region, and the application of NIR analysis has been limited more by the lack of com- prehension of the technique than by experimental problems. The Update Course aims to redress this situation by providing a basic grounding in the method for those with limited or no experience of NIR analysis. The course will consist of lectures and practical sessions covering: basic theory of absorption in the NIR region; instrumentation; statistics; sample selec- tion, preparation and presentation; the problem of reference analysis; practical experience with NIR instruments (includ- ing the use of computer programs to produce and test calibrations from NIR data); and current developments and future prospects.The course leader will be Tony Davies, who until recently worked at the Institute of Food Research, but has now joined Oxford Analytical Instruments as Senior Product Specialist to help develop the first British NIR instrument for general use. Tony has been involved in NIR analysis since 1979 and has been instrumental in promoting the use of the technique through the organisation of several RSC meetings and conferences on the topic. He has been collaborating with his co- tutor, Professor w . Fred McLure of the Department of Agricultural Engineering at the North Carolina State University, since 1982 on the application of Fourier transformation as a tool for NIR data processing.Professor McLure’s involve- ment in NIR analysis dates back to 1968. His original work concerned the design and construction of a scanning instrument and applications to tobacco constituents. Laser Based Analytical Mass Spectrometry After many years of research orientated studies, laser based analytical techniques are now in a phase of rapid commercial development. The ultimate limit of single atom detection has been achieved and rapid advances are currently taking place in the analysis and sequencing of biolo- gical materials. The Update will start with a general introduction and historical perspective of laser based analytical mass spectrometry. The hierarchy of methods that have been employed will be reviewed and fun- damental aspects of laser ionisation and ablation will be introduced.Individual methods will be dealt with, starting with techniques for ablation coupled with inductively coupled plasma mass spec- trometry. This will be followed by an introduction to methods that use the laser directly for ablation and ionisation under vacuum and to the laser microprobe technique. Applications of laser micro- probe analysis will be reviewed and ex- amples will be illustrated using data dis- played with commercial computer soft- ware. The final session will deal with meth- odologies for resonant ionisation, includ- ing the most recent instrumentation which employs separate steps for laser desorp- tion and ionisation. Tutorials and demon- strations will be used to supplement the lecture material. The course will be run by Professor Robert Donovan, one of the UK’s leading researchers in the field.Following his Welsh BSc (Aberystwyth) and his English PhD (Cambridge) he moved to his present Scottish institution (Edinburgh University) as lecturer in physical chemistry in 1970. He was promoted to reader in 1974 and to a Personal Chair in 1979. During his three-year period as Head of Department, he was appointed to the Chair of Chemistry at the University. In 1975, he was awarded the Corday- Morgan Medal and prize of the RSC. A number of other European researchers will be involved in tutoring the course. Information Technologies for Analytical Chemists The increase in the analytical literature makes effective searching difficult and time consuming unless computer based techniques are used.Computerised data bases are also invaluable aids in the interpretation of spectral data (particu- larly mass and infrared) and the modern analytical laboratory generates so much information that a computer based infor- mation management system is required to keep accurate track of it. Proficiency in the use of information technologies is as much part of the analytical chemist’s armoury of skills as is knowing the scope and limitations of the instrumental tech- niques in use in the laboratory. The course aims to provide an aware- ness of what information technologies are currently available and to offer first hand experience in the use of some of these tools at the RSC’s new facility in Cam- bridge. The course will be led by Mrs. Cheryl Teague, who as an RSC IT specialist spends much of her time lecturing and training in the chemical industry through- out Europe. Topics to be covered will include, Analytical Abstracts, Chemical Abstracts, the Mass Spectrometry Data Centre, Software for Analytical Chem- ists, The IR Spectrafile, Consultancy-type Information Services and the Provision of Information through Industrial Libraries. Other RSC staff will be involved, together with specialist staff from other IT com- panies. Registration Details of registration are available with the Notes to Participants for the SAC 89 Conference. The courses are open to delegates who are not registered for the SAC 89 Conference (a slightly higher registration fee is payable for such del- egates), but in either case early registra- tion is advisable as the course topics are likely to prove particularly popular. Preference will be given, in cases of over-booking, to delegates also registered for the SAC 89 Conference. All enquiries should be addressed, in the first instance, to Miss P. E. Hutchinson, Secretary of the Analytical Division, Royal Society of Chemistry, Burlington House, London W1V OBN.

