ISSN:0144-557X    

DOI:10.1039/AP98219FX032

出版商:RSC    

年代:1982

数据来源: RSC

ISSN:0144-557X    

DOI:10.1039/AP98219BX034

出版商:RSC    

年代:1982

数据来源: RSC

摘要:

ANPRDI 19(10) 455-508 (1 982) October 1982 Analytical Proceedinas I - Proceedings of the Analytical Division of The Royal Society of Chemistry AD President S. Greenfield Hon. Secretary Hon. Treasurer R. Sawyer D. C. M. Squirrel1 Hon. Assistant Secretary D. 1. Coomber, O.B.E. Hon. Publicity Secretary Dr. J. F. Tyson, Department of Chemistry, Loughborough University of Technology, Loughborough, Leicestershire, LE11 3TU Secretary Miss P. E. Hutchinson Editor, Analyst and Analytical Proceedings P. C. Weston Senior Assistant Editor Assistant Editors R. A. Young Mrs. J. Brew, Miss D. Chevin Publication of Analytical Proceedings is the responsi- bility of the Analytical Editorial Board: J. M. Ottaway (Chairman) J. M. Skinner L. S. Bark J. D. R. Thomas G. J. Dickes A. M. Ure 'G. W.Kirby 'P. C. Weston A. C. Moffat J. Whitehead T. 6. Pierce 'Ex officio members All editorial matter should be addressed to: The Editor, Analytical Proceedings, The Royal Society of Chemistry, Burlington House, Piccadilly, London, W1 V OBN. Telephone 01 -734 9864. Telex 268001. Advertisements: Advertising Department, The Royal Society of Chemistry, Burlington House, Piccadilly, Analytical Proceedings (ISSN 01 44-557X) is pub- lished monthly by The Royal Society of Chemistry, Burlington House, London W1 V OBN, England. All orders, accompanied by payment, should be sent to The Royal Society of Chemistry, The Distribution Centre, Blackhorse Road, Letchworth, Herts., SG6 1 HN, England. 1982 Annual Subscription price if purchased on its own: UK f40.00, Rest of World f42.00, US $95.00, including air speeded delivery.Air freight and mailing in the USA by Publications Expediting Inc., 200 Meacham Avenue, Elmont, N.Y. 11 003. USA Postmaster: Send address changes to : Analytical Proceedings, Publications Expediting Inc., 200 Meacham Avenue, Elmont, N.Y. 11 003. Second class postage paid at Jamaica, N.Y. 11431. All other despatches outside the UK by Bulk Airmail within Euro e, Accelerated Surface Post outside Europe. P R l d E D IN THE UK. Q The Royal Society of Chemistry 1982 London, W1 V OBN. Telephone 01 -734 9864. Obituary Ronald Belcher, BSc, PhD, DSc, Hon. DSc (Queen's Belfast, Saar- land), CChem, FRSC (1 909-82) The death of Ronald Belcher, Emeritus Pro- fessor of Analytical Chemistry in the University of Birmingham, on 29th June, 1982, brought to an end a career of outstanding achievement and internationally acknowledged brilliance.Born in Nottingham on 9th December, 1909, Ronald Belcher spent most of his formative years in Sheffield where the family had moved after the death of his mother. He received his education a t the Central Secondary School, later to become the High Storrs Grammar School, and matriculated in 1927. Although he had shown a distinct aptitude and liking for chemistry a t school, and indeed had gained a distinction in the subject on matriculation, it was no easy matter to find suitable employ- ment in the depressed economy of the late 1920s. However, after surviving a short spell with the well known firm of Mappin and Webb, he applied for and obtained a technical post in the Department of Fuel Technology a t the University .of Sheffield.Here began his lifelong interest in the chemistry of coal and coke, initiated and fostered by Professor R. V. Wheeler and his co-workers, one of whom was Ronald Holroyd, later to become Director of Research and Vice-chairman of ICI. As techni- cal research assistant to Professor Wheeler, Belcher was allowed a fairly free hand in the coal constitution laboratory, and he developed a special interest in the analysis of coal and coke. Most organic analysis was done by classi- cal macro-methods, but by 1937, Belcher had convinced his superiors that such methods were time-consuming and wasteful of material and he was sent to the Pregl Laboratory in the Medical Chemistry Institute of the University of Graz to acquire knowledge and experience of the techniques which had won for Pregl the Nobel Chemistry Prize in 1923.This was perhaps the most significant event in Belclier's scientific career for it inspired him, on his return to Sheffield, to devote most of his time and effort to the application of microchemistry to many of the challenging problems of fuel 455OBITUARY Anal. Proc. 456 analysis. Meanwhile he studied in his own time for the Associateship of the Institute of Chemistry which he obtained by examination in 1939, followed by the Felloyship in 1942. Ronald Belcher These years were a very productive period in Belcher’s career. In collaboration with A . E. Beet he developed a semi-micro method for the determination of nitrogen in coals.This was followed by a method for sulphur and halogen in coals and cokes which made use of the empty-tube principle. The method allowed rapid combustion of the sample in a fast stream of oxygen, the gaseous products being absorbed and subsequently titrated. The empty-tube method was further applied by Belcher and Spooner for the simultaneous determination of carbon, hydrogen, sulphur and chlorine in coals and cokes. These methods were so far ahead of any others that they were adopted first as British Standard methods and subsequently IS0 methods. Even 40 years after their intro- duction, they still are used, a fact which gave Belcher very great satisfaction in the later years of his life. During the early years of the 1940s, Belcher’s interests in microanalysis brought him into contact with C.L. Wilson. Together they resurrected the virtually defunct Microchemical Club and gave it new life as the Microchemistry Group of the old SPA. Thus began a long and fruitful association which was ended ,only by Cecil Wilson’s untimely death in 1974. To- gether they produced a book on qualitative inorganic microanalysis (1946) , which was subsequently enlarged (1957) to include quanti- tative methods. In 1955, there appeared “New Methods in Analytical Chemistry, ” a book inspired by an earlier volume by A. D. Mitchell and A. M. Ward. “New Methods” ran to a second and extensively revised edition in 1964. The award in 1941 of a Leverhulme Research Fellowship at Sheffield University to study the anodic oxidation of coal allowed Belcher to concentrate on personal research.This work was published in a series of papers in the Journal of the Society of Chemical Industry during 1948 and formed the basis for the degree of PhD which he was awarded in 1952 by the University of Birmingham (vide infra) . Meanwhile, the empty-tube principle con- tinued to interest him as a rapid micro-method of combustion of all organic compounds and work, first with C. E. Spooner and then with G. Tngram, led to the development of the method first for carbon and hydrogen (1950) and then sulphur and chlorine (1952). The introduction of granular manganese dioxide as external absorbent for nitrogen oxides allowed fast flows of oxygen through the specially constructed baffles in the combustion tube, very rapid com- bustion of the organic material and rapid absorption of the gases in the less restricted Flaschentrager absorption tubes-all a very great improvement over the classical Pregl micro-method with its packed tube of copper oxide, lead chromate and lead dioxide.This rapid combustion method was widely adopted in organic microanalytical laboratories for 20 years or more until the development of auto- matic C,H,N analysers supplanted these direct combustion methods for routine organic ele- mental analysis. On the expiry of his research fellowship, Belcher obtained a lectureship in chemistry at Rotherham Technical College in the heart of the steel-making industry. His attention was firmly fixed on the problems of teaching analytical chemistry and analytical techniques. The supervision of practical classes involving both qualitative and quanti- tative inorganic analysis required suitable laboratory exercises which students could per- form without undue difficulty or excessively complex equipment. With M.B. Thompson, he wrote his first book for student use, “An Introduction to Quantitative Analysis” (1946), a small but extremely useful laboratory manualOctober, 1982 OBITUARY 457 which formed the basis for a larger student manual, “Quantitative Inorganic Analysis, ” published in 1955, with A. J. Nutten as co- author. This book appeared in two completely revised subsequent editions (1960, 1970) and was unique in its collection of laboratory exercises, especially in gravimetry and titri- metry. Belcher’s great interest in redox indi- cators and redox processes in general led I.M. Kolthoff to approach him concerning the third part of “Volumetric Analysis” which was to deal with redox methods and had been only partially researched. Although this was to be a major undertaking, Belcher accepted the invitation to complete this important reference work, which was published in 1957. He took great pride in this co-authorship with Kolthoff and in the immense value of the text as the major source of information on redox titri- metry. But in the 1940s, fuel technology still held his main interest and the spell a t Rotherham was followed by a return to Sheffield and an appointment with the British Coke Research Association. At the conclusion of hostilities in Europe, British Intelligence Objective Surveys were organised in Germany to obtain informa- tion on all German scientific development during the war.With D. Phillips, Belcher was required to report on microchemistry. This led, among other things, to his first meeting with J. Unterzaucher at I.G. Farbenindustrie, Lever- kusen, and the realisation that the micro- determination of oxygen in organic compounds was done on a routine basis in Germany throughout the war. His first book (with A. L. Godbert) on organic analysis, “Semimicro Quantitative Organic Analysis, ” appeared at this time (1945), a second revised edition being produced in 1954. Towards the end of 1946, Belcher moved to Aberdeen. Professor H. W. Melville, then Head of the University’s Chemistry Department and no mean judge of men, had been perceptive enough to select the apparently less well quali- fied Belcher from a short list of suitably qualified academics for the teaching of inorganic and analytical chemistry.This, his first uni- versity appointment, provided him with the opportunity to supervise graduate students as well as to pursue his own research interests. His teaching duties were particularly onerous in those immediate post-war years with classes inflated by the considerable number of ex- servicemen rejoining their studies. Discipline in first-year classes was often difficult for the less experienced lecturers to maintain, but not so in Belcher’s lectures. He could stamp his authority on his audience at his first appearance, and his ability to lecture always without notes, and if necessary quoting complete literature references during his performance, kept his listeners spell-bound by this histrionic ability.His first research student at Aberdeen was A. J. Nutten, the Gold Medallist in Chemistry for 1948. Here began the work on benzidine chemistry which aimed at a relationship between molecular structure and analytically important behaviour such as sulphate solubility and redox reactions. The Aberdeen connection was, however, to be severed all too soon. Melville had departed to become Mason Pro- fessor of Chemistry in the University of Birmingham in succession to Sir Norman Haworth. Unsettled by the Melville exodus, Belcher was on the point of accepting an industrial appointment in which his wide experi- ence of fuel technology would be put to good use, when he was invited to Birmingham to continue the sort of teaching of analytical chemistry he had initiated at Aberdeen and to develop the work on organic elemental analysis which he had so ably pioneered in his Sheffield days with A.E. Beet and C. E. Spooner. A particular challenge was the analysis of a wide variety of fluorine-containing organic com- pounds which were then being synthesised in the Department after the secret war-time work on uranium hexafluoride had been transferred to AERE, Harwell. Thus, in September 1948, was the foundation laid for the Birmingham School of Analytical Chemistry, which for 29 years was to be directed by Ronald Belcher. Starting with only a personal research assistant, Ralph Goulden, work on the analysis of fluorine compounds began in earnest. In the Autumn of 1949, Nutten transferred from Aberdeen and with T.S. West (freshly graduated from Aberdeen), S. J. Clark and J . W. Robinson (Birmingham graduates) the nucleus of a research team was formed which was to develop into one of the largest and most productive units of its type in Europe. During these years, more than 150 graduate research students passed through the School and some 600 publi- cations showed the results of their endeavours. Assisting him with the supervision and research direction of these students were A. J. Nutten (1951-54), T. S. West (1952-61), W. I. Stephen (1955-77), A. M. G. Macdonald (1956-77), A. Townshend (1964-77), P. Zuman (1966-70), P. C. Uden (1966-70) and C. L. Graham (1970- 77). The researches have covered a very wide range of subjects.Over the years, considerable attention was given to organic reagents, used as precipitants, spectrophotometric reagents,458 OBITUARY Anal. Proc. redox and compleximetric indicators. Amongst these are 3,3’-dimethylnaphthidine, 4-amino- 4’-chlorobiphenyl and alizarin fluorine blue. Much general work was done on organic ele- mental microanalysis, especially fluorine-con- taining compounds, but most effort was directed towards the scaling down of micro-methods by a factor of 100, so that samples of only 30-50 pg were required. A long series of papers on these sub-micro methods appeared in the Journal of the Chemical Society over a 20-year period. Most of this work is described by Belcher himself in “Submicro Methods of Organic Analysis,” published in 1966.In more recent years, the work of Belcher’s school widened considerably to include work on volatile metal chelates which could be subjected to gas chromatography, polarography of organic compounds, membrane electrodes, kinetic methods and further studies of organic reagents. New methods of trace analysis were investigated and the techniques of candoluminescence and molecular emission cavity analysis (MECA) were developed for a variety of analytical applications, MECA being particularly well suited for the determination of sulphur, halogens and phosphorus. At the time of Belcher’s appointment a t Birmingham, the University statutes allowed higher degrees to be conferred only on indi- viduals possessing a first or Batchelor’s degree.Soon after his appointment, in 1950, Belcher as a Faculty member, applied for an official BSc by thesis, and submitted most of his coal and coke work. The two external examiners recommended it for the degree of PhD. This was to follow 2 years later (1952), now that he had obtained the necessary qualification. Then, in 1955, the minimum permissible time after the award of the PhD, he was awarded the degree of DSc. Promotion also came rapidly; he was made Senior Lecturer in 1951, Reader in 1954, and then Professor of Analytical Chemistry in 1959. He and his great friend and colleague, Cecil Wilson, who was appointed to a Chair a t Queen’s University, Belfast, in 1958 were, for several years, to be the only holders of Chairs in analytical chemistry in the UK, a situation very much regretted by Belcher and one which he did his utmost to remedy through publicity in lectures and articles. Regrettably, on his retiral in 1977, his Chair, which was a personal one, disappeared, despite his hope that an established Chair might have been created to replace it.He never forgave the Faculty for this dereliction of their duty and he died without ever again setting foot inside his old Department. During his sojourn in Aberdeen, Belcher had given his attention to the anomalous value for the solubility product of cadmium sulphide, which indicated that even in concentrated hydrochloric acid, CdS would be precipitated. This led to a wider appreciation of the limita- tions of most schemes of qualitative inorganic analysis and the deficiencies of most text-books on the subject.In an attempt to remedy this situation, a scheme of analysis was prepared by Belcher, Nutten and Stephen, and privately printed for use in the undergraduate classes at Birmingham. Although helpful, the new scheme brought more inadequacies to the fore and also the realisation that the problems needed a wider forum for discussion and study. Thus was born in 1954 the Midlands Association for Qualitative Analysis, the brain-child of Ron Belcher and always one of his most cherished interests. Over the years, MAQA has investi- gated and solved many problems of qualitative analysis and within the last 2 years it has achieved its major objective by the publication of definitive text-books on inorganic reaction chemistry-fitting tributes to Belcher’s stimu- lus, perseverance and scientific acumen.With the consolidation of the research school a t Birmingham, Belcher found time to partici- pate in many extra-mural activities. One of his chief interests lay in the Analytical Chemis- try Division of IUPAC, in which he served as a member of its various commissions, its divisional committee and as its President during 1957-61. A t the time of his death, he was National Representative on the Commission for Reagents and Reactions, thus having served IUPAC in one capacity or another for an unbroken period of 31 years. During these years he travelled widely on IUPAC business and fostered friend- ships with analytical chemists in many coun- tries. Following a series of lectures given a t Coventry in the summer of 1949, and a t the request of many industrial analysts in the Mid- lands, Belcher organised the Midlands Analytical Methods Discussion Group as a forum for the presentation of papers and discussion of analytical problems.In 1954, this body was re-named the Midlands Society for Analytical Chemistry, an independent organisation of analytical chemists. Meanwhile, the SPA had become the Society for Analytical Chemistry and, anxious to promote regional activities, it wooed and won over the Midlands Society, largely as a result of the efforts of D. W. Kent- Jones, then President of the SAC, who convinced Ronald Belcher of the many advantages to be gained by the merger. Thus, professional analytical activities in the Midlands were restored to the parent Society and, withOctober, 1982 OBITUARY 459 Belcher’s encouragement and support, the Midlands Region went from strength to strength.Belcher’s love for scientific jamborees was given full rein in Birmingham. Five international symposia have been held-in 1952, 1954, 1958, 1962 and 1969-the last one celebrating Belcher’s 60th birthday. In 1977, the Analyti- cal Division of the Chemical Society held SAC 77 a t Birmingham, one result of which was the nomination of Belcher as a candidate for the Presidency of the Division. After a ballot, he was duly elected President and served with much distinction during 1978-80. His successor in this office, Professor L. S. Bark, has given details of Belcher’s activities for the Analytical Division in The Analyst (October, 1982, 107, 1105).Throughout his career, Belcher’s publishing activities had been prodigious by any standards. Apart from his direct involvement with several hundred research papers and the numerous text-books already mentioned, he was a member of the advisory and editorial boards of many analytical journals. He was responsible for the introduction of the new journal Talanta in 1957 and maintained his position as Chairman of its Advisory Board up to the time of his death. First with L. Gordon and then with H. Freiser, he edited an important series of monographs on analytical chemistry, published by Pergamon Press. With D. M. W. Anderson, he edited a series dealing with organic functional group analysis for Academic Press. He was much in demand as a referee and always tried to be constructive and helpful to less experienced authors.The influence of Belcher’s research school has been far-reaching, profoundly affecting the development of analytical chemistry in many academic centres in the UK and abroad. Many postgraduate students from overseas have been attracted to Birmingham ; in particular, a succession of Spanish chemists have received their training in research with R. Belcher. In recognition of this, he was made an Honorary Councillor of the Spanish High Council for Scientific Research in 1972. Many former students and co-workers occupy Chairs of analytical chemistry in the UK and in several countries throughout the world. Belcher en- joyed keeping in touch with his many friends throughout the world, either by personal visit or by correspondence.He was an avid letter writer and was never without his personal tape machine into which he would dictate memo- randa to his staff and innumerable letters to friends and business associates. Throughout his long professional life he was much in demand as a lecturer, his individual style and clarity of presentation (always without notes) proving a fascinating and always educative experience for his audience. There can be few if any individuals who have, over a period of some 45 years, contributed more to the promotion and application of analytical chemistry than Ronald Belcher. Throughout his professional life he showed him- self to be a prodigious worker-his list of publications being a fitting testimony of his exceptional productivity.He worked cease- lessly for the proper recognition of analytical chemistry in British universities and by his example a t Birmingham, he gave great en- couragement to others. The creation of new centres in the UK owes much to his support of promising young chemists. Many honours, national and international, were bestowed on him. He was an Honorary Member of the Austrian Chemical Society, an Honorary Member and Medallist of the Japan Society for Analytical Chemistry, Lomonosov Medallist of the University of Moscow, Mende- leef Medallist of the Mendeleef Society of the USSR, Talanta Gold Medallist and recipient of an Honour issue of Talanta to celebrate his 60th birthday in 1969. He received also the Medal of Honour of the Bulgarian Academy of Science. He was awarded the degree of DSc (honoris causa) by Queen’s University, Belfast, and the University of Saarland, Saarbrucken. He was SAC Gold Medallist in 1969, and Theophilus Redwood Lecturer in 1976.He gave two Bicentennial lectures in the USA during the celebrations of that event in 1976. In this rapidly changing world, values are easily altered, but a sense of duty and purpose must remain secure and inviolate. Ronald Belcher had such singlemindedness in abun- dance. To some, he was perhaps a rather enigmatic person, but to his many friends his most endearing trait was the ability to make and keep friendships over long periods of time. His prodigious memory helped him enormously to keep the clear mental pictures so essential for their survival. Support for his friends and former students was always forthcoming when- ever it was requested.Ronald Belcher’s over-all contribution to the advancement of analytical chemistry cannot be simply categorised. It contains many facets, each of which reflects a distinctive area of endeavour. In times to come, historians of our science will debate his role in the progress of analytical chemistry. Those of us who have been privileged to work with him and observe him have little doubt about his magnitude as a460 YOUNG PHARMACISTS AWARD Anal. PYOC. scientist. Retirement] in September 1977, did not come easily to him. He found the break from a way of life which had started half a century ago to be almost unacceptable. He was given the title Emeritus Professor and became an Honorary Senior Research Fellow in the Department of Clinical Chemistry a t the University’s Medical School. He was also appointed to a similar position in the Chemistry Department of the University of Aston where he gave freely of his time to advise on research and to help with the teaching of analytical chemistry. Belcher’s leisure interests centred round his love of travel and history. He was an extremely well read historian and his punctiliousness in according correct precedence to the work of others in his own scientific writing lay deeply in his desire to ensure historical exactitude. He was intolerant of the lack of this in the writings of others, especially journalists, and he was quick to correct their errors. He loved good food and good wine and was an excellent judge of both. His wise counsel will be missed by many both in and outwith the profession of chemistry. Analytical chemistry in the UK has lost its greatest protagonist during five decades. His like shall never be seen again, for he was unique in every respect. W. I. STEPHEN

ISSN:0144-557X    

DOI:10.1039/AP9821900455

出版商:RSC    

年代:1982

数据来源: RSC

摘要:

460 YOUNG PHARMACISTS AWARD Anal. PYOC. Young Pharmacists Award R. P. Scherer are to present an award worth ,tIlOOO to pharmacists working in industry or graduates undertaking pre-registration experi- ence in industry who are under 30 years of age on July 22nd, 1983. The award will be pre- sented for a paper on any topic associated with the science or practice of pharmacy in industry. In addition, to mark the 50th anniversary of paper is specifically related to the use of the soft elastic gelatin capsule. Candidates must submit a title and an outline of the proposed paper by October 29th, 1982, and the full paper by July 22nd, 1983. For further information contact W. B. Rhodes, Assistant Secretary, The Pharmaceuti- cal Society of Great Britain, 1 Lambeth High the company, R.P. Scherer will increase the award to A1500 if the content of the winning Street, London, SEl 7JN. Reprint of an Important Analytical Chemistry Review In an attempt to ensure that major developments in chemistry reach as wide an audience as possible the RSC is to make available a reprint of an important review which was published in Chemical Society Reviews Vol 10, No 1, pp 11 3-1 58 entitled : Modern Analytical Methods for Environmental Polycyclic Aromatic Compounds by K. D. Bartle, M. L. Lee, and S. A. Wise Polycyclic aromatic compounds are major pollutants of the environment, originating from many sources. available for identification and analysis and provides the reader with a comprehensive and authoritative source of information on the subject. The paper is divided into the following sections: INTRODUCTION; SAMPLE PREPARATION; CHROMATOGRAPHIC METHODS; MASS SPECTROMETRY; SPECTROSCOPIC METHODS This review, which contains more than 400 references, will be of interest to environmental, petroleum and analytical chemists.f 2.50 ($5.00) by sending a stamped addressed envelope measuring 6" x 9" minimum, together with your remittance, to: This paper reviews the techniques that are A copy may be purchased for Dr. A. Kabi, The Royal Society of Chemistry, UKCIS, The University, NOTTINGHAM, NG7 2RD EnglandOctober, 1982 ANALYTICAL PROCEEDINGS 461 The Royal Society of Chemistry Specialist Periodical Reports Environmental Chemistry Vol. 2 Senior Reporter: H. J. M. Bowen The first volume of this series was published in 1975 and emphasized environmental organic chemistry whereas this second volume is deliber- ately slanted towards inorganic chemicals, covering the broad fields of the atmosphere and the hydrosphere, soils, and human diets.Reviewers of all these subjects agree that far too little information is available on the chemical forms of the elements in environmental reservoirs, thus laying down a challenge to analytical chemists. A broad review of mycotoxins is how- ever included partly to redress the balance of inorganic topics. Brief Contents : Inorganic Particulate Matter in the Atmos- phere : Methods of Sampling and Analysis; General Physical and Chemical Composition of Particu- lates; Characteristics of Emissions from Specific Sources; Atmospheric Transport and Dispersion of Particulates; Removal of Particulates from the Atmosphere; Effects of Airborne and Deposited Particulates; Future Research Needs and Con- clusions; The Elemental Content of Human Diets and Excreta : Outline of Ingestion, Absorption, Excretion; Methodological Problems, Inputs, Outputs, Deficient Concentrations, and Oral Toxicities of the Elements; The Elemental Constituents of Soils: The Alkali Metals: Lithium, Sodium, Potassium, Rubidium, and Caesium; The Alkaline Earth Elements : Beryllium, Magnesium, Calcium, Strontium and Barium; Titanium, Zirconium, and Hafnium; Vanadium, Niobium, and Tantalum; The Lanthanides or Rare Earth Elements, and Yttrium and Scandium; Molybdenum and Tungsten; Chromium, Manganese, Iron, Cobalt, and Nickel; Copper, Zinc, and Cadmium; The Noble Metals; Mercury; Boron, Aluminium, Gallium, Indium, and Thallium; Carbon, Silicon, Germanium, Tin, and Lead; Nitrogen, Phos- phorus, and Sulphur; Hydrogen and Oxygen; The Halogens: F, CI, Br, and I; Arsenic, Selenium, Antimony, and Bismuth; Thorium and Uranium; Radio n ucl id es, 0 rga n ic Soils; Mycotoxins : Biogenesis of Mycotoxins; The Importance of Mycotoxins in the Environment; Analysis of Mycotoxins; Occurrence in Food and Animal Feed; Metabolism and Mode of Action of Myco- toxins; Control of Mycotoxins in the Food Chain; Occurrence, Distribution, and Chemical Speciation of some Minor Dissolved Constituents in Ocean Waters : Individual Elements; Additional Aspects of Chemical Speciation; Hardcover 301 pp 0 85186 765 0 Price f 33.00 ($71 .OO) RSC Members f 19.00 Still available: Volume 1.Hardcover 212pp 0 85186 755 3 Price f15.50 ($33.00) RSC Members f7.50 Special Package Price (Vols 1 & 2) Non-RSC Members only f39.00 ($83.00) Miscelfane o us Publications The Periodic Table of the Elements The Royal Society of Chemistry has produced a colourful wall chart measuring 125cm x 75cm covering the first 105 elements as they exist today. Each group is pictured against the same tinted background and each element, where possible photographed in colour and discussed with regard to its position in the hierarchy of matter. Additional information for each element includes chemical symbol, atomic number, atomic weight and orbits of electrons. This chart is particularly useful for both teachers and students and would make a worthwhile addition to any establishment. Price f2.00 ($4.00) RSC Members fl .OO RSC members should send their orders to: The Royal Society of Chemistry, The Membership Officer, 30 Russell Square, London WC1 B 5DT. Non-RSC members should send their orders to: The Royal Society of Chemistry, Distribution Centre, Blackhorse Road, Letchworth. Herts SG6 1 HN. The Royal Society of Chemistry Burlington House London WlV OBN

ISSN:0144-557X    

DOI:10.1039/AP9821900460

出版商:RSC    

年代:1982

数据来源: RSC

摘要:

462 MICROCOMPUTERS AND MICROPROCESSORS Anal. Proc. ANNUAL CHEMICAL CONGRESS The Annual Chemical Congress of the Royal Society of Chemistry was held at the University of Aston in Birmingham on March 30th-April 2nd, 1982. A Symposium on Microcomputers and Microprocessors in Analytical Chemistry was organised by the Analytical Division. Microcomputers and Microprocessors in Analytical Chemistry The following are summaries of eight of the papers presented at the Annual Chemical Congress on March 30th-April lst, 1982. Microcomputers in the Research Laboratory E. B. James Computer Centre, Imperial College, London, S. W.7 Conventional computers have been used to support laboratory research for more than a genera- tion. Therefore, why should it be necessary to discuss the use of microcomputers in the labora- tory? Will not microcomputers be employed in essentially the same way as their larger brethren ? I believe that the use of microcomputing systems of the type we will specify will lead to a revolution in the way in which we organise laboratory-based research.So what is the essential difference between the big ones and the small ones? What quality is it that enables this revolution ? Many would believe that it is the new developments in microelectronics incorporated in the microcomputer that are significant. While the development of microelectronic techniques has made the microcomputer possible, I do not believe that the significant impact is at that level. Others may point to the epithet “micro” and suggest that it is the minute size of the micro- processors involved that is significant.In fact, many of the previous generation of mini- computers can fit very conveniently into a small laboratory, and so I do not think that the further decrease in size is especially important. The really important factor is, I believe, the relatively low cost of the microcomputer. This low cost makes possible the dedication of a powerful general purpose computer to requirements of a single researcher or a small research team, so that for the first time we can have a genuinely personal computing service. This situation has obtained for some time, but the full impact has hardly started to make itself felt. Let us explore what a personal computing service implies, and suggest why this quality of service can never be provided by a centralised computing system.Many larger laboratories have had their own minicomputers for some years, and a more limited number of laboratories have used them in on-line control of experiments. However, most computer use has involved the collection of data in the laboratory in a fairly labour- intensive way. Often, readings from various sensors have been transcribed by hand. These data have been collected together and processed in what we call the batch mode, as a single monolithic entity. Typically, statistical tests have been carried out on the batch, and the results have been presented in the form of printed numbers. When the researcher has obtained the results of this analysis it has often been found that certain control values in the experiment were not set suitably and, as a result, that most of the data collected was useless.The time scale for a repetition of the experiment with corrected control values may have been several days. This type of operation has often represented a terrible waste of computing resources. If the researcher had been able to see immediately the results from the first few seconds of the experiment, then it could have been suspended and re-started with correct controls. If we look harder at the data sent to the computer, even on a successful run, we will discover that most of them were not significant, and if a small amount of processing power had been available close to the experiment to filter out the unimportant readings, then possibly 90% or more of the data produced by the experiment need not have been processed further.Looking harder at the results themselves, we may find them represented typically as a large number of figuresOctober, 1982 MICROCOMPUTERS AND MICROPROCESSORS 463 arranged in columns. Perhaps some workers have had available a plotter, which could provide a graphical representation of the results, but in centralised system this may have added a day or more to the turn-round time. In any case, obtaining results in a convenient form has taken either a lot of time or further hand processing. First, the control values for the experiment can be set through the computer keyboard. These values can be checked for reasonableness as they are entered and the current settings of all controls can be continuously displayed on the screen.Any control value can be adjusted immediately it becomes obvious that it was set wrongly. As the experiment runs, we can display the readings from any number of sensors on the screen and close to each other. It is no longer necessary to keep our eyes on several different instruments at once. Any function of any number of the sensor values can be displayed in graphical form at essentially the same time as they occur. The control loop consisting of control setting, experiment run, evaluation of results, new control setting can be reduced in elapsed time from several days to several minutes. Many experienced researchers may feel that I have merely re-invented the familiar situation in a non-computerised laboratory. What specifically does the microcomputer add to the situation ? For instance, we can inspect im- mediately a heavily-processed version of the information available from the experiment sensors.If necessary, a great deal of non-significant data can be simply ignored. For example, we can ask to be displayed only readings above a certain value, or only those readings which are significantly different from some function of the previous readings. The researcher can be freed from the curse of too much data to process further. For example, we may require to optimise some function of the sensor outputs. The value of this function can then be dis- played continuously as a function of time and progress towards the optimum can clearly be seen. Naturally, since the input controls are applied through the machine, there is no reason why an optimising program should not be running at the same time and adjusting inputs to- wards some required objective, just as in the case of full-scale production plants. Secondary advantages of controlling the experiment inputs from a microcomputer include preventing an inexperienced worker from setting inappropriate values and the possibility of setting values much more precisely than can be achieved manually.The principles of writing such interactive experiment controllers are well established already as parts of programs used to control simulated experiments in computer-assisted learning. We require only to add the interfaces to the real experiment. Perhaps it is best always to practise the control of a simple simulation of the proposed experiment before we undertake the real thing. The second major advantage of employing a microcomputer is connected with the enor- mously increased potential for the employment of standardised software and hardware compon- ents.Previously, the program for the statistical processing of the results of the experiment would almost certainly have been constructed by a local specialist. The costs of such work relate to the “custom-built, one-off” approach and will have been very high, although possibly not obviously so, since they may have been disguised as “chemistry research.” If a commer- cially-available program has been used instead, then its cost will have been related to a compara- tively small “production run,” probably on the computer of one particular manufacturer only.The cost will also be connected with the original cost of the hardware, that is, with a mini- computer or larger machine. In each instance we are concerned with “Rolls-Royce” prices. When we move to a micromputer, we enter a different world. A well-designed statistical program written for a standard, widely available computer may be able to achieve sales of 50000 copies. The price is likely to be between El00 and l300, or a few days of the researcher’s time. I t is no longer relevant to consider the writing of such programs oneself. Before long, it will probably not be sensible for the researcher in chemistry to consider the writing of any program for laboratory control, except for very short sections which specify how a collection of standard programs will co-operate.In the same way, it is no longer necessary to design and build the interfacing equipment between the experiment and the microcomputer. Anything required can be quickly assembled from standardised control and sensing modules available “off the shelf,” which communicate with the micromputer in world-wide standard fashion. There should soon be available com- plete hardware - software packages, which include computer-assisted instruction modules to Now let us consider the scenario made possible by the microcomputer. But we can go much further. There are several important improvements available.464 MICROCOMPUTERS AND MICROPROCESSORS Anal. PYOG. train the researcher in putting together the equipment for a particular experiment. The costs for such standardised hardware and software will be related more to Woolworths than to Rolls-Ro yce.The approach outlined here may contrast very considerably with previous experience of using microcomputers in the laboratory. Often this has involved the specialised construction of hardware and software at a very detailed level by assistants with a very considerable expertise in microelectronics and programming. While this has been necessary in order to get things going, I do not believe that it is a sensible way forward for the majority of workers in chemistry. I would suggest that researchers in chemistry should get involved with the details of the com- puter and program as little as possible. Their main task will be to specify very precisely how the computing system should communicate with the user, and insist that their decisions are not over-ruled for the convenience of the program package providers.Now let us consider how we can start to become involved most effectively in microcomputer use. This is by going to a manufacturer of computer hardware and buying a particular piece of equipment without considering carefully the sort of experiments it will be used in, or the programs involved. The ideal starting situa- tion is to have the regular use of a computer which is provided for evaluation in a training laboratory. Associated with such a training laboratory I would expect to see training courses on the use of microcomputers. After a suitable course it should be possible to see much more clearly the likely impact of microcomputer use on your laboratory method, and the style of computing likely to be most suitable.Such a combination of training laboratory and training course is available, for example, at Imperial College in a joint operation between the Chemistry Department and the Computer Centre*. I would expect to see associated with the laboratory and course several experienced people with whom you could discuss particular requirements, and from whom you could receive assistance in the choice of hardware and software. I have provided elsewhere a paper which attempts to help those who do not have access to an experi- enced ana1yst.l I provide here some comments that highlight the various decisions which you may have to face. Many people believe that the cost of the microcomputer itself is the principal cost of any com- puting activity.Those with experience know that it may not even be a significant part of the cost. In a way, this is the impact of the microcomputer revolution. The cost of the people involved in the laboratory will usually be far greater than that of the equipment involved. I would caution against allowing young and enthusiastic researchers in chemistry to re- invent wheels in computing. Many laboratories are at present building from scratch hardware and programs that already exist and can be obtained at comparatively low cost. The usual argument put forward to enable this activity to continue is that “this laboratory has special requirements.” I would caution against the over-elaboration of experiments, in particular the use of compli- cated control theory which will lead to uncontrollable complexity in the control programs.The computer is probably best used for the routine and tedious data processing and the presen- tation of results in a suitable form. The researcher is best involved in making good control decisions, given the high quality of information available from the microcomputer. I would caution against any fresh attempt to centralise facilities and to put them in the charge of a computer manager in the name of efficiency. I would suggest that in any argu- ment put forward for centralisation you should substitute the word slide-rule, or typewriter, or tea-cup in place of “microcomputer.” Then, the speciousness of the argument will immedi- ately become obvious.The essence of the microcomputer revolution is that the computer becomes a personal tool, not subject to the constraints of a self-perpetuating bureaucracy. In order to continue to fight successfully against the centralisation of facilities it will be necessary to keep the microcomputer system simple. Systems which are so complex as to require more than one operator other than the researcher should be avoided. Another problem has arisen recently that is actually caused by the success of microelectron- ics. Manufacturers of laboratory measuring and control equipment are putting a micro- processor into every piece of equipment that they supply. This turns out to be a curse in disguise, because very few laboratory suppliers have the necessary experience of computer use to enable them to provide a sensible interface to a professional microcomputing system.All * For details of the course write to: Dr. N. J . Goddard, Chemistry Microcomputing Unit, Chemistry First, I would suggest how one should not start. This is usually an emotional need rather than a demonstrated fact. Department, Imperial College, London, S.W.7.October, 1982 MICROCOMPUTERS AND MICROPROCESSORS 465 the drawbacks of a too-low-level approach to computing are most effectively demonstrated. Often the manufacturer will have incorporated some software and hardware in the instrument through an outside consultant, and when this proves unsatisfactory in use, the only recourse of the purchaser will be to go to the original consultant and pay through the nose for a “one-off” modification.When purchasing equipment or programs it is best to suspect the integrity of every salesman and act accordingly. In particular, it will be necessary to insist on demonstrations of all equipment and programs working together rather than to depend on an assurance that device A cozdd be joined to device B. Man-years of effort can be wasted by accepting such statements. In the same vein, users are cautioned against doing research on untried computers on behalf of the manufacturer. This is best prevented by choosing equipment and programs in the main stream of development, which have already been tried and tested for some time. All of the problems implied by the last few paragraphs can be avoided by approaching a fellow chemist with experience in the practical application of microcomputers before you plan any activity of your own.So far we have considered the application of microcomputers to the control of laboratory experiments only. When you obtain a general purpose microcomputer for use in the labora- tory, you will soon discover that it can be applied in many other directions. It may well change your conception of what is meant by laboratory-based research. As an example, we may mention several ways in which the microcomputer can have an impact on the management of the laboratory. In the first place, a significant laboratory experiment would normally be expected to yield results which could be written up as a paper. It will be discovered that the general purpose microcomputer can undertake all the activities of word processing at a much lower cost than the specialised word processor.If this is not the case, then it is likely that you have purchased too specialised a microcomputing system. The researcher will find that with its aid, research papers can be composed, developed and edited up to publication standard by the most inexperi- enced of typists, and the production time compared with that obtained through conventional process of typing and retyping drafts can be cut surprisingly. Results in graphical form can easily be produced from the experimental data and inserted into the relevant positions in the paper. Ideally, the finished product from the microcomputer can be fed directly to an auto- matic typesetter. Equipment lists for a particular experiment can be checked against an existing inventory and the printout of orders for missing equipment can readily be arranged.More generally, the current value of all laboratory stocks can easily be maintained and the inventory can be very much at the user’s finger tips. This situation can hardly ever be achieved with a centralised computer system because of the processing delays involved and the batching together of inventory data inputs over several days in the name of processing efficiency. Finally, let us mention two new and exciting developments made practical by the micro- computer. Those who have seen a colour display demonstrating the progress of an experiment will have no doubts as to its superiority over the ordinary black and white presentation. The amount of information available from a well designed colour display is much greater than that for black and white.The second development concerns the input and output of information through the spoken word. It is now possible to monitor the output of any sensor and arrange that the current value is spoken as frequently as required. Once a researcher busy with a complicated appara- tus has experienced the advantages of hearing the parameter value spoken, rather than having to watch the output of a typewriter or a dial or screen display, there will be no question of the importance and value of speech. Rather further away in practical terms but advancing rapidly is the possibility of laboratory control through spoken input. Again, this is clearly much more convenient for the researcher than the use of keyboard input, especially for the inexperienced typists amongst us.Let us hope that with the aid of microcomputers in the laboratory we may be able to improve our experimental technique so that the last word from our computing system will not be “You are interfering incompetently with the progress of this experiment. I have stopped sensing your inputs and will now take over myself.” A second example of subsidiary use is in laboratory stock control. The first concerns the presentation of results in colour.466 MICROCOMPUTERS AND MICROPROCESSORS Anal. PYOC. Reference 1. James, E. B., “Personal Computing Systems for Research and Development,” Computer Centre, Imperial College of Science and Technology, London, 1981.Interfacing and Communication Networks J. V. Simons Laboratory Apparatus Section, Research Department, Imperial Chemical Industries PLC, Petrochemicals and Plastics Division, P.O. Box 6, Welwyn Garden City, Hertfordshire, AL7 1HD Microcomputers are dropping in price and as this happens more of them will be applied in areas of laboratory control, measurement and data analysis. This is a trend which will accelerate as cheaper, more powerful devices appear on the market. Many of the instruments that are produced today already have a microprocessor built in. The ability to link the computers is important as it helps to minimise total costs, enables data to be transmitted easily from one location to another, and perhaps most important of all, it is possible for an organisation to ensure that important data generated at several different locations are stored, backed up and generally looked after by a professional group, which will be used to ensuring that important information is not lost, Within the computer industry the use of networks grew up for two reasons.Firstly, to make better use of computer equipment, especially expensive peripherals such as disk and tape drives, printers and plotters. As the price of computer hardware continues to drop the first reason assumes less import- ance, while the second becomes more important, especially as the results of sophisticated measurements such as nuclear magnetic resonance and mass spectroscopy will increasingly be used to control processes. Secondly, to share software/data with other users.Types of Computer Interconnection The simplest example is the connection of two machines. It is important that standards are adopted from the outset. These standards enable transmission errors due to malfunction of equipment or electrical noise interference to be reduced to a minimum. This use will require problems of correct data sequencing and synchronisation of the transmitter and receiver to be solved. The solution consists of a data communicating link protocol that assures the correct sequencing and integrity between systems. To allow communications between computers a uniform method of exchanging information is needed. This requires the establishment of a character code structure for interpretation of bits as characters, a message syntax to form characters into messages and data communic- tions control procedures for exchanging the messages.A typical code, and the most popular, is ASCII (American Standard Code for Information Interchange). Connection of equipment to the public telephone network has to be carefully approached. Even though a computer/instrument is connected to the network through an approved Modem it should have been approved by British Telecom; most machines that are sold today have no such approval. In real life it is usual for several machines to be connected to a central machine in a star configuration. If care is not exercised it will be possible to crash the whole system. The main problem of the star connection is that if the computer at the centre breaks down the whole system stops.It is possible, especially over a limited distance, to connect computers together using a bus configuration. A typical bus standard that we have adopted in connecting six computers together is the IEEE 488. Five of the computers are attached to mechanical testing instru- ments, such as tensile testing machines, drop-weight testers or impact machines. The sixth machine runs a data base management package. The computers are all Hewlett-Packard, two HP 9826, two HP 85, one HP 9825 and one HP 9845. The data-base package from Hewlett- Packard “Image and Query” runs on the HP 9845. The other machines collect and analyse the data from the various tests and the results are passed on to the data-base computer. The So far the problems of connecting two machines have been examined.October, 1982 MICROCOMPUTERS AND MICROPROCESSORS 467 problem of such a system is that the bus is limited to 20 m total length, unless expensive fibre optic repeaters are used.Local Area Networks (LAN) LAN’s are designed to provide a high speed, low error rate communication path between computers and other devices that are connected to the system. The data are carried on a cable (coaxial/twisted pair/fibre optic/multicore) over a limited distance, usually a few kilometres. Transmission rates on the system should be at least 10 megabits per second. Cambridge Ring Fig. 1 is a typical datagram for a Cambridge Ring system. Each device connected to the ring, when it wishes to transmit a datagram, looks at slots that are circulating in the ring, and when the next available empty slot appears it places its datagram into it.The transmitted datagram is then moved to each of the stations on the ring, which then read the destination address. If a station recognises its address it sets control bits in the check part of the datagram to signify accepted, busy or rejected. The datagram then returns to the source where it is checked to see if it was accepted at the destination address; if so the slot is then marked empty, if not the datagram is again sent to its destination. To prevent the ring becoming clogged with datagrams that cannot be accepted by their destination stations, the source is only allowed to place the same datagram on the ring for two consecutive cycles; it then has to be removed for a period of time.LAN’s can be viewed as a system for transporting datagrams. r I I 1 1 I I I I I I I I I I I I I Destination I Source I I I I I I I I address I address I Length I Data I Check I Fig. 1. Typical datagram for a Cambridge Ring system, Ethernet It was first designed and implemented by the Xerox Corporation in 1975. In September 1980 three companies, Digital Equipment Corporation, Intel Corporation and Xerox Corporation published a document entitled “The Ethernet a Local Area Network,” which gives details of the Ethernet specification. Ethernet has the following characteristics: (i) data rate: 10 million bits per second; (ii) maximum station separation: 2.5 km; (iii) maximum number of stations: 1024; and (iv) medium : shielded coaxial cable. Ethernet can be divided into three layers as shown in Fig.2, which are defined as follows. (a) Client layer : collective term used to describe any layer of a network architecture, which This is a different system as it is in effect a bus. uses the Ethernet data link and the client interface. I I I Client layer I : Interface- I I Data link layer Interface - I i I Physical layer I , Fig. 2. Ethernet layers.468 MICROCOMPUTERS AND MICROPROCESSORS Anal. Proc. (b) Data link layer: the higher of the two layers in the Ethernet design, which implements a medium independent link level communication facility on top of the physical channel provided by the physical layer. (c) Physical layer: the lower of the two layers of the Ethernet design, implemented by the physical channel using the specified coaxial cable medium.The physical layer insulates the data link layer from the medium dependent physical characteristics. When the client layer requests the transmission of a datagram, a data encapsulation module constructs the datagram from the client supplied data and the datagram is then handed to the transmit link management component for transmission. Transmit link management attempts to avoid contention with other traffic on the channel by monitoring the carrier sense signal and deferring to passing traffic. When the channel is clear, datagram transmission takes place and is effectively transmitted to all stations on the system. On arrival at each station, the station data encapsulation module checks the datagram’s destination address field to decide whether the datagram should be received by the station.If so, it passes the contents of the datagram to the client layer, where it is checked to ensure that an error-free transmission has taken place. If multiple stations attempt to transmit at the same time there is a mechanism wbich detects the problem and allows re-transmission to take place when the system is clear. There are many suppliers of LANs, such as Netlone from Ungennann-Bass, Santa Clara, CA, 2-Net from Zilog Cupertino, CA, XINET from Xionics, London, as well as a host of simplified systems for microcomputers, such as Nestar Clustar for the Apple computer from Zynar Limited, Uxbridge, Middlesex. In the US an IEEE committee is working on a standard which will be similar to Ethernet and will be known as IEEE 802.Conclusion The benefits that might be achieved with the use of a high speed data network can be set 1. Direct computer storage of experimental results. 