ISSN:0144-557X    

DOI:10.1039/AP9892600141

出版商:RSC    

年代:1989

数据来源: RSC

摘要:

142 ANALYTICAL PROCEEDINGS. APRIL 1989, VOL 26 Recent IUPAC Recommendations Definitive Recommendations symbolism of interest to analysts have Values for Infrared and Raman Intensity The following definitive recomrnenda- been published since January, 1988. Measurements, Pure Appl. Chem., 1988, tions on nomenclature, terminology and Presentation of Molecular Parameter 60, 1385.ROYAL SOCIETY OF CHEMISTRV lnformat ion Services NUCLEAR MAGNETIC RESONANCE Vol. 17 Senior Reporter: G. A. Webb, University of Surrey Nuclear Magnetic Resonance Volume 17provides a review of the literature published between June 1986 and May 1987. Brief Contents: N.M.R. Books and Reviews; Theoretical and Physical Aspects of Nuclear Shielding; Applications of Nuclear Shielding; Theoretical Aspects of Spin-Spin Couplings; Nuclear Spin Relaxation in Liquids; Solid State N.M.R.; Multiple Pulse N.M. R. ; Natural Macromolecules; Synthetic Macromolecules; Conformational Analysis; Nuclear Magnetic Resonance of Living Systems; Oriented Molecules; Heterogeneous Systems. Nuclear Magnetic Resonance Volume I 7 contains a foreword by the Senior Reporter, and a detailed contents list. Each chapter includes extensive references. ISBN 0 85186 402 3 Hardcover 546 pages Specialist Periodical Report (1988) Price E l 10.00 ($220.00) SPECTROSCOPIC PROPERTIES OF INORGANIC AND ORGANOMETALLIC COMPOUNDS VOl. 21 Senior Reporters: G. Davidson, UniversityofNottingham, and E. A. V. Ebsworth, University of Edinburgh This book reviews the recent literature published up to late 1987.Brief Contents: Nuclear Magnetic Resonance Spectroscopy; Nuclear Quadrupole Resonance Spectroscopy; Rotational Spectroscopy; Characteristic Vibrations of Compounds of Main-group Elements; Vibrational Spectra of Transition- element Compounds; Vibrational Spectra of Some Co- ordinated Ligands; Mossbauer Spectroscopy; Gas-phase Molecular Structures Determined by Electron Diffraction. ISBN 0 85186 193 8 Hardcover 525pp Specialist Periodical Report (1988) Price 3320.00 ($240.00) For further information, please write to: Royal Society of Chemistry, Sales and Promotion depart1 Thomas Graham House, Science Park, Milton Road, Cambridge CB4 4WF. U.K. nent. To Order, please write to: Royal Society of Chemistry, Distribution Centre, Blackhorse Road, Letchworth, Herts SG6 1HN.U.K. or telephone (0462) 672555 quoting your credit card details. We can now accept AccessIVisd MasterCard/Eurocard. RSC Members are entitled to a discount on most RSC publications and should write to: The Membership Manager, Royal Society of Chemistry, Thomas Graham House, Science Park, Milton Road, Cambridge CB4 4WF. U.K.ROYAL SOCIETY Of CHEMISTRY ciEMKALsARTY cH%SHERz; @ lnformat ion Services All solvents have hazardous properties, yet find ubiquitous use in industry and are among the most widely used chemicals in society. This important new book aims to cover every aspect of the hazards of these solvents, providing invaluable information in a concise but readable format, with full references for further investigation if required. Chemical Safety Data Sheets Volume 1 - Solvents provides up-to-date information on over 100 representative solvents. Included will be the full range of CHEMICAL, PHYSICAL AND BIOLOGICAL hazards likely to be encountered by their use, as well as safe handling, emergency precautions, CHEMICAL SAFETY DATA SHEETS 1 Volume 1 - Solvents Volume 2 is scheduled for publication mid 1989 and will be entitled Main Group Metals and their Compounds. SOLVENTS IN COMMON USE: HEALTH RISKS TO WORKERS ISBN 0 85186 088 5 Hardcover 308pp Published 1988 Price E60.00 ($120.00) For further information, please write to: Royal Society of Chemistry, Sales and Promotion department, Thomas Graham House, Science Park, Milton Road, Cambridge CB4 4WF.U.K. To Order, please write to: Royal Society of Chemistry, Distribution Centre, Blackhorse Road, Letchworth, Herts SG6 1HN.U.K. or telephone (0462) 672555 quoting your credit card details. We can now accept AccesslVisal MasterCard/Eu rocard. RSC Members are entitled to a discount on most RSC publications and should write to: The Membership Manager, Royal Society of Chemistry, Thomas Graham House, Science Park, Milton Road, Cambridge CB4 4WF. U.K.ANALYTICAL PROCEEDINGS, APRIL 1989. VOL 26 145 Nomenclature, Symbols, Units and Their Usage in Spectrochemical Analysis. VII: Molecular Absorption Spectroscopy, Ultraviolet and Visible (UViVIS), Pure Appl. Chem., 1988, 60, 1449. X: Preparation of Materials for Analy- tical Atomic Spectroscopy and Other Related Techniques, Pure Appl. Chem., 1988, 60, 1461. Comments on these recommendations would be welcomed, addressed to the originating IUPAC Commission (for addresses see the appropriate issue of Piire Appl.Chem.), with copies to Dr. Alan McNaught, Secretary, Joint Royal SocietyiRoyal Society of Chemistry Panel on Chemical Nomenclature, Thomas Graham House, Science Park, Milton Road, Cambridge CB4 4WF, UK. Provisional Recommendations IUPAC has recently made available several sets of provisional nomenclature and symbols recommendations, sum- marised as follows. Classification of analysers in clinical chemistry A classification scheme is suggested which should be helpful in making understand- able the various concepts of mechanised and automated analytical systems. It should be used as a guide for teaching automation in clinical chemistry, and as a base for describing new instrumentation by manufacturers and professionals.A mechanised analytical system com- prises an analyser and the reagents required to perform a specified analysis. The term analyser describes a measuring system, which is defined as a complete set of measuring instruments and other equipment assembled to carry out a speci- fied measurement task. Usually analytical systems are classified according to the principle of their trans- port system, e.g., discrete and flow pro- cedures. In the document a further sub-division is achieved by considering methodology, number of tests, sampling and processing procedures or test selec- tion. Common examples are included in the scheme presented. Comments by December 31, 1989. Glossary of atmospheric chemistry terms The Glossary contains definitions of over 600 scientific terms in common use in atmospheric chemistry. The diversified nature of the scientists involved in research in atmospheric chemistry, che- mists, meteorologists, physicists, biolo- gists, engineers, health scientists, and others, points to the very special need for a definition of the common terms employed by each specialist.The Glos- sary was prepared to provide unambigu- ous definitions of terms and units employed by the international research community in atmospheric chemistry to help achieve reliable communications between all parties. Where alternative terms are in common use to describe a given process, piece of equipment, feature or quantity used in atmospheric chemistry, recommended choices are given.The range of terms includes those encountered in describing the properties and composition of the atmosphere, clouds, solar-radiation, chemical and physical changes in atmospheric com- ponents, instrumentation employed in analysis of the atmospheric components and in air quality control, and in effects of certain trace gases on materials, plants, and animals. Comments by October 31, 1989. Proposals for the description and measure- ment of analytical carry-over effects in clinical chemistry Carry-over phenomena occur both in manual and mechanised procedures and are often neglected in practice. Even with the latest development of clinical chem- istry analysers, carry-over phenomena are observed. This paper makes recommen- dations concerning the terminology of carry-over and its classification.The con- ceptual aspects of specimen-dependent and specimen-independent carry-over are outlined, and both the experimental determination and calculation of carry- over effects are described in detail. The term carry-over is commonly used to describe a process by which extraneous materials are carried into a reaction mix- ture. These materials can be either parts of a specimen, or reagents including the diluent or wash solution. In such instances carry-over means the transfer of material (specimen or reagents) from one con- tainer, or from one reaction mixture, to another one. It can be either unidirec- tional or bidirectional in a series of specimens or assays. Carry-over effects should be expressed in units (e.g. , in moll-’ or U 1-1) which are used to present the results rather than as quantity fractions. This concept of present- ing carry-over effects as a difference of two results or its corresponding percentage value has two advantages: it isapplicable to all conditions which at present are encoun- tered in practice, and it directly informs on how much a particular result deviates from the correct value which is obtained in the absence of carry-over effects. Comments by December 31, 1989. IUPAC would welcome comments on these recommendations, prior to the pro- duction of definitive versions for publica- tion in Pure Appl. Chem. Copies of the texts can be obtained on request from Dr. Alan McNaught, The Royal Society of Chemistry, Science Park, Milton Road, Cambridge CB4 4WF, UK. In order that comments may be considered by IUPAC, they should be received by the dates given above.