2. Availability of powerful, easy to use computer packages at every desk in a department, e.g., statistics, library searches, data-base storage and manipulation and access to external data bases. 3. Reduction in the amount of paper handled. 4. Message transmission and storage facilities. 5. Immediate recall and manipulation of historical data. 6. Ability to manipulate, cross reference and correlate the work of many people who are working on the same subject. 7. Reduction of secretarial effort due to direct entry of experimental results. out as below. Software for Microcomputers and Microprocessors D.C. Bateman Computing Laboratory, University of Kent at Canterbury, Canterbury, Kent, CT2 7NZ Microcomputers offer a limited choice of software compared with mainframe and minicomputer systems. This paper summarises the capabilities, advantages and disadvantages of some of the system software currently available on 8-bit single-user microcomputers. Operating Systems All disk-based microcomputer systems have at least a rudimentary operating system. User requirements from an operating system vary, but may include a choice of programming languages, an editor, linker and debugger and utilities for making use of hardware resources, such as sending listings to a printer and making copies of disk files. CP/M Operating system It is written in 8080 assembler to run on any SO80/8085/ZSO processor with at least 20K bytes of CP/M has become the de facto standard operating system on 8-bit microcomputers.October, 1982 MICROCOMPUTERS AND MICROPROCESSORS 469 RAM.In practice, to run BASIC one requires at least 32K bytes, and to run other high-level languages, such as PASCAL or FORTRAN, at least 48K is needed and 64K is usually recom- mended. CP/M is divided into two parts: a small resident part of about 8K bytes, which is in memory all the time, and a transient part consisting of a number of separate programs that are stored as executable files on a system disk and which can be loaded into memory one at a time as required. The resident part of CP/M contains the code for interpreting and executing a number of user commands, control characters and basic input/output routines.The transient programs supplied may vary, but normally include editor, assembler and standard CP/M utility programs such as DUMP, DDT, LOAD, PIP and STAT. One of the advantages of CP/M is its flexibility; it can be easily tailored to a non-standard environment incorporating, for example, laboratory devices by adding new 1/0 routines to the CP/M BIOS sub-system. Enhancements to CP/M V2.2 include a facility to protect disk files against accidental deletion and the capability of supporting hard-disks. UCSD PASCAL Operating System The UCSD PASCAL operating system (hereafter abbreviated to UCSD) is more sophisticated than CP/M. As its name implies, it is written almost entirely in PASCAL, and is available on a number of different processors including the 8080/8085/280, 6502, 6809, 9900 and LSI-11.Whilst UCSD provides more facilities and is more portable than CP/M, it requires at least 48K of RAM and greater disk capacity to store the transient programs. Programming Languages High-level Languages UCSD supports compilers for extended versions of BASIC and PASCAL and a sub-set of FORTRAN-77. Programs written in these langugages are compiled to the same intermediate code called p-code, which is interpreted by a small run-time interpreter. CP/M supports several PASCAL compilers. PASCAL/Z and PASCAL/MT+ compile to assembly language and native machine code, respectively, wlule PASCAL/M compiles to p-code. Programs produced by a native code compiler will normally execute faster than a p-code interpreted program, and although p-code is the more compact object code, the run-time interpreter has to be in RAM as well when the program is running.FORTRAN programs can also be compiled under CP/M by Microsoft’s FORTRAN-80 compiler. In spite of its name, FORTRAN-80 is based on the older ANSI FORT RAN-^^ standard, and not on the FORT RAN-^^ standard. Although both native code and pseudo-code BASIC compilers exist which run under CP/M, BASIC programs are usually interpreted on microcomputers. Most interpreted programs run slowly compared with compiled programs, and the interpreter itself occupies between about 8K and 16K bytes of RAM. However, most BASIC interpreters provide a particularly “user- friendly” environment, with a built-in screen editor and interactive debugging facilities.Language Extension In their standard form, both BASIC and PASCAL are inadequate for writing applications programs. Although most microcomputer implementations of high-level languages contain extensions, they have not been provided in a uniform way. The result is that although the extensions are necessary, their use reduces a program’s portability on to other systems. Most versions of BASIC, PASCAL and FORTRAN support a number of enhancements that are essentia€ for laboratory applications, for example : access to 1/0 ports; logical operators/bit- wise manipulation ; and linkage to assembly language and/or pre-compiled routines. Some BASICS and PASCALS also support a range of graphics functions, including high-resolution graphics. While most BASICS support dynamic arrays, and the PASCALS generally do not, PASCAL is superior to BASIC in many other respects.PASCAL has better control statements, allows long variable names, and is a strongly procedure-oriented language. BASIC is most suitable for writing short programs, whereas PASCAL is a superior language suitable for writing efficient, reliable, well structured programs, that can be maintained easily. Programmers developing large applications programs in PASCAL face several problems that can become acute on microcomputers. Most of the currently available 8-bit systems have470 MICROCOMPUTERS AND MICROPROCESSORS Anal. Proc. little room in which to compile large programs. Procedures and functions can usually be compiled into a library of routines which can be linked together at run-time as required. An additional advantage of this facility is that one can build up a library of commonly used rout- ines.Most PASCALS also support program segmentation and memory overlays. An important consideration in the selection of a particular compiler or interpreter may be whether it uses a binary representation or BCD representation for storing numbers. On %bit machines, real numbers are usually stored in binary to about 7 decimal digits of accuracy, over the range 10-38-1038. A BCD representation usually gives more digits over a larger range, and although BCD arithmetic is much slower, it introduces fewer round-off errors. The FORTRANS, of course, have double-precision reals, and some of the PASCALS offer an extended precision for reals as well as long integers.Assembly Languages The facilities that allow high-level languages to communicate with devices has reduced the total dependence on assembly languages for many aspects of laboratory control. ASSEMBLER code may still be required, however, for such tasks as making a $critical section of program execute faster, achieving precise timing, or running under interrupt control. Current and Future Software Developments Major software development is now taking place on the new 16-bit microcomputers, which promise greater execution speeds and more memory capacity. Both CP/M and UCSD are competing in this market, where they are in competition with numerous versions of the more advanced UNIX operating system. These developments will, in turn, lead to the availability and use of more sophisticated programming languages such as C and ADA.Using a Microcomputer in an IR Laboratory M. J. Adams and 1. Black The Macaulay Institute for Soil Research, Craigiebuckler, A bevdeen, A B9 2Q J , Scotland The increasing availability and awareness of the “home” or personal microcomputer is now appreciated by analytical instrument manufacturers and laboratory staff. Offering powerful computing facilities for moderate cost, a major advantage of the microcomputer is its ease of use in a conversational mode rather than the batch processing mode associated with more conventional mainframe units. Modern microcomputers contain a microprocessor, input - output facilities, a memory for program and data storage and, commonly, one high-level programming language, usually BASIC, enabling many useful programs to be developed by the user without recourse to outside specialist assistance.The major uses for a computer in an analytical laboratory can be summarised as follows: instrument control, requiring a bidirectional link between the computer and the instrument ; data logging, often with a single, undirectional link from instrument to computer; arith- metical operations ; data formatting, with selective output procedures; and data storage. Instrument control and data logging can be more easily achieved with the microcomputer than with larger and more complex mainframe computers, although the latter usually have more extensive data storage facilities and their data management functions are superior.The use of a microcomputer for even a moderately complex laboratory application can require a detailed appreciation of the internal architecture of the computer and its use of available memory. In the Department of Spectrochemistry at the Macaulay Institute an Apple I1 microcomputer is employed as an aid in the acquisition and analysis of inorganic, mineral, infrared spectra. The advantages of this machine for laboratory use include its high-resolution graphics capability (now becoming common on all microcomputers) , the ease of access to its input - output ports for expansion and interfacing and the availability of high- quality interfacing hardware. Although this is a relatively slow-running language, the ease with which machine-coded routines can be BASIC is the standard language for this computer,October, 1982 MICROCOMPUTERS AND MICROPROCESSORS 47 1 incorporated within the program for speed-dependent operations helps to overcome any timing problems that may be experienced. Part of the infrared instrumentation and computer system is illustrated schematically in Fig.1. The computer, with twin floppy-disk units and video monitor, is linked to a Perkin- Elmer 580B spectrometer and an Eclipse (Data General) mainframe computer via a single RS232C interface card. Selection of the spectrometer or Eclipse computer is achieved with a manual switch. As well as transferring spectral data from the microcomputer to the main- frame system for library storage, the Apple computer can be used as a dumb terminal for access to the Eclipse facilities.To reduce problems of data transmission associated with the distance (approximately 100 m) between the computers, a pair of line-drivers are employed in the communications link. The 580B spectrometer contains its own intelligent RS232C interface, with a comprehensive catalogue of commands for controlling the instrument and logging and re-plotting data via a remote ASCII keyboard. The input of spectral data to the microcomputer is achieved directly from the spectrometer during wavelength scanning. Because of the explicit format of the data transmitted to and from the spectrometer, all communications between it and the computer, as well as all data-formatting operations, are handled by machine-coded routines. Spectral data can also be entered into the computer via a digitising tablet.This provides computer storage and access to many thousands of pre-recorded spectra obtained on various spectrometers. All digitised spectra are automatically scaled, in terms of wavenumber resolution, to a similar format for compatability in storage and manipulation. Disks r 1 Computer - Tablet t Printer Monitor * L Fig. 1. The microcomputer and data transfer lines in the infra- red laboratory. ROM DOS M. CODE Data Graphics Program Int. use Fig. 2. A memory map for the Apple I1 computer illustrating the memory usage for a typical infrared applications program. Much of the 64 K of memory is used by ROM, the Disk Operating System (DOS), high resolution graphics display and internal use. The available memory space (shown unshaded) for program, data and machine code storage needs to be carefully man- aged. The suite of programs for use in the infrared laboratory runs as a turn-key system, requiring no prior knowledge of computing by the operator.The major arithmetical program used is concerned with the manipulation of spectral data. Up to three spectra can be retained in the computer memory simultaneously, and such a complex data-handling program requires extens- ive use of the computer memory map in the development of programs. A typical memory map for the spectral manipulation program is illustrated in Fig. 2. Although this is a single program, for convenience it can be considered in two parts, file management and active472 MICROCOMPUTERS AND MICROPROCESSORS Anal.Proc. manipulation. File management commands do not modify the spectral data but allow spectra to be retrieved from or passed to disk storage. The data can also be transferred within the microcomputer system and viewed, between specified wavenumber limits, on the video monitor. Active manipulation routines modify data and include procedures for absorbance - transmission conversion, adding off set, flattening a base line, curve smoothing, summing spectra and determining the difference spectrum from two samples. Output and re-plotting of data can be achieved on the 580B spectrometer or a flatbed plotter unit. All plotting is under microcomputer control and uses the video monitor to format, scale and locate the relative positions of multiple spectra before producing the final hard copy of the data. Further details of the programs employed can be obtained from the authors. Optimisation of High-performance Liquid Chromatographic Separations with the Aid of a Microcomputer J.C. Berridge Analytical Chemistry Depavtment, Pfzer Central Research, Sandwich, Kent When faced with the task of developing a new high-performance liquid chromatographic (HPLC) separation the chromatographer uses a mixture of experience, theory and guesswork to select the column type and length and the principal components of the mobile phase. The separation is then optimised by adjusting the mobile phase composition until the desired selectivity, analysis time or other suitable criteria are met. Until recently this latter process tended to be carried out in a rather arbitrary manner but current literature suggests this situa- tion to be changing ra~idly.l-~ The advent of microcomputer controlled HPLC, with its associated computational power, means that it is now possible to optimise HPLC separations in a systematic manner without the need for intervention by the chromatographer.There are a number of schemes available to assist in the optimisation of reversed-phase separations with hydrocarbon bonded phases. These are based on theoretical or semi-empirical models1,6 or use sequential or statistical search techniques. 9 9 59 The Simplex Procedure The simplex algorithms is an efficient, multi-dimensional, sequential search technique that has been applied to a variety of analytical problem^.^^*^^ The algorithm directs the adjust- ment of experimental conditions away from those which give a poor result, or response, towards conditions which give a more favourable response.The detailed operation of the simplex procedure has been described by other workers.8 The current work used the variable simplex size procedure of Nelder and Mead.lo Before using the simplex procedure in HPLC it is necessary to have a means of quantita- tively assessing the quality of a chromatogram. The concept of a chromatographic response function (CRF)7 provides a numerical description of the quality of a separation which may be used as the response for the simplex procedure. In this work the form of the CRF used was: where R is the resolution between adjacent peak pairs and L the number of peaks detected, TA is a specified analysis time, T , is the retention time of the last eluted peak, T , the retention time of the first eluted peak and To a specified minimum elution time; all time units are expressed in minutes.The parameters may be manually determined for each chromatogram but this makes the application of the simplex procedure time consuming and laborious. These limitations are removed with the use of a computer-controlled chromatograph.October, 1982 MICROCOMPUTERS AND MICROPROCESSORS 473 Start v I I Input boundary conditions for first parameters Initiate autosampler Flush column Hold autosampler - I I Compute CRF I CRF= - 50 First procedure CRF= - 100 violation Still I Yes \ Experiments --+ Print report -+ Fig. 1. Flow chart of program TERNOPT.474 MICROCOMPUTERS AND MICROPROCESSORS Anal.Proc. Materials and Methods All separations were carried out using an Analyst 7800 liquid chromatograph with a Chrom- atography Control Module (Laboratory Data Control, Stone, Staffordshire). Where mobile phases containing three solvents were used a third pump (Constametric I1 G) was added to the system. Columns were all 10 x 0.5 cm i.d. (Shandon Southern, Runcorn, Cheshire) and were packed with 5 pm LiChrosorb RP-18, Hypersil ODS or Partisil ODs-3. Methanol and acetonitrile were HPLC grade (Rathburn Chemicals, Walkerburn, Scotland) ; water was freshly glass distilled. Solutes were laboratory-reagent grade and used as received. Results The unattended optimisations were carried out using three BASIC programs, each requiring approximately 16K of memory.The program titles and function are : ISOOPT, binary mobile phase composition and flow-rate ; GRADOPT, gradient elution profile ; and TERNOPT, ternary mobile phase composition. Each program interacts with the chromatographic files as provided by the instrument manufacturer for instrument control and integration results. The integration output of peak retention times, heights and areas is used to calculate resolutions, and hence the CRF, and then the files are modified to set up new chromatographic conditions. Fig. 1 is a simplified flow chart of the program TERNOPT: the number of experiments is limited to 30 because of restrictions on dynamic memory. For the vast majority of separa- tions an optimum has been located before this limit is reached.Figs. 2, 3 and 4 show examples of optimised separations carried out using the programs ISOOPT, GRADOPT and TERNOPT, respectively. Fig. 5 shows the movements of the simplexes produced during the optimisation process, which gave the separation shown in Fig. 4: converg- ence on the optimum is rapid and direct. 0 5 10 Time min Fig. 2. Optimised isocratic separation of 2- substituted pyridines using ISOOPT with a 10-min time target. Column, Hypersil ODS ; eluent, aceto- nitrile - water - ammonia (16 + 84 + 0.1) ; flow- rate 1.4 ml min-1; 24 experiments conducted. Peak identities : 1, 2-aminopyridine; 2, 2-formamido-3- methylpyridine ; 3, 2-amino-5-methylpyridine ; and 4, 2-ethylpyridine. 0 1 2 3 Time ,m i n Fig. 3. Optimised gradient separation of anti- oxidants using GRADOPT with a 4.0-min time target.Column, LiChrosorb RP-18; flow-rate, 2.0 ml min-l; eluent, solvent A, acetonitrile - water (95 + 5 ) and solvent B, acetonitrile - water (5 + 95); linear gradient A - B (56 + 44) to 100% B in 1.5 min. Peak identities: 1, propyl gallate; 2, BHA; 3, un- known; and 4, BHT. Conclusion The availability of microcomputers within the laboratory brings a wide range of mathe- matical schemes within the reach of every chromatographer. By incorporating the simplex algorithm into programs written for a microcomputer controlled liquid chromatograph it becomes possible to carry out the completely unattended optimisation of HPLC separations. Although only reversed-phase separations have been considered to date there are no reasons why similar procedures could not be applied to normal-phase chromatography.October, 1982 MICROCOMPUTERS AND MICROPROCESSORS 475 0 2 4 Time min Fig. 4.Optimised separation using TERNOPT with a time target of 4 min. Column, Partisil ODS-3 ; eluent, acetonitrile - methanol - water - ammonia (10 + 5 + 85 + 0.1) ; flow-rate, 2.0 ml min-l; 20 ex- periments conducted. Peak identi- ties : 1, 2-methyl-5-nitroimidazole ; 2, 5-(hydroxymethy1)furfural; 3, 1- (2-h ydroxyethyl) -2-methyl-&nitro- imidazole (metronidazole, May and Baker) ; 4, 1-[2-(ethylsulphony1)- ethyl]-2-methyl-5-nitroimidazole (tinidazole, Pfizer) . 80 c 100 A 20 40 60 Water concentration, o/o Fig. 5. Movements of simplexes during optimisation with TERNOPT. ABC is the initial simplex.The simplex size con- tracts until the optimisation is terminated with simplex CDE, which contains the optimum mobile phase composition. The use of a sequential search technique, such as the simplex procedure, does not rely upon ideal or predictable behaviour of the solutes under study. The examples presented show that optima cafl be reliably located with the minimum expenditure of the chromatographer’s time and effort. Whilst a located optimum may prove not to provide the over-all best possible separation, it is a simple matter to repeat the procedure by re-starting the simplex in a different region of the experimental variables. Such multiple runs bring the goal of true automated HPLC method development one step closer. 1. 2. 3. 4. 6. 6. 7. 8.9. 10. References Gant, J . R., Dolan, J. W., and Snyder, L. R., J. Chromatogr., 1979, 185, 153. Glajch, J . L., Kirkland, J . J., Squire, K. M., and Minor, J. M., J. Chromatogr., 1980, 190, 67. Berry, V. V., J. Chromatogr., 1980, 199. 