ISSN:0144-557X    

DOI:10.1039/AP9892600142

出版商:RSC    

年代:1989

数据来源: RSC

摘要:

ANALYTICAL PROCEEDINGS, APRIL 1989, VOL 26 145 Conferences and Meetings Chromatography Into the '90s April 27, 1989, Londori The Chromatographic Society are holding their Spring Symposium on Thursday April 27 at The Shell Centre on London's South Bank. The programme covers a wide range of subjects including GC/ FTIR/MS , Capillary Zone Electrophore- sis, SFC and Injection Flow Analysis. The main speakers include Professors Engle- hardt and J. N. Miller and Dr. C. F. Simpson. Lunch is included and there is also an exhibition. Further details are available from: The Executive Secretary, The Chromato- graphic Society, Trent Polytechnic, Bur- ton Street, Nottingham NG1 4BU. Food Microstructure May 1-5, 1989, Salt Lake City, Nevada, USA Food Microstructure will be the subject of a programme scheduled at the Red Lion Inn, Salt Lake City.Emphasis will be on food structure as it relates to processing and ingredient changes, storage, product acceptability and other aspects of dairy, meat, cereal and oil products. Over sixty papers were presented at the last Food Microstructure programme held in Read- ing in September, 1988. The organizers of the program are S. H. Cohen of the US Army Natick R&D Command Food Research Laboratory, Natick, MA, E. A. Davis of the Univer- sity of Minnesota, St. Paul, D. N. Hol- comb of the Kraft Technology Center,146 ANALYTICAL PROCEEDINGS. APRIL 1989, VOL 26 Glenview, IL, M. Kalab of the Food Research Branch, Agriculture Canada, Ottawa and W. Wolf of the USDA in Peoria, IL. The organisers are also the Editors of the semi-annual journal, Food Microstructure.More information about the pro- gramme, including housing arrangements and other details, may be obtained from any of the organisers or from Dr. Om Johari at the SMI office. Fifth International Symposium of the ISSA Section “Iron and Metal Manufac- turing Industry” May 8-1 1, 1989, Mainz, FRG This symposium will be in two parts: “Occupational Safety and Health-hdi- cators of Management Quality”; and “Dangerous Substances-New Findings and Problems.” The latter part will be divided into Cutting Coolants and Weld- ing Fumes. The address of the Secretariat is: Arbeitsgemeinschaft der Eisen- und Metall-Berufsgenossenschaften, Kreuz- strasse 45, D-4000 Dusseldorf 1, Bundes- republik Deutschland. The New Regulations Controlling Labora- tory Work with Chemicals May 16, 1989, London The Control of Substances Hazardous to Health Regulations were made in October, 1988, and will come into force in October, 1989.They represent one of the most significant pieces of safety legisla- tion since the Health and Safety at Work Act of 1974 and will apply to all work- places, including laboratories. A period of time is allowed between the making of the Regulations and their coming into force so that all employers can prepare to meet the new obligations that they impose. This meeting will prepare atten- dees for October 1989 and alert them to the measures needed to meet the regula- tions. Most existing legislation is limited to a particular substance or process and applies only to factories.The COSHH Regulations will replace much of this and will set out the principles of occupational hygiene to be followed in all workplaces. Employers will be required to carry out an assessment of any work situation which may expose employees to a hazardous substance. The implications of this and the other requirements for laboratories are far reaching. It will be necessary to have a more systematic approach to assessing risk, to making decisions on control methods, to using and maintain- ing controls, and to deciding whether ongoing monitoring or health surveillance is needed. This meeting will cover the content of the regulations, will show what the new statutory requirements mean in practical terms for the management of laboratories, and will provide an oppor- tunity to discuss problems with other participants and the panel of speakers.Each participant will be provided with a copy of the Regulations, which includes the Approved Codes of Practice. The Meeting will be held in The Com- monwealth Institute, Kensington High Street, London W.8. For information write to Scientific Symposia Ltd., 33-35 Bowling Green Lane, London EClR ODA. Third International LIMS Conference June 6-8, 1989, Egham The Third International LIMS Confer- ence, the most significant meeting on this subject to be held in Europe, will take place at the Anugraha Conference Cen- tre, Egham, Surrey. The initial announce- ment of the conference attracted con- siderable interest and the organising com- mittee are currently finalising a technical programme of the highest calibre.The first two conferences in the series, both held in the USA, brought together state of the art knowledge of LIMS (Laboratory Information Management Systems) and associated techniques. This third international conference will con- tinue the tradition, focusing on the latest thinking on LIMS, from implementation strategies to the effect on quality and GLP and from automation to networking and the future impact of information tech- nology in the laboratory. A distinguished panel of speakers will include: Mr. Richard Mahaffey (Eastman Kodak) on LIMS and the Foundation of Information Technology in the Labora- tory; Dr. Nancy Woo (Merck) on LIMS and Quality; Dr. Rolf Arndt (Mettler) on LIMS and Automation; and Mr. Ken Leiper (Glaxo) on the Future of LIMS in the Laboratory.The conference will be of particular interest to laboratory and cor- porate management, analytical chemists, quality assurance and computing special- ists, production and control engineers and all those interested in the wide ranging application of this technology. Further details of the conference can be obtained from Dr. C. J. Jackson, Health and Safety Executive, Broad Lane, Shef- field S3 7HQ. Gordon Research Conference August 7-1 1, 1989, New Hampton, N H , USA The analytical Gordon Research Confer- ence will be held at New Hampton School. The topics discussed will be: Nuclear Magnetic Resonance Structural Techniques; NMR Imaging; Polymer Characterisation; Capillary Electro- phoresis; Optical Imaging; Nuclear Characterisation of Electrode Surfaces; Expert Systems; and Near-infrared Spec- t roscopy .For further information contact: Mr. A. M. Cruickshank, Gordon Research Center. University of Rhode Island, Kingston, Rhode Island 02881-0801, USA. Analysis for Drugs and Metabolites, Including Anti-infective Agents September 5-8, 1989, Guildford The focus of this, the 8th International Bioanalytical Forum, held in the Univer- sity of Surrey, is the setting up of sensitive methods, especially chromatographic, for drugs in blood, with some emphasis on anti-infectives, including antivirals and antiparasitics, on immunosuppressives, and on relevant metabolites. State of the art topics include HPLC pre-column steps, laser detection, TLC - MS, biosen- sors, NMR, and the selectivity of RIA.There will be attention given to detection limits, statistics, and other aspects per- tinent to producing results acceptable to regulatory authorities. The contributions, near-40, will be largely from pharmaceut- ical company staff. The fee (f104) includes the post-Forum book. On-site living costs are about &27 per day. Attendance is limited to 100 persons. Address brochure requests to Dr. E. Reid (Chief Organiser), Guildford Academic Associates, 72 The Chase, Guildford GU2 5UL. 103rd AOAC Annual International Meet- ing and Exposition September 25-28, 1989, St Louis, M O USA This meeting will be held at the Clarion Hotel, St Louis, Missouri, and will spot- light “Environmental Concerns In the Laboratory and Community-Who’s Taking the Risks?” The Symposia will be on: “Laboratory Information Manage- ment Systems; Laboratory Waste Dispo- sal Technology; Enantiomeric Separa- tions; Risk Management in the Labora- tory; Detection of Environmental Con- taminants and Natural Toxins in Food Products of Animal Origin; and Methods of Analysis for Drugs of Abuse.” The subject of the keynote lecture will be “Scientific Progress versus Environmental Safety-a Morality play for the Next Century.” For further details contact: the Associa- tion of Official Analytical Chemists, Suite 400. 