219. Toon, S., and Rowland, M., J. Chromatogr., 1981, 208, 391. Lindberg, W., Johansson, E., and Johansson, K., J. Chromatogr., 1981, 211, 201. Bemdge, J. C., J. Chromatogr., 1980, 202, 469. Watson, M. W., and Carr, P. W., Anal. Chem., 1979, 51, 1835. Deming, S. N., and Morgan, S. L., Anal. Chem., 1973, 45, 278A. Berridge, J. C., J. Chromatogr., 1982, 244, 1. Nelder, J. A., and Mead, R., Comput. J., 1965, 7 , 380. Microcomputers, Industry and Education A. Braithwaite Department of Physical Sciences, Trent Polytechlaic, Clifton Lane, Nottingham, NG11 8NS Work in analytical chemistry laboratories, in common with all other areas of industry where repetitive work is carried out and large amounts of information are generated, is rapidly changing owing to the technological revolution.One result of the arrival of microcomputers and microprocessors on the bench is that new techniques and a new language have to be learnt. Re-training or “in service education” is frequently required; however, this often amounts to the enthusiasm of a few individuals, particularly the younger analysts. A parallel problem476 MICROCOMPUTERS AND MICROPROCESSORS Anal. PYOC. is to identify areas of application and potential uses of microcomputers in order to improve the over-all performance of the laboratory. Educational institutions, especially those with part-time students, review their courses periodically to meet the ever changing needs of indus- try whilst still covering the essential basic chemistry.Ths paper is in two parts, the educa- tional curriculum aspects followed by examples of practical exercises, which illustrate the capabilities of microcomputers. Educational Aspects The over-all aim of a course is to generate chemical common sense and at the same time to develop a marketable expertise. Such a course is a careful balance of basic and applied studies to develop a basic knowledge of chemistry, learning skills, laboratory skills, expressive skills including report writing, verbal communication and initiative and personality. Analy- tical chemistry is perhaps the most developing branch of chemistry as it moves into a new technological era.Analytical chemistry courses therefore need to be modified to enable students to understand the new instrumentation, data processing and modified techniques. The development of knowledge and learning skills starts at school. However, “0” and “A” level syllabuses have expanded to include more and more material and are often drawn up by specialists who seem to lack foresight. In many instances pupils are becoming learning machines instead of developing the correct skills and learning how to use and expand on the knowledge presented to them. Unfortunately, the habit of this learning pattern is carried on into further education and work, resulting in a lack of initiative and an inability to work up or develop a method or task presented to them.A further problem generated at school and/or by society is a fear ‘of anything mathematical, including chemistry and physics; the image presented of these sciences appears too abstract. A more applied approach relevant to today’s technologies would help to dispel the “difficult” images that these subjects have gained. Although new courses such as SMP mathematics and Nuffield sciences were thought to be a breakthrough they only seem to have compounded the problem. A good working knowledge of the relevant mathematics is essential for chemistry and physics students and although the new mathematics does include topics such as matrices, sets, transformations, number patterns and number bases, which help with computing and data processing, there are some omissions.There is surely a need for an “A” level mathematics for science and technology. It is important to look at the whole of the educational system as an integrated set of courses that can achieve the aims outlined above. All too often syllabuses are designed by specialists without enough consideration of the applied aspects of the subject and support for other areas, such as the sciences. Post “A” level courses fall into two areas, part-time courses leading to HTC (Higher Techni- cians Certificate) and an honours degree by part-time study, and secondly, a full-time degree with or without industrial training. Analytical chemistry is now taught in many of these courses as an integrated module or as an option. In addition to the more familiar aspects of analytical chemistry, e.g., spectroscopy, chromatography, electrochemistry, sampling and data evaluation, it is essential to include such topics as the physics of analytical instrumenta- tion to develop an understanding of the principles and mechanics of instruments, the variables associated with a technique, the nature of detector/output signals (what they are and what they represent) and the presentation of the information or results.Also, microcomputers have radically affected two aspects of instrumentation : firstly, the control of the instrument parameters and variables and, secondly, collection and processing of data. Thus, an analytical chemistry course really needs to include introductions to computing, microprocessors and their use with analytical instruments, data processing and microcom- puter applications so that students have sufficient knowledge to apply these skills as required in their future work.A computing core should aim to teach the basic programming skills based initially on the BASIC programming language but also including an introduction to PASCAL and FORTRAN. It should also include the role of mainframe computers and the integrated systems now being used in large companies, chemical plants and polytechnics and universities, covering features such as company networks linking many computers, local area networks for laboratories or chemical plants, word processing and office mailing and the use of data bases. The introduction to microcomputers should aim to put the subject into per- spective with respect to laboratory instrumentation as outlined above. Although the micro-October, 1982 MICROCOMPUTERS AND MICROPROCESSORS 477 computers used are complete functional units an introduction to the hardware and software of microcomputer systems is appropriate and provides a working knowledge of the functional building blocks and an understanding of computer jargon. The programming and use of interfaces that extend the basic microcomputer into a controller, data collection system, mainframe terminal or port on a network need to be covered to illustrate the full capabilities of microcomputers and also to illustrate future possibilities.The use of the computing power available in analytical chemistry may be covered in a data processing course which covers such topics as computing techniques for data systems, evaluation of data, number presentation, number patterns, number crunching, extrapolating data, calculation and construction of graphs and bar charts, pie charts, Venn diagrams, storage of data in reduced format, data reference files and data bases. System Analogue signal Level Boosted analogue Microcomputer Digital signals Microcomputer b system interface 4 I being ' converter Practical Example of Microcomputer Control and Data Processing In order to demonstrate the use of microcomputers we can use commercial instrumentation that today will contain a microprocessor system to control the instrument variables and calculate and present the data.However, such instruments should not displace practical experiments that clearly demonstrate the principles and practice of the technique. To this end, many old, manually operated instruments are being maintained for precisely this purpose.Exam- ples of commercial instrumentation that would present a balanced introduction to the uses and capabilities of microcomputers include : an infrared spectrophotometer with a data station to demonstrate use and construction of reference files of reduced spectral data, spectral enhance- ment, addition and subtraction of spectra; a programmable computing integrator for chrom- atography; an ultraviolet spectrophotometer with derivative functions to demonstrate deconvolution of peaks ; and an atomic-absorption instrument to demonstrate extrapolation of calibration data.A simple practical example that unravels the black box mystery of the dual function of microcomputer control and data collection and processing is the automation of a potentio- metric titration. Such a system is described below and is part of an integrated undergraduate laboratory course. The analysis of diamox (acetazolamide) tablets may be achieved by polarography and by a non-aqueous potentiometric titration (BP method). Students carry out both methods and compare the accuracy and precision of their results. Briefly, in the potentiometric method the acetazolamide is made up in dimethylformamide and titrated with tetrabutylammonium hydroxide solution previously standardised against benzoic acid solution. The automation of the titration includes control of an automatic burette to add An important part of any course is the practical work in support of a lecture course. observed 1 and buffer i signal *.ADC/DAC etc. * I Trigger I Opt0 isolator Electrode switch and transistor IMotor] transducer - pH meter I 1 Titrai 4 - I In I 4 - DAC / I or I/O port , I t I I I I - I I 10 mV,'pH unit I I - - + 1 , / - /// I High ijpedence- I , Autotitration system I - buffe: + ADC I amplifier '/, 5, VDU + Apple microcomputer + floppy discs + printer I - -478 MICROCOMPUTERS AND MICROPROCESSORS s Instructions Standardisation 0-l Mass of sample? Minimum titre? Standardisation information maximium titre J increments 4 Set up Set up assay standardisation routines routines lnitialise titration b Read mV routines Check reading 1 k Y C I 1:.Set scaling I values for I plotting I I 1 Draw axes Label 4 plots Anal. Proc. Differential calculations 1 Draw axes I I Plot I 1 End-point calculation for assay End-point calculation Print-out 0 (End] Fig. 2. Software flow diagram. specified amounts of titrant, collection of the millivolt signal from a glass electrode and a calomel reference electrode, and calculation of the various functions for plotting the results. In addition to the plot of the millivolts (mV) against volume of titrant (V millilitres) to give the usual end-point curve, a plot of d(mV)/dV against A V/2+V is calculated to obtain theOctober, 1982 MICROCOMPUTERS AND MICROPROCESSORS 479 first derivative, which in this instance is a peak, the maximum of which gives the end-point.The second derivative is also calculated and plotted and is used to determine the end-point from the zero crossing point. This gives greater accuracy and reduces the necessity for small increments in the titre needed to define the end-point in the first derivative curve. A schem- atic diagram of the over-all system is given in Fig. 1 and consists of four sections: the system under investigation; the buffer/level converter ; the microcomputer interface ; and the (Apple) micro com put er . System Description The titration system requires a control signal to trigger the motor driving the autoburette syringe for the stepwise addition of the titrant. The signal is derived from a software com- mand that opens a channel in an output port or in a DAC (digital to analogue converter) in the microcomputer interface and thus produce a 5-V pulse.The output is isolated using an integrated opto-isolator chip that has a Darlington output driver. The resulting signal is used to switch a driver transistor, which in turn controls a power transistor switch. The milli- volt output from the glass electrode needs to be amplified by a high input impedance buffer amplifier. This may conveniently be a pH meter with an analogue recorder output or an op amp circuit with a high input impedance and a gain of x 100. If the pH meter output is too low, eg., 10 mV per pH unit, then a x 100 amplifier will also be required. The 0-1 V or 0-5 V boosted analogue signal is then converted into digital information in the microcomputer interface. This consists of an 8-bit analogue to digital converter (ADC) and an %bit digital to analogue converter and associated buffer and timing electronics on a single card placed in slot 3 of the Apple expansion bus.The slots can be directly addressed using Applesoft BASIC and therefore all the programme including the ADC and DAC algorithms may be easily written in BASIC. The ADC/DAC card has on-board buffers and the inputs/outputs can be adjusted for single pole or bipolar operation and for a range up to 0-10 V. A schematic diagram of the system hardware is included in Fig. 1. The software to control the system, that is to send out trigger pulses from the DAC to control the autoburette, trigger the ADC conversion cycle and read in the digital information, is all written in Applesoft BASIC.A flow diagram of the over-all programme is shown in Fig. 2. The programme consists of a series of sub-routines that are called by the main programme. Hence, the general purpose control routines can be incorporated into programmes for other applications where the calculation and data processing requirements differ. Bibliography Poole, L., McNiff, M., and Cook, S., “Apple I1 Users Guide,” Osborne McGraw-Hill, New York, 1981. Titus, J., Larsen, D. G., and Titus, C. A., “Apple Interfacing,” Howard W. Sams, Indianapolis, IN, 1981. Zaks, R., “From Chips to Systems,” Sybex, Berkeley, CA, 1979. Camp, R. C., Smay, T. A., Triska, C. J., “Microprocessor Systems Engineering,” Matrix Publishers, Portland, OR, 1979. The Use of Microprocessors in a Physical Chemistry Laboratory A.G. Ferrige, A. C. R. Strutt and A. J. Everett Wellcome Research Laboratories, Langley Court, Beckenham, Kent, B R 3 3 B S Combinations of electronics, mechanical engineering and Apple and PET microcomputers have played an important part in the automation of instrumentation and data processing in the Department of Physical Chemistry at our laboratories. A number of projects have been completed in the last year and examples will be shown from the following, which demonstrate our progress to date. Nuclear Magnetic Resonance The complete automation of a Bruker Fourier Transform HFX-90 nuclear magnetic reson- ance spectrometer has been achieved. Data acquisition and processing are accomplished via a DEC PDP-11/16 with software to allow automatic processing and plotting of data.A sample changer, constructed entirely from non-ferromagnetic materials, fits on to the probe arm. Movement of the sample-carrying frame in both X and Y directions for sample positioning is achieved by stepping motors driving lead screws.480 MICROCOMPUTERS AND MICROPROCESSORS Anal. PYOC. The entire unit is under control of an Apple microcomputer, as are certain spectrometer functions and their timing. The system operates outside normal working hours, enabling more efficient use of spectrometer time. Microanalysis A PET has been used to automate a Carlo Erba CHN analyser and to perform automated data processing. Here sample masses and descriptors are input along with data relating to standards, blanks, warm-up cycles and expected molecular formulae where known.Data from each cycle are acquired directly into the PET and, at the end of a run, blanks are analysed with “bad” values being rejected using statistical methods. Calibration graphs are calculated and corrections are made to all data. Rigorous mathematical assessments of errors are performed on sample data and the CHN analyses are output along with computer fitting of the data to produce the best fitting for two- and three-component mixtures. Fluorescence An Apple has been interfaced to a Spex Fluorolog and a DEC PDP-11/34. The Apple acts as a data logger and controls basic instrument functions such as scan parameters. The acquired data can then be processed directly by the Apple or sent to the PDP for speediei processing. The software for acquisition of data for fluorescence polarisation spectra has been written in BASIC and although rather slow it prevents tying up the PDP for unacceptable lengths of time.Before this development, 1-2 d were required for hand processing; now the process i: limited only by the data acquisition time. The software also includes spectrum subtraction, smoothing, cutting, spectrum overlays and deconvolution to enhance resolution or sensitivity via Fourier transformation. Ultraviolet Spectrophotometry and Titrations An Apple has been used to control and acquire data from a Beckman ACTA CV spectro- photometer. The data reduction software includes base-line corrections, smoothing, peak listing, plotting routines, etc. In addition, this Apple is used to control simultaneously a potentiometric titration system which incorporates a Beckman 4500 digital pH meter and glass electrode. Stepping motors driving syringes capable of delivering 0.1 pl of titrant are controlled by Acorn micros, slave to the Apple, parameters and titration rates being automatically and continuously varied by instructions computed from the Apple.The ultraviolet and titration systems have been linked, which permits the automatic acquisition of data for spectroscopic pK determination. All routines are written in BASIC. Microcomputer Data Processing in Water Analysis L. G. Royle Severn-Trent Water Authority, Lower Trent Division, Mapperley Hall, Lucknow Avenue, Nottingharn The system described here was initially conceived to handle the data produced by the three sewage treatment laboratories in the Lower Trent Division of the Severn-Trent Water Auth- ority.All three laboratories are of a comparable size, each analysing about 12000 samples per year and each employing about seven analysts. The work ranges from the routine analysis of crude and treated sewage, sludges, soils and trade effluents to more specialised analyses of, for example, pesticides and the rarer trace metals. Results produced at the laboratories are directed internally to operational scientists, locally to operations controllers, to divisional headquarters for the use of senior management and to regional headquarters for archiving. For the information to be of the greatest possible benefit, it has to be validated and transmitted to the prime users, the operations controllers and operational scientists, with the minimum delay possible.October, 1982 MICROCOMPUTERS AND MICROPROCESSORS 481 Prior to the microcomputer system’s installation, the reporting system was manual and required the use of multi-part forms that were completed by individual analysts and then despatched after assessment for accuracy by the senior analyst at each laboratory.Aims of a Microcomputer System The low cost of microcomputers facilitated the justification for purchase of such an instru- ment. After the software had been designed and written and the system had been proved viable in one of the laboratories, it was to be extended to the other two, thus permitting the capture of all the waste-water data generated in the division.Some requirements of the system were: (i) rapid registration of samples; (ii) automatic production of work sheets; (iii) calculation of results from raw laboratory data; (iv) avail- ability to the laboratory manager of the current state of the day’s analysis schedule; (v) computer assessment of the likelihood of each calculated result; (pi) daily production of individually tailored reports; (vii) a carefully designed data base for the permanent storage of results ; and (viii) facilities for utilising the data base to produce period reports, statistics, etc. Hardware Since 1978, the availability of microcomputers in the UK has increased rapidly and the number of different models on the market has proliferated. Certain criteria were laid down, which at the time of purchase, February 1980, only a limited number of the available machines could meet.These included an 80 character screen and a dual 8-in disk drive and led to the choice of a Vector Graphic model. As hardware has developed at a tremendous rate since this purchase, there is little point in dealing with this aspect in greater detail: many machines now have comparable capabilities. Software Operating System The standard CP/M operating system was chosen and it was decided to use the Microsoft MB~src5 high level language supplied with CP/M. This proved to be a very powerful and fast version of BASIC, occupying 24-kbytes of memory. Laboratory Data Processing System The primary object was to create a satisfactory data file structure for the system that would be easily accessible to both producers and users of the information.This proved difficult to effect with a high degree of efficiency and so two major data files were used. The first of these files holds a series of records presented for analysis. These are stored in a purely chronological order, thereby permitting rapid access by the laboratory to samples currently being analysed. However, for long-term storage a second file was set up to which each record is automatically transferred after being verified as complete and correct. This second file holds records sorted into sites and sample types. Subsequent searches of the data carried out, for example, in order to determine the behaviour trends of a particular plant, will find all relevant data stored together, thus making the search rapid and efficient.Use of the System The system is currently being successfully operated in the Division’s three sewage treatment laboratories. It is intended to be used by both senior and junior analysts and each program offers step-by-step prompting instructions to minimke the need for operating manuals. An outline is shown in Fig. 1. This initiates the system and the computer automatically updates its index files before presenting on the screen a “menu” of the available facilities. This procedure is carried out in a matter of seconds. The first stage in the sequence, usually performed at the end of a day, is to run the program REGISTER. This adds to the chronological file the details of all samples to be analysed the following day. A comprehensive series of screen prompts leads the operator rapidly through the procedure, to ensure that the data are entered accurately.Upon completion of this After loading the required disks, the user has merely to press a single key.Anal. Proc. process, and after requesting details of any repeat analyses that might be required, the system prints out the following day’s worksheets, one for each determinand. Only if a particular parameter’s determination has been requested on a given sample will that sample appear on the relevant work-sheet. 482 MICROCOMPUTERS AND MICROPROCESSORS 4 Register { Results -+ 4 Acprint l- f i l e r! f i l e Master d atafile Transfer s , X Z - ( F / datafile I Retrieve Fig. 1. Software. During the following day, each analyst, having completed his worksheet where possible, enters his raw data using RESULTS. As each result is computed, it is displayed, together with a recommendation from the microcomputer on the likelihood of this result for the par- ticular type of sample in question. Using this information for guidance, the analyst can approve the result, upon which it is stored in the correct record, or reject it. If rejected because of a transcription error, the data can be re-entered: if the analysis itself proves to be at fault, the sample is marked for a repeat analysis. At any time during the day, the senior analyst can inspect the current state of the day’s work by running LABPRINT, or by using EDIT he can delete or adjust any entry. A password access system prevents any abuse of this edit facility. With the exception of the BOD results, the analysis schedule is normally complete towards the end of the day. At this time, the senior analyst can use ACPRINT to print out as separate reports a summary of the day’s results for each area manager. This procedure is repeated five days later to provide an updated report containing BOD results and any amendments necessitated by repeat analyses. Thus the data users are offered the benefit of rapid reporting to permit swift action, together with more complete information later for their records. Housekeeping procedures, such as making security copies of the disks and running the TRANSFER program, are carried out at regular intervals by a senior member of staff. Data retrieval from the sorted file can be quickly achieved by use of the program RETRIEVE. This program offers tabulated output and graphical representation of data together with various analyses of trends. Reporting of the data to divisional headquarters is via disks delivered through the internal mail system. Each disk holds a current copy of a laboratory’s master file and can be re- cycled for updating at any frequency demanded. Disks containing information required by the regional archive are periodically produced in the standard IBM format and fed into theOctober, 1982 POTENTIOMETRIC STRIPPING ANALYSIS 483 Division’s ICL 2903 main frame computer. The main advantage of adopting this procedure of data transmission by disk is the avoidance of purchase or rental of the hardware that would be necessary to interlink the computers by land-line. Conclusions The potential of the microcomputer is enormous and its flexibility makes it ideally suited to laboratory data handling. As related costs are low, it can be economically justified even in an organisation that has its own mainframe computer system. Although the system described here is tailor-made to the specific requirements of three particular laboratories, it is nevertheless sufficiently flexible to be altered to meet other needs within a short space of time and with very little extra effort.