2200 Wilson Boulevard, Arlington, VA 22201-3301, USA. Analyticon ’89 September 26-28, 1989, London Analyticon 89 will be held at the Olympia Conference Centre, London W14. This is a month earlier than in 1988 but again coincides with other events in the British Laboratory Week.A programme of eigh- teen topics has been set by the Pro- gramme Advisory Committee and these will be dealt with in half-day sessions. Laboratory economics, which was notANALYTICAL PROCEEDINGS. APRIL 1989, VOL 26 147 covered specifically in 1988, will be re- introduced. Other repeats from earlier programmes include rapid microbio- logical methods and laboratory informa- tion management systems. The problems associated with the new COSHH regula- tions will be covered. Other topics in the safety category include good laboratory practice, process analysis, expert systems and quality assurance. Immunoassays, FTIIR. LCIED, LCI MS and thermal methods will feature amongst the sessions on specific labora- tory techniques. Techniques for environ- mental monitoring will also be covered.Data treatment and evaluation will be covered at two levels; one session on elementary statistics and another on more advanced chemometric techniques. For an insight into the rapidly increasing variety of software packages for labora- tories there will be a new session. Also topical will be a special session for dis- cussion of the implications of 1992 for laboratories. In order to receive the complete pros- pectus, detailing the lectures and speakers for each session, contact the organisers of Analyticon 89, Scientific Symposia Ltd, 33-35 Bowling Green Lane. London EClR ODA. Third International Meeting on Chemical Sensors October 1-5, 1989, Toronto, Canada This meeting will take place in L’Hotel, Toronto. For information contact Profes- sor M.Thompson or Professor U. J. Krull, Department of Chemistry, Univer- sity of Toronto, 80 St. George Street, Toronto, Ontario, Canada M5S 1Al. 2nd International Symposium on Philo- sophy and History of Analytical Chemistry and Their Consequences October 6-7, 1989, Vienna, Austria The above symposium is to be organised by the Institute for Analytical Chemistry of the Technical University of Vienna and the Austrian Society for Microchemistry and Analytical Chemistry and supported by the Working Party on Analytical Che- mistry of the Federation of European Chemical Societies. The invited lecturers on the philosophy of analytical chemistry will be J. Brandmuller, G. Eder, A. Lewenstam, H. Malissa, 0. Preining, G. Vollmer and H. Zemanek, while those on the history of analytical chemistry will be D.Thorburn Burns, L. Niinisto, U. Palm and E. Roth. There will also be discussion sessions on Analytical Chemistry Towards the 21st Century and Future Trends in Teaching Analytical Chemistry. For all topics discussion contributions of 5-10 minutes duration are invited. For further details contact: Professor M. Grasserbauer, Technical University of Vienna, A-1060 Wien, Getreidemarkt 91151, Austria. Euroanalysis VII August 26-31, 1990, Vienna, Austria This meeting, organised by the Federa- tion of European Chemical Societies and the Austrian Society for Microchemistry and Analytical Chemistry, is to be held in the Technical University of Vienna. The scientific programme will consist of invited plenary and keynote lectures, contributed papers, special sessions and workshops. Possible topics for contri- buted papers are Applications of analy- tical chemistry (Environmental Systems and Food, Pharmaceutical and Biomed- ical Science, Biotechnology , Materials Science and Arts and Archaeology), Methods of Analytical Chemistry (Atomic Spectroxopy, Molecular Spec- troscopy, Separation Techniques, Elec- trochemical Methods, Sensors, Radio- chemical and Nuclear Techniques, Ther- mal Analysis, Local and Surface Analysis, Structure Analysis of Solids, Immunoas- say, Other Methods) or Special Sessions and Workshops (Sampling and Sample Preparation, COBAC V, Quality Assur- ance in Analytical Chemistry, New Trends in Teaching Analytical Chem- istry). For information write to: Euroanalysis VII, Professor Dr. M. Grasserbauer, c/o Interconvention, Austria Centre Vienna, A-1450 Vienna, Austria.

ISSN:0144-557X    

DOI:10.1039/AP9892600145

出版商:RSC    

年代:1989

数据来源: RSC