ISSN:0144-557X    

DOI:10.1039/AP9821900462

出版商:RSC    

年代:1982

数据来源: RSC

摘要:

October, 1982 POTENTIOMETRIC STRIPPING ANALYSIS 483 Potentiometric Stripping Analysis The following are summaries of two of the papers presented at a Meeting of the Electroanalyti- cal Group held on September 17th, 1980, at the Lillie Hotel, Lillie Road, London. A third (review) paper, presented at this Meeting by D. Jagner, was published in the June issue of The Artalyst, p. 593. Measurement of Copper in Seawater at Environmental pH by Potent iomet r ic S t r i ppi ng Ana I ys i s N. Sheffrin and E. E. Williams Department of Zoology, The University, Shefield, S10 2TN The intricacies of copper complexation in seawater present the marine toxicologist with many problems. Review papers have illustrated some of the theoretical and practical problems.1-3 That the problems are sufficiently complex to cause diasgreement among marine chemists is demonstrated by the conflicting theoretical calculations of inorganic speciation occurring in model systems.*y5 It is important for the biologist to measure the copper in the environment at the pH en- countered by the animal.The significant alteration of the speciation of copper with changing pH has been ~alculated,~ and it may be inferred that any pH change affecting the available copper will alter the response to it by the test organism. In many analytical techniques it is necessary to pre-treat and acidify the sample before measurement. This means that the sample no longer resembles the natural environment and a total metal concentration is obtained, as the copper complexes are broken down during sample treatment.Potentiometric stripping analysis (PSA) can be used to measure the labile species of copper in seawater samples, taken while monitoring toxicity experiments with animals in the laboratory. These labile species are generally agreed to be the biologically active forms of copper .6-10 Experimental A Radiometer ISS 820 ion scanning system was used for the determination of copper in distilled water and seawater samples. The electrochemical principles incorporated in the machine and the procedure followed were as described by Jagner and co-~orkers.~~-~* Copper was determined in 20-ml samples containing 2-200 parts per lo9 (p.p.b.). A11 samples were de-aerated with white-spot nitrogen before plating at -0.6 V. Mercury was added to give a concentration of 5 p.p.m. The glassy carbon electrode (GCE) was pre-plated with mercury from a de-aerated sample and used for 3-5 days before being polished and replated.The GCE was stored overnight together with the platinum electrode in distilled water. The saturated calomel electrode was stored dry. A Radiometer test solution (2 ml) was diluted to 20 ml with distilled water to give a con- centration of 200 p.p.b. of copper. This solution was used to monitor the correct operation of the mercury film and the machine.484 POTE NTI OMETRI C STRIPPING ANALYSIS Anal. Proc. All seawater samples analysed were filtered through a 0.45-pm Millipore filter, so only the dissolved species were measured.15 Some inorganic and organic particles may have passed through the filter, giving the seawater some complexing and adsorbing capacity.16 Aristar-grade hydrochloric and nitric acids were used to acidify samples.AnalaR-grade mercury(1) chloride was used to make a 1000 p.p.m. solution of mercury in de-ionised, distilled water. Copper solutions in de-ionised, distilled water were prepared from AnalaR-grade copper( 11) sulphate and copper( I) nitrate standard solution for atomic-absorption spectroscopy (BDH Chemicals). The addition of copper and mercury solutions did not change the pH of the samples, but deoxygenation was found to increase the pH by approximately 0.2 unit. When seawater samples were measured, the analysis was performed several times until a stable trace was obtained. Measurement of Copper at High pH The speciation of copper is different at high and low pH.At pH 1.0 most of the copper will be labile and a total copper concentration will be measured. At pH 7.7 there should be a smaller proportion of labile copper, as much will be complexed in various forms, depending on the constituents of the seawater. Because of this complexation capacity, any standard addition performed at high pH will not return lOOyo of the spike, so a true value for the copper concentration cannot be calculated. Therefore, after an initial measurement at high pH the sample was acidified to pH 1.0 with 0.5 ml of acid and another trace obtained. This compared the amount of copper released at low pH with the labile fraction at high pH. Standard additions were performed on the sample at low pH, so almost all of the spike was returned.This allowed an estimate to be made of the percentage of total copper that was labile at high pH and the quantification of this fraction in parts per 109. This is illustrated graphically in Fig. 1. I / 1 A a n d a r d Trace length after acidification to low pH , additions // at low pH,/ / Concentration of total copper at /Trace length measured at high pH Concentration of 1 &labile copper at high pH Copper concentration -+ Fig. 1. Measurement of labile copper a t high pH. Results and Discussion The reproducibility achieved with the test solution of 200 p.p.b. of copper in distilled water was a standard deviation of 2% for six consecutive traces. The reproducibilities obtained with seawater samples at low and high pH were standard deviations of 2% and 4y0, respectively, for five consecutive traces.The accuracy for seawater is indicated by a 100 p.p.b. copper spike, which returned 101.5 -& 9.90, and also additions of 2 p.p.b. to a seawater sample with no added copper gave a straight line with a correlation coefficient of 0.991. The measurement of total copper by PSA depends on the way any bound copper is released, that is, whether the sample is acidified and to what pH, whether it is acidified and boiled, or treated with ultraviolet radiation and then acidified. Results obtained using these different methods are given in Table I, which compares the analysis of a “poor quality,’’ i.e., low pH, aquarium seawater by PSA and by atomic-absorpt ion spectrometry (A AS) after extract ion with ammonium t et ramet hylene- dithiocarbamate - isobutyl methyl k e t ~ n e , l ~ ~ ~ * and also a PSA analysis of a “good quality,”October, 1982 POTENTIOMETRIC STRIPPING ANALYSIS TABLE I ANALYSIS OF “POOR QUALITY” SEAWATER BY PSA AND AAS AND “GOOD QUALITY” SEAWATER BY PSA E w- .2 20 n - C .- L g 10- 8 P - m c 485 ..- 0 0 0 I I I I I I Analysis PSA analysis of “poor quality” seawater . . AASlATDC - IBMK* analysis of “poor quality” seawater . . PSA analysis of “good quality” seawater . , Measured copper concentration, p.p.b. 8.3 8.6 6.8 9.6 8.6 14.0 15.8 Z = 10.24 & 3.30 35 samples: 5 = 12.4 f 3.10 1.4 2.2 8.6 0.36 Electrolvsis Plating Sample treatment voltage PH 1.7 Acidified - 0.6 1.1 Acidified - 1.1 1.7 Acidified -0.6 1.7 Acidified -0.6 1.3 Acidified and boiled (15 min) - 0.6 1.6 Acidified and boiled (15 min) - 0.6 1.6 Acidified and boiled (15 min) - 0.6 1.3 Acidified and boiled (15 min) - 0.6 0.9 Acidified -0.6 1.3 Acidified -0.6 7.9 Ultraviolet irradiation (67 min) -0.6 tirnelmL 8 8 8 16 32 8 8 32 32 32 32 * Ammonium tetramethylenedithiocarbamate - isobutyl methyl ketone.When the seawater was acidified with nitric acid, the low pH trace was longer than the high pH trace in the control samples only. For concentrations of copper at 20 p.p.b. and above the high pH trace was longer than the low pH trace. However, when the sample was acidified with hydrochloric acid, the low pH trace was longer than the high pH trace up to concentra- tions of 60 p.p.b.; at higher concentrations the results were reversed, as with nitric acid.These results suggest that there was more labile copper at high pH than at low pH, which contradicts chemical theory. This phenomenon did not occur in the experiment, the results of which are shown in Fig. 2, using low pH buffered seawater. The anomalies cannot be explained by a n effect of dilution, as adding 0.5 ml of de-ionised, distilled water instead of acid had no effect on the trace length. Nor was it an effect of plating time, as the ratio obtained for the high pH trace to the low pH486 POTENTIOMETRIC STRIPPING ANALYSIS Anal. PYOC. trace did not alter from 1.17 -& 0.065~ for plating times of 0.5-32 min at 100 p.p.b. Addition of a further two 0.5-ml aliquots of hydrochloric acid to a 100 p.p.b. sample finally gave a low pH trace of greater length than the high pH trace and further reduced the pH from 1.2 to 0.8 units.From this the total copper concentration was measured and the percentage of labile copper at high pH was calculated. Data for five different concentrations were obtained and the percentage of labile copper was calculated as in Fig. 3. TABLE I1 HIGH AND LOW pH MEASUREMENTS OF SEAWATER WITH HYDROCHLORIC AND NITRIC ACIDS Acid used HNO, (0.5 ml) . . .. HCl (0.5 ml) . . .. Concentration of added copper, p.p.b. Control 20 40 50 60 125 200 20 40 60 100 125 Trace length/cm A r \ High pH (7.7) N.D.* N.D.* 3.50 7.15 4.35 11.70 6.10 19.80 2.80 6.30 9.75 5.65 2.60 5.10 6.25 LOW PH (1.2j 0.70 1.25 3.40 6.75 3.17 9.30 4.25 3.70 7.40 9.80 5.70 2.85 4.50 5.10 13.0 Measured total copper content, p.p.b.2.8 2.2 23.8 47.4 60.4 116.4 21.8 40.5 56.0 58.9 71.2 112.5 - - - * N.D. = not detectable. The percentage of labile copper at pH 7.7 was 85%, which was significantly higher than the value of 20% obtained in Fig. 2. The difference may be attributed to a decrease in the com- plexation capacity of the “good quality” seawater by Millipore filtration and an increase in the complexation capacity of the “poor quality” seawater by the formation of inorganic particles and complexes, the latter occurring when it was buffered to pH 7.7 with sodium hydroxide. 100 I I Copper concentration, p.p.b. Fig. 3. Percentage of total copper present in the labile form at pH 7.7 for un- buffered “good quality” seawater. Why the trace length was shorter at pH 1.2 than at pH 7.7, i.e., indicating less labile copper than expected, needs further investigation.As the method worked successfully with control samples, it seems the copper concentration and the buffers used are important (this phenom- enon is currently under investigation). Notwithstanding the anomalies cited above, it is clear from this investigation that PSA is a valuable technique for the measurement of labile copper at the environmental pH of seawater and, as such, should greatly assist marine toxicologists in their investigations. This work was supported by a grant from Cathodic and Electrolytic Engineers Co. Ltd., Chesterfield.October, 1982 POTENTIOMETRIC STRIPPING ANALYSIS References 487 1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15. 16. 17. 18. Goldberg, E. D., Editor, “The Nature of Seawater,” Dahlem Konferenzen, Berlin, 1975.Schmidt, R. L., CRC Crit. Rev. Enuiron. Control, 1978, 8, 101. Burton, J . D., Phil. Trans. R . SOG. London, Ser. B , 1979, 286, 443. Dyrrsen, D., and Wedborg, M., in “The Sea: Ideas and Observations on Progress in the Study of the Sea,” Volume 5, Wiley-Interscience, New York, 1974, p. 181. Zirino, A., and Yamamoto, S., Limnol. Oceanogr., 1972, 17, 661. Canterford, G. S., and Canterford, D. R., J . Mar. Biol. Assoc. U.K., 1980, 60, 227. Lewis, A. G., Whitfield, P. H., and Ramnarine, A., Mar. Biol., 1972, 17, 215. Stebbing, A. R. D., PhiE. Trans. R. SOC. London, Ser. B, 1979, 286, 465. Steeman Nielsen, E., and Wium Andersen, S., Mar. BioE., 1970, 6, 93. Sunda, W., and Guillard, R. R. L., J . Mar. Res., 1976, 34, 511.Jagner, D., and Graneli, A., AnaE. Chim. Ada, 1976, 83, 19. Jagner, D., and h b n , K., Anal. Chim. Acta, 1978, 100, 375. Jagner, D., Anal. Chem., 1978, 50, 1924. Jagner, D., and h e n , K., Anal. Chim. Acta, 1979, 107, 29. Batley, G. E., and Florence, T. M., Mar. Chem., 1976, 4, 347. Sharp, J . H., Limnol. Oceanogr., 1973, 17, 494. Brooks, R. R., Presley, B. J., and Kaplan, I. R., Anal. Chim. Acta, 1967, 38, 321. Brooks, R. R., Presley, B. J., and Kaplan, I. R., Talanta, 1967, 14, 809. Use of Potentiometric Stripping Analysis in a General Chemical Testing Laboratory E. C. WeIler Research Division, Kodak Limited, Headstone Drive, Harrow, Middlesex, HA 1 4TY A potentiometric stripping analysis system has been evaluated in a general chemical testing laboratory with regard to its suitability as a method for analysing chemicals for trace metals.As part of the routine examination of raw materials (e.g., potassium bromide, ammonium thiosulphate, sodium bisulphite, hydroquinone, methanol and acetone) in this laboratory, heavy metals are determined quantitatively by spectrophotometry together with the use of a continuous-flow automatic analyser. The spectrophotometric methods are well established and the automatic analyser has allowed us to shorten analysis times when large numbers of samples are involved. However, sample ashing is often required and single analyses are relatively time consuming. A method that is fast, suitable for single determinations and requires little sample treatment is required and several alternatives have been compared. These include continuous-flow automatic analysis (CFAA) , flow injection analysis (FIA), differential-pulse polarography (DPP) , anodic-stripping voltammetry (ASV) , potentiometric stripping analysis (PSA) and atomic-absorption spectrophotornetry - inductively coupled -0.9 - 0.7 -0.5 a3 tl, 0 > -0.3 u - -0.1 L Time Fig.1. Multi-ion potentiometric stripping analysis. Concentration of all ions = 0.04 mg 1-1.488 -0.9 -0.7 -0.5 a -0.3 WJ c. - 8 -0.1 POTENTIOMETRIC STRIPPING ANALYSIS Anal. Proc. Time -+ Fig. 2. Normal and derivative potentiometric stripping analysis. Concentration of all ions = 0.4 mg 1-l. plasma (AAS- CP). FIA has the advantage of speed over CFAA but still suffers from sample treatment problems. DPP and ASV have adequate selectivity and sensitivity but there may be problems with the routine use of mercury electrodes in a general chemical testing laboratory.The available equipment for AAS is already fully utilised and an increased work- load would require new facilities. A disadvantage of AAS, as with FIA and the CFAA, is that it analyses single elements only. An inductively coupled plasma (ICP) could provide a multi-element analysis system but would be costly. Hence, PSA appears to offer a fairly cheap alternative to DPP and ASV. The first phase of the evaluation exercise was to use the PSA system for the determination of copper, lead, cadmium, zinc, bismuth and iron. The detection limit for each heavy metal ion was set at 0.5 p.p.m. in the samples. Depending on thse sample treatment this could mean solution detection limits of about 0.05 p.p.m.Fig. 3. Potentiometric stripping analysis of lead, copper and cadmium ions. Concentration of all ions = 0.4 mg 1-l. At this level, the method recommended for PSA is the de-aerated technique. A four- element scan by this method at the 0.04 p.p.m. level required an 8-min deposition time (Fig. 1). Additions equivalent to 0.04 p.p.m. were made and good calibration graphs were obtained. A reproducibility study was carried out for a solution containing lead and bismuth. For lead atOctober, 1982 POTENTIOMETRIC STRIPPING ANALYSIS 489 the 0.04 p.p.m. level a relative standard deviation of 5% was obtained. The measurement of the time plateaux, corresponding to concentration, was tedious and time consuming and operation in the derivative mode might have advantages.Such a scan is shown in Fig. 2 for the same four metal ions. The concentrations were 0.4 p.p.m. and the deposition time was 2 min. Measurement of the distances between peaks was found to be easier than constructing tangents, etc., for the normal scan. However, if there are small waves in the presence of larger ones in the normal scan, the element peaks may be lost in the derivative mode. There are five peaks, in the derivative mode, for four elements present. Therefore, for three ele- ments, four peaks would be expected. In Figs. 3, 4 and 5 there are four peaks but, in each Fig. 4. Potentiometric stripping analysis of lead, cadmium and bismuth. Concentration of all ions = 0.8 mg 1-l.instance, different elements are present. Lead, copper and cadmium are present in Fig. 3. Lead, cadmium and bismuth give a similar pattern in Fig. 4. In Fig. 5 the same peak pattern exists, but there are four metal ions present: lead, copper, bismuth and cadmium. It would seem, therefore, that although the derivative mode makes the time measurement easy, a normal scan is required for the identification of the metals present. 0 - Normal Time ---+ Fig. 5. Potentiometric stripping analysis of lead, copper, bismuth and cadmium. Concentrations of ions: Cd, Pb, Bi, 0.8 mg 1-l; and Cu, 0.4 mg 1-l.490 POTENTIOMETRIC STRIPPING ANALYSIS Anal. Proc. So far, only the analysis of the six metal ions chosen for the first phase of the evaluation has been described. This excludes zinc.If both zinc and copper are present, an intermetallic effect occurs. When the deposition voltage is raised negatively to observe zinc this intermetallic effect can be observed. The zinc wave decreases while the copper wave increases. In these instances, copper could be analysed with a deposition voltage of -0.9 V, while zinc can be determined after the addition of gallium(II1) ions, which complex copper ions more strongly. The copper wave will also deteriorate if the mercury level is not high enough. A scan of a 20% solution of potassium bromide is shown in Fig. 6. An addition equivalent to 0.04 p.p.m. of cadmium, lead, copper and bismuth has been made, showing no evidence of these metals in the The deposition voltage has not exceeded -0.9 V for the scans so far.Examples of some analyses of typical chemicals are shown in Figs. 6 and 7. I Time __+ Fig. 6. Potentiometric stripping analysis of potassium bromide : A, 20% potassium bromide ; and B, addition of 0.04 mg 1-1 of Cd2+, Pb2+, Cu2+ and Bi2+. Time __+ Fig. 7. Potentiometric stripping analysis of sodium sulphate (10% solution). sample at this level. A 10% solution of a particular batch of sodium sulphate contains zinc at a high level (Fig. 7). With methanol, there is no dilution factor, thus increasing sensitivity. For the chemicals studied so far the PSA system has the necessary sensitivity but unfortu- nately the scan times are long, ranging from approximately 1 min for solvents to approximately 8 min for 10% solutions of chemicals, Le., for 0.5 p.p.m. levels in the chemicals.If it is necess- ary to obtain a quantitative result, at least four scans (sample + three standard additions) would be required, and possibly five (two runs of the sample to check reproducibility). Thus, I \ I Fig. 8. Anodic-stripping voltammogram of lead, cadmium, bismuth and copper. A, Concentration of all ions = 0.04 mg 1-I; B, addition of 0.04 mg 1-' of Pb2+, Cde+, Bi2+ and Cu2+; and C , further addition of 0.04 mg 1-1 of all ions.October, 1982 EQUIPMENT NEWS 491 one sample could take nearly 1 h for total analysis. If used as a limit test it would be quicker. Anodic-stripping voltammetry has better sensitivity and can give considerably reduced analysis times. Fig. 8 shows an ASV scan for four elements together with known additions. The relative standard deviation for this method using a hanging mercury drop electrode (HMDE) was less than 3%. Comparing multi-ion analysis times for various techniques, ASV is undoubtedly the quickest. However, problems have been experienced with hanging drops and in our current studies we are investigating ASV with HMDE for use in a routine environ- ment. If it is found that the system is satisfactory, ASV would appear to be more suitable for us than PSA. So far we have not been able to determine iron by PSA but there is a response that we might use by ASV. Also, the measurements of current peak heights in differential-pulse ASV (DPASV) are easy. Therefore, for several reasons ASV in the DP mode might be a better proposition than continuing with PSA unless the following requirements can be met: micro- processor for easier measurement, shorter analysis times and a method for iron. With regard to the applicability of electroanalytical techniques for the analysis of trace metals by direct dissolution, without ashing, etc., further work needs to be carried out.

ISSN:0144-557X    

DOI:10.1039/AP9821900483

出版商:RSC    

年代:1982

数据来源: RSC

摘要:

October, 1982 EQUIPMENT NEWS 491 Equipment News Further details of all items reported below are available from the companies concerned. For rapid information please complete the Reader Enquiry Service card (circle the appropriate number mentioned), rather than approaching companies direct. Atomic-absorption Spectrometer Software A package that is available to run on Commo- dore computers allows several modes of opera- tion, including construction of a calibration graph and calculation of results with reference to it. Anaspec Limited. Circle 501. Infrared Spectrophotometers The 1400 series of ratio recording instruments consists of two models, the Model 1420, covering the range 4000-600 cm-', and the Model 1430, which scans from 4000 to 200 cm-I. Both feature integrated scan controls and ordinate scale expansion from x 1 to x 100.The Model 1500 Fourier Transform Infrared System, featuring high-speed interferometric scanning and data processing, employs the 3600 IR Data Station. Perkin-Elmer Ltd. Circle 502. Spectrophotometric Instrumentation A range of Shimadzu instruments includes the UV120 single-beam instrument, the UV150 double-beam, digital, ultraviolet - visible or visible-only spectrophotometer, the UV190 double-beam scanning instrument, the UV300 and UV365 dual-wavelength recording spectro- photometers and the UV240 microprocessor- controlled ultraviolet - visible recording instru- ment. A full range of accessories is also available. V. A. Howe & Co. Ltd. Circle 503. Chromatography Data Systems Nelson Analytical systems, based on Hewlett- Packard microprocessors, include the 440 single instrument system based on the HP-85 and a multi-instrument system based on the HP-9826.They include all the necessary hardware and software. Anaspec Ltd. Circle 504. Luer Fittings for HPLC Various SSI Luer fittings are available for priming of HPLC systems. They can be panel mounted. Scientific Glass Engineering (UK) Ltd. Circle 505. Syringe The Hamilton Model 7000.5 is a half-microlitre syringe with its total capacity in the needle. A seal can be tightened to operate at pressures up to 400 bar. V. A. Howe & Co. Ltd. Circle 506.492 ANALYTICAL PROCEEDINGS Anal. Proc. INTEGRATING POWER AT ECONOMICAL RATES Buying an integrator? Don't accept anything less than ac- curate, precise integration.Look at the extras like a BASIC interpreter, autosampler control etc. Then look at the price. For f1,725 + VAT, we can provide you with a computing in- tegrator (complete with cables and a 45 page instruction manual). How do w e do it? We took a well known microcomputer and designed a dynamic range 2-channel analogue/digital convertor interface (1 -1 O6 dynamic range, 0.025% resolution). We then spent several months developing a really brilliant piece of software. . . . The result is 4 k of pura machine code (available only in ROM) which 'takes over' the microprocessor within the computer to integrate-as in a dedicated integrator. There are a possible 42 individual integration parameters, although only 10 are required before integration will begin. The parameters (slope sensitivity, threshold etc) are entered as BASIC statements.Four different baseline tracking modes are available. The results (area, retention time and peak height) are returned in arrays-ready for the power of your o w n BASIC programme. Don't spend more on data analysis that you did for the chromatograph ! Digital Measurement and Analysis Ltd. 906 Woodborough Road, Mapperley, Nottingham NG3 5QR Tel:- (0602) 622686 Circle A404 for further information. V. A. Howe B Co. have been associated with Shimadzu of Japan for over twenty years. Recently there have been several outstanding new products from Shimadzu worthy of mention. The first is the UV240, UV/Visible Spectrophotometer. Originally introduced in Autumn 1 981, this instrument is a totally micro- processor controlled, double-beam UV/Visible spectrophotometer.The introduction of the UV240 rep- resented a totally unique approach to the use of microprocessors in spectrophotometers, since at the heart of the system is a thermal printer/plotter unit which contains all the operating functions for total control of the instrument. The UV250 has been produced to complement the UV240. The UV250 has the same graphic printer/plotter unit as the UV240 but the optical unit is a double-beam dual mono- chromator system giving high energy, extremely low stray light and high precision. Although both the UV240 and UV250 are impressive instruments with an abundance of functions, a whole new dimension of spectroscopic analysis is opened by the addition of a microcomputer.Interfaces are available for the UV240 and UV250 for use with most popular micros, including Apple and HP85F. Another Shimadzu product with } microcomputer control is the UV/VIS/NIR double-monochromator UV365. This instrument not only has prism-grating double monochromator to provide excellent resolu- tion and minimum stray light, but the UV365 features derivative spectra, auto-baseline correction and partial spectral expansion as standard. Shimadzu will shortly be releasing the I R435, another micro- processor controlled instrument, this time in the lnfra red region, which features a fascinating and extremely useful facsimile chart recorder. A microprocessor controlled instrument from Radiometer, Copenhagen, is the DTS833 digital titration system. This instrument can handle all types of titration and can titrate to any number of end points with the computer mathematically predicting the end point and automatically slowing down the titrant delivery accordingly just as a human would ! HOWE V.A. HOWE & CO. LTD., Telephone: 01 -874 0422 Telex No : 2621 10 12-14 ST. ANN'S CRESCENT, LONDON. SW18 2LS Circle A403 for further information.October, 1982 EQUIPMENT NEWS 493 Clinical Chemistry Analysers Digital/Analogue Meter The Eppendorf ACP 5040 is a single-channel “Harmony” is a panel meter providing a digital instrument for the determination of enzymes, display and trend indication. It can be pro- substrates, immunoglobins and EMIT. It has grammed to read in any engineering unit a maximum throughput of 300 enzymes per hour and is programmable for up to 16 different methodologies.The Eppendorf PCP 6121 is a semi-automated photometer. Circle 507. Baird & Tatlock (London) Ltd. Gas Analysis The Model 3061 Autospot is portable and is certified to Cenelec standard Ex ia IIc T5. It allows measurement of TDI, hydrogen sulphide, including non-linear quantities. It can also function as a meter relay initiating signals at fixed or variable set points. Sifam Ltd. Circle 512. Digital Multimeters A range of four Metrix models provides for measurement of temperatures from -20 to + 1200 OC, decibel measurements from -40 dB to +50 dB and frequency measurements up to 50 kHz. They also read the true RMS value Phosgene, chlorine, hydrogen cyanide, sulphur dioxide, aliphatic amines, nitrogen dioxide, and memorise peak values.hydrazine, ozone, formaldehyde and ammonia. Digitron Instrumentation Ltd. Circle 5 13. MDA Scientific (UK) Ltd. Circle 508. Conductivity Meter The Model 2051 portable instrument has a triple range: 0-19.99 pS resolved to 0.01 pS; 0-199 p S to 1 pS; and 0-19.99 mS to 0.01 mS. V. A. Howe & Co. Ltd. Circle 509. Digital Thermometers Three portable models are available covering the range - 30 to + 1 200 OC. A range of sensors enables reading in liquids, semi-solids, air and surfaces. A differential temperature convertor is also available. V. A. Howe & Co. Ltd. Circle 510. Temperature Controller The 5190 Series pneumatic temperature con- troller uses plant air supply to drive a built-in generator powering the controller and sensing system.Fisher Controls Ltd. Circle 511. Digital Gaussmeter The RFL, Model 912, permits the measurement of permanent magnet, d.c. and a.c. fields. The display is bipolar, enabling field polarity to be determined. Measurement range is from 0.01 G to 100 kG. Wessex Electronics Ltd. Circle 514. Analogue/Digital Interface The SP800 8-channel analogue/digital interface expands the application areas for the ESlOOO digital electrostatic chart recorder by allowing any of 30 signal-conditioning modules to be used with the recorder. Gould Instruments Ltd. Circle 516. Transient Recorder The memograph records mains supply faults and disturbances and other similar electrical signals. It continuously monitors the input494 EQUIPMENT NEWS Anal. Proc. signals but the recording lamp and paper drive Tubing Cutter are switched on only when a fault or disturbance The Terry Tool Tubing Cutter cuts &-in metal is detected.tubing in one step. Bell & Howell Ltd. Circle 517. Scientific Glass Engineering (UK) Ltd. Circle 522. Recorder The Model 500 single- and two-pen recorder has full-scale sensitivity from 1 mV to 50 V and 20 Literature chart speeds from 3 mm h-l to 600 mm min-1. Tekman Electronics Ltd. Circle 515. Single or Dual Channel Microcomputer This system processes output from the Auto- matic Analyser system. Features include variable throughput rate, optional drift corrected and/or raw data results, store data facility, timed sample interval printout and continuous sample data update display. Gradko International Ltd.Circle 5 18. A booklet describes the Spectrosol range of materials for atomic-absorptiofi spectroscopy including aqueous and oil-soluble standards, ionisation buffers, release and complexing agents and extraction solvents. BDH Chemicals Ltd. Circle 523. Application Note 81-162 reports on the use of the CSI 740 X-Ray Analyser in the analysis of silver ores. Data tables give examples of how the instrument is set up for various types of ores. Columbia Scientific Industries Corporation. Circle 524. A leaflet gives information on a modular HPLC system for the separation of biopolymers. LKB Instruments Ltd. Circle 525. A data sheet shows analyses of amino acids by HPLC resins. These resins are designed for use with narrow bore columns but may also be used with 9 mm i.d. columns.Field Instruments Co. Ltd. Circle 526. A data sheet gives information on a range of low dead-volume fittings for chromatography. Among the products available are the Universal ooo p.s.i.g. automatic sample injector and 3000 p.s.i.g. sample injection valves. Also available are guard columns, post-column Centrifuge The MK IV has electronically acceleration giving reproducible spin speeds. An automatically activated brake brings the motor to rest within 30-90 s with minimum sediment disturbance. Baird ' (London) Ltd* 519* reaction end fittings, micro-HPLC column end Filter-papers Microfiltration Systems qualitative papers are available in three grades: the No. 1 retains particles greater than 10 pm, the No. 2 retains above 5 pm and the No. 131 retains particles less than 5 pm.There are seven grades of quantitative paper. V. A. Howe & Co. Ltd. Circle 520. Tissue Processor The Polaron E9000 automatic instrument can duplicate any sequence of manual operations used to prepare biological samples for resin embedding. V. A. Howe & Co. Ltd. Circle 521. fittings and the ATOC-1 automatic trace organics concentrator. Field Instruments Co. Ltd. Circle 527. A catalogue describes the Ohio Valley Speciality Chemicals chromatography products. Also available is information on OV-351, a new stationary phase for GC. Field Instruments Co. Ltd. Circle 528. A booklet illustrates a wide range of products for thin-layer chromatography. TLC products are also described in the Analabs general chromatography catalogue. Field Instruments Co.Ltd. Circle 529.October, 1982 ANALYTICAL PROCEEDINGS PI.ri[nted I"ecoIQ(s in Meftler thernral anaiysis alicvays clear and comple kw example: automatic d a t a n n i ~ O b g W ~ ~ -m- All the parameters necessary to carry out analysis and evaluate results are stored in the control instrument of Mettler's TA3000 Thermal Analysis System. All that is necessary before starting the test is entry of the respec- tive method number. The connected printer/plotter records the measuring curve and prints out the results - clearly and completely. DSC, Ir;, IMA. Easy, economical and mtsatik The Mettler TA3000 System is easy to operate and can be expanded without problem. Although it is moderately priced, it is extremely versatile. Compre- hensive evaluation programs for the various measuring modules are per- manently stored in the memory of the TC10 Control Instrument.The programs range from the DSC integration program to cornplete kinetic evaluation of DSC or TG measuring data. 77mmalana&sk farmmamh,deveIopmentand Quality- The Mettler TA3000 System covers the complete range of applications in thermal analysis. The following are just a few examples: - Crystallinity - Glass transition temperature - Oxidation stability - Solid-liquid fraction plots - Curing times - PUrity determination - Specific heat - Melting/crystallization behavior - Rate of chemical reaction Our applications lab is constantly developing new applications, the results of which are published in a series of Application Bulletins. Bulletins for the areas which are of interest to you are available on request.495 lnformaoibncoupon 13 I would like to know more about the Mettler TA3000 System. Please call me to make an appointment. 0 Please send me detailed information. 0 I am interested in obtaining Applica- tion Bulletins in the following field: Name: Company: Address: Tel. No. Please mail coupon to: Mettler lnstrumente AG CH-8606 Greifensee, Switzerland Tel. (01) 941 22 41, Telex 54592 6377.72 1 Mettler is represented in more than 120 countries, UK: MSE Scientific Instruments, Manor Royal, Crawley, Sussex RHlO 2QQ. Circle A401 for further information.496 PUBLICATIONS RECEIVED Anal. Proc. A catalogue describes Dynatech Precision Sampling products for GC and HPLC. These include syringes, samplers for pressurised liquids, mininert valves and other accessories.Field Instruments Co. Ltd. Circle 530. A range of air pollution monitors and accessor- ies is the subject of a brochure, which also des- cribes precision calibrators for NO, NO,, H,S, SO, and 0,, clean air sources and sample condi- tioning systems. Techmation Ltd. Circle 53 1. Technical literature is available on the B series Ohaus electronic balances, which comprise seven models, including three dual-range units. Optional extras include software interface connections for recording and computing. Boro Labs Ltd. Circle 532. A data sheet is available on the DE-MIST fume cupboard scrubbing system for the removal of perchloric acid and other hazardous vapours. An automatic pH sensing and neutralising system is an optional accessory. Newmet Pifan Ltd. Circle 533. A brochure describes the range of Tescom pressure regulators for high-purity or corrosive liquids. Information is also available on the new 44-3400 Series, which is a two-stage pressure reducer in which all wetted parts are type 316 stainless steel or PTFE. Techmation Ltd. Circle 534. A brochure gives details of a range of sample conditioning equipment for the power industry. Kent Industrial Measurements Ltd. Circle 535. A catalogue gives information on the Nalgene range of laboratory plastic ware, which includes centrifuge tubes, test-tube racks, bottles, carboys, filter ware, etc. Circle 536. Baird & Tatlock (London) Ltd. A catalogue is available covering a range of agency products including the Porter range of low flow control products and the SSI range of HPLC accessories. Scientific Glass Engineering (UK) Ltd. Circle 537.

ISSN:0144-557X    

DOI:10.1039/AP9821900491

出版商:RSC    

年代:1982

数据来源: RSC

摘要:

496 PUBLICATIONS RECEIVED Anal. Proc. Publications Received Methods for the Examination of Waters and Associated Materials. Standing Committee of Analysts (to review Standard Methods for Quality Control of the Water Cycle) ; Department of the Environment, National Water Council. HM Stationery Office. Nickel in Potable Waters, 1981. Pp. 30. 1982. Price L2.80. ISBN 0 11 751604 X. Total Hardness, Calcium Hardness and Mag- nesium Hardness in Raw and Potable Waters by EDTA Titrimetry, 1981, Tentative Methods. Pp. 20. 1982. Price L2.40. ISBN 0 11 751600 7. Odour and Taste in Raw and Potable Waters, 1980. Pp. 19. 1982. Price L2.40. ISBN 0 11 751597 3. Analysis of Surfactants in Waters, Waste- waters and Sludges, 1981. Pp. 68. 1982. Price L4.20. ISBN 0 11 751605 8. Education and Teaching in Analytical Chemistry.G. E. Baiulescu, C. Patroescu and R. A. Chalmers. Ellis Horwood Series in Analytical Chemistry. Pp. 190. Ellis Horwood (distri- buted by John Wiley). 1982. Price L15. ISBN 0 85312 384 5 (Ellis Horwood); 0 470 27283 X (Halsted Press). In the development and training of an ana- lyst, to equip him to tackle the current problems of chemical analysis, the teaching and education he receives play an important role. This work lays out all the educational requirements in analytical chemistry. It promotes the concept of the analytical chemistry student being “situation oriented,” deliberately encouraged to educate himself. New Trends in Chemistry. Edited by F. L. Boschke, Topics in Current Chemistry, Volume 100. Pp. viii + 213. Springer-Verlag. 1982.Price DM98 ; $45.70. The critical reviews in this volume are : “Trends in Analytical Chemistry” by D. Betteridge and T. J. Sly; “Topics in Photochemistry” by H. E. Zimmerman ; “New Developments in Polymer Synthesis” by T. Saegusa ; “Biochemical Engin- eering” by H. Janshekar; “Chemistry and Spectroscopy of Rare Earths” by C. K. Jorgen- sen and R. Reisfeld; “Systematization and Structures of the Boron Hydrides” by L. Barton. ISBN 3 540.11287 1; 0 387 11287 1.October, 1982 PUBLICATIONS RECEIVED 497 L’Atomisation Electrothermique en Spec- trometrie d’Absorption Atomique et son Application dans les Etudes de 1’Environne- ment. Michel Hoenig, Stbphane Dupire and Rolland Woolast. Pp. vi + 218. Technique et Docu- mentation. 1982. Price Fr180; BFrl260.ISBN 2 85206 115 5. This book includes chapters on atomisation sources, interferences in atomisation, procedure for electrothermal atomisation, instrumentation, mineralisation and dissolution of samples, concentration and separation of analytes and discussions of individual elements. (In French.) Stable Isotopes. Proceedings of the 4th International Conference, Julich, March Edited by H.-L. Schmidt, H. Forstel and K. Heinzinger. Analytical Chemistry Symposia Series-Volume 11. Pp. xviii + 775. Elsevier. 1982. Price $127.75; Dfl275. ISBN 0 444 42076 2. The 85 contributions and 15 reviews in this volume give an overview of the state of investi- gations on stable isotopes of the main bio- elements as they occur in nature. The confer- ence emphasised stable tracer applications in medicine, pharmacology, agriculture and bio- chemistry, and added to the dimension of the theory and consequences of isotope effects, and the importance of stable isotopes in geochem- istry, cosmochemistry and environmental re- search.The papers compare recent results and meth- odology in the different disciplines obtained on the basis of isotope measurements. Inter- action between the disciplines was facilitated by a common methodology, which revealed that a particular problem could be approached from various angles and stimulus given for further investigations. Examples of new possibilities are the use of NMR in biological research and the introduction of “naturally labelled” com- pounds in nutrition physiology. 23-26’1981. A New View of Current Acid- Base Theories.Harmon L. Finston and Allen C. Rychtman. Pp. viii + 216. John Wiley. 1982. Price L35. The authors combine the various acid - base theories into a unified, all-encompassing theory, which includes oxidation - reduction processes. After tracing the historical development, the Arrhenius, Bransted-Lowry, solvent systems, Lewis and Usanovich theories are discussed. ISBN 0 471 08472 7. The final chapter is on procedures for the experi- mental verification and reconcilement of the various theories. Wilson and Wilson’s Comprehensive Analy- tical Chemistry. Volume XII. Thermal Analysis. Part B. Biochemical and Clini- cal Applications of Thermometric and Thermal Analysis. Edited by Neil D. Jespersen. Pp. xviii + 254. Elsevier. 1982. Price $79; Dfl170.ISBN 0 444 42062 2. This volume of papers reviews the progress that has been made in bioanalytical calorimetry. It brings together the diverse approaches of thermal and calorimetric analyses as applied to biochemical and clinical studies and describes several thermal, or calorimetric, techniques. The instrumentation section discusses thermo- metric titrimetry (both isoperibol and iso- thermal), direct injection enthalpimetry, differ- ential scanning calorimetry and heat conduction calorimetry (batch and flow). In addition, two other thermometric approaches are in- cluded : flow reactors employing immobilised enzyme reaction beds and thermistor probes of various designs. The application of these various techniques is then described, along with critical evaluation of their future applicability to routine clinical analysis.Reviews of pharma- ceutical analysis and macromolecules, lipid studies, enzyme analysis, protein studies and previous work with small ion analysis are also included. Pesticide Residues and Exposure. Edited by Jack R. Plimmer. ACS Symposium Series 182. Pp. x + 213. American Chemical Society. 1942. Price $27.95. ISBN 0 8412 0701 1. This 15-chapter book is based on a symposium sponsored by the Division of Pesticide Chemistry a t the Second Chemical Congress of the North American Continent (180th ACS National Meeting), Las Vegas, Nevada, August 26-27, 1980. The current problems of measuring and monitoring worker exposure are examined. Differences in climates and agricultural systems all contribute to the nature and longevity of chemical residues in different regions.The special problems of California are dealt with specifically. Re-entry guidelines, studies in the effectiveness of protective clothing, and the use of animal models to estimate potential exposure are discussed, as are the sites of pesticide entry into the body.498 PUBLICATIONS RECEIVED Anal. PYOC. The Theory of Vibrational Spectroscopy and its Application to Polymeric Materials. Paul C. Painter, Michael M. Coleman and Jack L. Koenig. Pp. x + 530. John Wiley. 1982. Price L44.50. ISBN 0 471 09346 7. The first 9 chapters introduce the general theory of vibrational spectroscopy in a straightforward manner. Computer methods for solving vibra- tional problems are outlined, and specific examples and recent methods for calculating infrared and Raman intensities are discussed.Tables of force constants that can be applied directly to the vibrational analysis of various polymers are included. There is a comprehen- sive example, the normal co-ordinate analysis of benzene, from initial band assignment through the details of the force field calculation. The discussion is extended to treat the vibrational spectra of polymer crystals and disordered polymers. The final chapters present the vibra- tional analysis of selected polymers. Developments in Polymer Characteris- ation, Volume 3. Edited by J. V. Dawkins. Developments Series. Pp. x + 266. Applied Science. 1982. Price L30. The six reviews in this volume are: Separation and Molecular Characterisation of Copolymers by Hiroshi Inagaki and Takeshi Tanaka; Study of Structure and Interactions in Polymers by Inverse Gas Chromatography by J.E. G. Lipson and J. E. Guillet ; Dielectric Techniques by H. Block and S. M. Walker; Spin Label and Spin Probe Studies of Synthetic Polymers by G. Gordon Cameron and A. T. Bullock; Tor- sional Braid Analysis (TBA) of Polymers by J. K. Gillham; and Applications of Ultraviolet Microscopy to Polymers by N. C. Billingham and P. D. Calvert. ISBN 0 85334 119 2. Fourier, Hadamard, and Hilbert Trans- forms in Chemistry. Edited by Alan G. Marshall. Pp. xii + 562. Plenum. 1982. Price $65. ISBN 0 306 409046. This volume will acquaint practising chemists with the basis, advantages and applications of Fourier, Hadamard and Hilbert transforms in chemistry. The emphasis is on practical aspects.In areas where the use of transform techniques is already well established (e.g., FT-NMR and FT-IR) the newest transform applications are described (such as two- dimensional FT-NMR and photoacoustic FT- . IR). New techniques covered include, for example, FT-ion cyclotron resonance (mass spectroscopy), FT-ENDOR, FT-Faradaic ad- mittance (a.c. polarography), Hadamard trans- form IR spectroscopy and Hilbert transform for spectral line shape analysis. Organic Analysis Using Ion-selective Electrodes: Volume 1, Methods; Volume 2, Applications and Experimental Procedures. T. S. Ma and S. S. M. Hassan. The Analysis of Organic Materials. Pp. xiv + 184 (Volume 1) ; xiv + 284 (Volume 2). Academic Press, 1982. Price L19.20, $39.50 (Volume 1); k24, $49.50 (Volume 2).ISBN 0 12 462901 6 (Volume 1); 0 12 462902 4 (Volume 2). This book is organised into three parts, pub- lished in two volumes. Volume 1 presents the background of ion-selective electrodes. The theoretical basis is discussed in a concise manner and the equipment and operations are described. The characteristics of various types of ion-selective electrodes, as well as the differ- ent measuring techniques, are also covered. Volume 2, which comprises Parts Two and Three, concentrates on the analysis of organic materials. Part Two involves an extensive survey of the literature. The methods and procedures for the determination of the ele- ments, functional groups, biochemical sub- stances, natural products and pharmaceuticals are reviewed. Potential applications of certain electrodes are indicated.Part Three presents 38 experiments as typical examples to cover the different areas of organic analysis. General Handbook of On-Line Process Analysers. D. J. Huskins. Ellis Horwood Series in AnalyticaE Chemistry. Pp. 239. Ellis Hor- wood. 1981. Price L30. ISBN 0 85312 329 2 (Ellis Horwood); 0 470 27292 9 (Halsted Press). This is the first book of a series on process analysers (the other 4 books are on Quality Measuring Instruments, Optical Methods, Elec- trical and Magnetic Methods and Gas Chromato- graphic Methods). The first volume provides an understanding of the proper use of analysers and describes the role of analyser systems, containing all the necessary detail, including background theory, and looks at all the considerations to be taken into account when an analyser system is to be installed. The main text is preceded by a list of abbreviations, symbols and pressure units.The equipment and the applications are ex- plained and the necessity for an adequate andOctober, 1982 PUBLICATIONS RECEIVED 499 accurate specification guide for all components of an analyser system is stressed. There is a guide to the selection of the most suitable method and a chapter on the economics involved in the selection of analyser systems and equip- ment. Separation and Preconcentration Methods in Inorganic Trace Analysis. J . Minczewski, J. Chwastowska and R.Dybczyh- ski. Ellis Horwood Series in Analytical Chemistry. Pp. xii + 543. Ellis Horwood (distributed by John Wiley), Wydawnictwa Naukowo-Tech- niczne.1982. Price L37.50. ISBN 0 85312 165 6 (Ellis Horwood) ; 0 470 27169 8 (Halsted Press). This text provides a theoretical pathway for understanding the basic principles underlying modern separation and pre-concentration methods, together with trace-element orientated examples of application. It points out both the advantages and disadvantages of the methods available and discusses the improve- ment in detection limits which these isolation methods can achieve. The book deals with methods based on precipitation and coprecipita- tion, volatility of constituents, liquid - liquid extraction, ion-exchange and reversed-phase chromatography. Atmospheric Pollution 1982. Proceedings of the 15th International Colloquium, Paris, France, May 4-7, 1982.Edited by Michel M. Benarie. Studies in Environmental Science, Volume 20. Pp. xii + 404. Elsevier. 1982. Price $88.25; Dfl190. ISBN 0 444 42083 5. Comprising a selection of papers from the 1982 Colloquium, this volume presents developments in the more classical aspects of air pollution, i.e., modelling (10 papers), health effects- pollution control (6 papers), aerosols ( 12 papers) and surveys and monitoring (6 papers), and includes coverage of air pollution problems of hot and desert regions (18 papers). These papers have also been published as a special issue of The Science of the Total Environment (Volume 23, 1982). A Dictionary of Spectroscopy. Second Edition. R. C. Denney. Pp. xiv + 205. Macmillan. 1982. Price j515. ISBN 0 333 31670 3. A Dictionary of Chromatography.Second Edition. R. C. Denney. Pp. xiv + 229. Macmillan. 1982. Price j515. ISBN 0 333 31667 3. The Second Editions (complete updates and revisions of the First Editions) of these two dictionaries are a result of the fast-changing and expanding fields of spectroscopy and chromato- graphy as it is increasingly difficult for the non- specialist to keep informed of all the develop- ments that have occurred. They aim to assist those who are not expert in the subjects by explaining clearly and concisely expressions and techniques most frequently employed ; for example in spectroscopy, infrared, ultraviolet and nuclear magnetic resonance spectroscopy are all explained, as are mass, Raman, Moss- bauer and Auger Spectroscopy. Both books contain numerous diagrams and substantial lists of references to more specialised texts on the various subject areas.As far as is practi- cable symbols and nomenclature have been standardised and updated in line with most recent recommendations, adhering to those published by the Symbols Committee of the Royal Society and IUPAC, employing SI units. Recent Advances in Analytical Spectro - scopy. Proceedings of the 9th InternationaI Conference on Atomic Spectroscopy and 22nd Colloquium Spectroscopicum Inter - nationale, Tokyo, Japan, 4-8 September 1981. Edited by Keiichiro Fuwa. IUPAC Sympos- ium Series. Pp. x + 325. Pergamon. 1982. Price $75; j537.50. This meeting was organised by the Japan Society for Analytical Chemistry, with the cooperation of the Spectroscopical Society of Japan, under the sponsorship of the Ministry of Education, Science and Culture of Japan, the Science Council of Japan, IUPAC, the Japan Society of Applied Physics and the Chemical Society of Japan. The 20 sessions encom- passed the whole field of analytical spectro- scopy, including for example, plasma emission, Zeeman atomic absorption, computers in analytical spectroscopy and applications to life science.This volume includes 26 of the invited lectures. ISBN 0 08 026221 X. Methods for the Examination of Waters and Associated Materials. Standing Committee of Analysts (to Review Standard Methods for Quality Control of the Water Cycle) ; Department of the Environment National Water Council. HM Stationery Office. Ammonia in Waters 1981. Pp. 47. 1982. Price L3.80.ISBN 0 11 751613 9.500 ANALYTICAL PROCEEDINGS Anal. Proc. Analytical Sciences Monographs No. 4 Electrothermal Atomisation for Atomic Absorption Spectrometry by C. W. Fuller Since the introduction of atomic absorption spectrometry as an analytical technique, by Walsh, in 1953, the use of alternative atomization sources to the flame has been explored. At the present time the two most successful alternatives appear to be the electrothermal atomiser and the inductively- coupled plasma. In this book an attempt has been made to provide the author's views on the historical development, commercial design features, theory, practical considerations, analytical parameters of the elements, and areas of application of the first of these two techniques, electrothermal atomisation.Hardcover 135pp 0 85186 777 4 f 18.00 ($38.00) RSC Members f 13.50 No. 5 Dithizone by H. M. N. H. Irving The author of this monograph, who has been closely associated with the development of analytical techniques using this reagent for many years, and who has made extensive investigations into the properties of its complexes, has gathered together a body of historical and technical data that will be of interest to many practising analytical chemists. Hardcover 112pp 0 85186 787 1 f 12.50 ($27.00) RSC Members f 9.50 No. 6 lsoenzyme Analysis Edited by D. W. Moss This monograph attempts to draw together the most important experimental techniques which have resulted from the modern recognition that enzymes frequently exist in multiple molecular forms.This monograph also indicates the advantages and limitations in isoenzyme studies of these modern experiments. Brief Contents: Multiple Forms of Enzymes; Separation of Multiple Forms of Enzymes; Selective Inactivation of Multiple Forms of Enzymes; lmmunochemistry of Multiple Forms of Enzymes; Catalytic Differences between Multiple Forms of Enzymes, Methods of Obtaining Structural Information, Selection of Methods of Analysis. Hardcover 171 pp 0 851 86 800 2 f 12.00 ($26.00) RSC Members f 9.00 No. 7 Analysis of Airborne Pollutants in Working Atmospheres The Welding and Surface Coatings Industries by J. Moreton and N. A. R. Falla This Monograph covers the following: Part I The Welding Industry: Airborne Pollutants in Welding; Sampling of Welding Workshop Atmospheres; Analysis of Welding Fumes and Pollutant Gases.Part II The Surface Coatings Industry: Origin of Airborne Pollutants in the Surface Coatings Industry; Collection and Analysis of Gaseous Atmospheric Pollutants in the Surface Coatings Industry; Collection and Analysis of Particulate Atmospheric Pollutants in the Surface Coatings Industry; Future Trends Relating to Sampling and Analysis in the Welding and Surface Coatings Industries. Hardcover 192pp 0 85186 860 6 f15.00 ($32.00) RSC Members f12.00 No. 8 The Sampling of Bulk Materials by R. Smith and G. V. James The literature of analytical chemistry exhaustively covers the many techniques now available to the analyst. feature common t o all analyses, is in contrast only sparsely documented. Comparatively few original papers on this subject have been published in the last fifty years; there are very few reviews available, and perhaps as a result sampling is badly neglected i n most instructional courses i n analytical chemistry.This Monograph will go some way towards filling a gap in the literature and should stimulate interest in the development of sampling as a field of study. Brief Contents Introduction; Glossary of Terms; Establishment of a Sampling Scheme; Sampling Theories; Apparatus for Sampling; Sampling Methods; Appendices 1-4. Hardcover 200pp 0 851 86 81 0 X f16.50 ($35.00) RSC Members f10.75 Orders: RSC Members should send their orders to: The Membership Officer, The Royal Society of Chemistry, 30 Russell Square, London WC1 B 5DT All other orders should be sent to: The Royal Society of Chemistry, Distribution Centre, Blackhorse Road, Letchworth, Herts.SG6 1 HN Sampling, the one The Royal Society of ChemistryPUBLICATIONS RECEIVED 501 October, 1982 Cobalt in Potable Waters 1981. Pp. 22. 1982. Price L2.40. ISBN 0 11 751603 1. Cadmium, Chromium, Copper, Lead, Nickel and Zinc in Sewage Sludges by Nitric Acid/AAS 1981. Pp. la. 1982. Price i1.85. ISBN 0 11 751615 5. Collaborative Interlaboratory Studies in Chemical Analysis. Lectures Presented at the International Symposium on Harmon- ization of Collaborative Analytical Studies, Helsinki, Finland, 20-21 August 1981. Edited by H. Egan and T. S. West. IUPAC Symposium Series. Pp. xiv + 171. Pergamon. 1982. Price $40; L20. ISBN 0 08 026228 7. The papers presented in this volume are mini- mally edited versions of most (29) of those de- livered at a Symposium organised jointly by the Analytical Chemistry Division, the Applied Chemistry Division and the Clinical Chemistry Division of IUPAC.The Symposium con- sidered the role and design of collaborative studies, with special reference to analytical parameters which are important in the valida- tion and intercomparison of methods (e.g., accuracy, precision, reproducibility), and the definition and practical interpretation of such parameters. National and International organ- isations interested in the development and use of standard methods were represented and were able to exchange the benefit of their experience in this field. An index is included which features the parameters that require discussion and the key bodies and committees involved with the subject at present.Dynamische thermische Analysenmethoden Kalus Heide. Pp. 324. VEB Deutscher Ver- lag fur Grundstoffindustrie. 1982. Price DM48. Bestell-Nr. 541 330 0. (In German.) This book appears to be a reprint of a book published in 1979. Chemische Thermodynamik. Gert Wolf and Wolfgang Schneider. Pp. 262. VEB Deutscher Verlag fur Grundstoffindustrie. 1982. Price DM27. Bestel-Nr. 541 405 5. (In German.) International Conference on Industrial Inorganic Elemental Analysis, Metz 1-5 June 1981. Conference Proceedings. Edited by J . Lee-Frampton. Pp. ii + 158. Philips. 1982. Price $25. This publication contains summaries of all the papers presented, the invited papers and a selection of the submitted papers, in English and the language of origin.Proceedings of the Seventeenth Annual Meeting of the National Council on Radia- tion Protection and Measurements, held on April 8-9, 1981 at the National Academy of Sciences, Washington, D.C. Proceedings No. 3. Critical Issues in Setting Radiation Dose Limits. Pp. vi + 287. National Council on Radiation Protection and Measurements. 1982. Price $15. ISSN 0195 7740. This is the third of a series initiated by the Council in 1980 as part of its effort to dissemi- nate information about radiation protection and measurement. Eleven scientific papers are included, together with the opening remarks and the Fifth Taylor Lecture, all of which address the subject of “Critical Issues in Setting Radia- tion Limits” from different points of view.Benzodiazepines. A Handbook. Basic Data, Analytical Methods, Pharmaco- kinetics and Comprehensive Literature. Harald Schutz. Pp. xii + 439, Springer- Verlag. 1982. Price DM198; $88.00. ISBN 3 540 11270 7 ; 0 387 11270 7. The “Analytical Data” section of this book gives a comprehensive collection of data, e.g., general and chromatographic as well as spectral, of 19 commercial preparations, 23 important metab- olites and 18 hydrolysis derivatives. Informa- tion about biotransformation and the possible formation of aminobenzophenone derivatives is also given. The most important analytical methods are then presented in a review, in order to make it possible to select the optimum method on the basis of essential data. Another review and set of diagrams facilitate the interpretation of quantitatively determined blood, plasma or serum concentrations.A review of literature and list of references deals with analytical methods and pharmacokinetics in literature that has appeared since the early 1960s. Column Selection in Gas Chromatography. Audio Course. Harold M. McNair. Professional Development Courses (Catalog No. 66). Four audiotape cassettes (4.2 hours) + 140 pp. manual. American Chemical Society. 1982. Price $265; additional manuals $16. The selection of the proper column and column operating parameters determines the effective- ness of gas-chromatographic separations. This course emphasises the selection process from both a theoretical and practical point of view. Topics discussed include criteria for evaluating and choosing liquid phases, the most commonly used liquid phases, the criteria for choosing502 PUBLICATIONS RECEIVED Anal.PYOC. solid supports and the results that can be obtained. Column operating parameters such as flow-rate, temperature, length, diameter and per- centage liquid loading are also discussed. While a short set of problems follows most sections of the course, no background in higher mathe- matics is required. Previous experience in gas chromatography is not essential for this course. An outline of the course is : Introduction and Definitions ; Selecting the Liquid Phase ; Classi- fying Liquid Phases by McReynold’s Constants; Solid Supports ; Simplified Theory ; Column Operating Parameters ; Open Tubular Columns (Capillary Columns) ; Porous Polymers ; Ad- sorbents; Literature Sources; List of Suppliers ; and Guide to Silicone Liquid Phases.Pyrolysis Mass Spectrometry of Recent and Fossil Biomaterials. Compendium and Atlas. Henk L. C. Meuzelaar, Johan Haverkamp and Fred D. Hileman. Techniques and Instru- mentation in Analytical Chemistry, Volume 3. Pp. xiv + 293. Elsevier. 1982. Price $67.50; Dfl145. This book presents a discussion of basic prin- ciples (including sample requirements, short- and long-term reproducibility problems and data processing approaches) of pyrolysis - mass spectrometric (Py - MS) techniques. The Compendium of Basic Principles and Applications (Part I) has been put together by authors who have been involved in an extensively used fully automated Py-MS system. The advent of commercially available Curie-point Py - MS systems has prompted the authors to include a small Atlas of Selected Pyrolysis Mass Spectra (Part 11) of over 150 reference spectra of carefully selected biomaterials which should help users of these systems to “tune” their instruments to the existing systems and to evaluate unknown spectra.Examples of applications of the system and the analysis and data processing of biomaterials, such as bio-polymers, natural products, drugs, humic substances, geochemical materials and bacteria, are included. ISBN 0 444 42099 1. Methods of Biochemical Analysis. Volume 28. Edited by David Glick. Pp. x + 430. John Wiley. 1982. Pricek35. ISBN 0471 083704. This volume is in a review series designed to meet the need in the field of biochemical analysis.The topics to be included in the series are chemical, physical, microbiological and animal assays, as well as basic techniques and instrumentation for the determination of enzymes, vitamins, hormones, lipids, carbo- hydrates, proteins, etc. The reviews in Volume 28 are : Acquisition and Interpretation of Hydro- gen Exchange Data from Peptides, Polymers, and Proteins; Phase Partition-A Method for Purification and Analysis of Cell Organelles and Membrane Vesicles ; Detection of Ligand- induced and Syncatalytic Conformational Changes of Enzymes by Differential Chemical Modification ; Adaptation of Polarographic Oxygen Sensors for Biochemical Assays ; Visual Biochemistry : New Insight into Structure and Function of the Genome; The Use of Magnetiz- able Particles in Solid Phase Immunoassay ; Characterization, Assay, and Use of Isolated Bacterial Nucleoids; Analysis of the Cross- linking Components in Collagen and Elastin.There is also a cumulative author and a cumu- lative subject index for Volumes 1-28. Basic Facts, Chemistry W. A. H. Scott. Collins Gem. Pp. iv + 251. Collins. 1982. Price E1.50. ISBN 0 00 45887 8. Trace Analysis. Volume 1. Edited by James F. Lawrence. Pp. x + 331. Academic Press. 1981. Price k26.20; $39.50. ISBN 0 12 682101 1. Trace Analysis is a multi-volume publication intended to bring together detailed applications of analytical chemistry to the detection, identi- fication and quantitation of trace amounts of substances in many different sample types. Volume 1 is devoted to state-of-the-art critical discussions of selected topics in the use of HPLC for both organic and inorganic trace analysis.The first article deals with an assess- ment of liquid chromatographic methods for the determination of trace organics in aqueous environmental samples. This is followed by a discussion, both theoretical and practical, of the various types of electrochemical detectors avail- able for liquid chromatography. There is then a discussion of recent trends in the separation and determination of metal species by ion exchange and chelation. There is an article on liquid chromatographic analysis of mycotoxins , and the final article is devoted to applications of ion chromatography in trace analysis, particu- larly of anions. Details are given on the ration- ale for the ion-chromatographic technique, descriptions of the various components and actual sample applications. Two - Dimensional Nuclear Magnetic Resonance in Liquids. Ad Bax. Pp. vi + 200. D. Reidel Publishing Co. 1982. Price Dfl170; $29.50. ISBN 90 277 1412 6.October, 1982 CONFERENCES AND MEETINGS 503 Two-dimensional NMR spectroscopy is an experimental method of particular importance to those concerned with the assignment of homo- nuclear (lH) or heteronuclear ( 13C) coupled spins. The three main categories of two- dimensional Fourier transform spectra-shift correlation, J - and multiple quantum spectro- scopy-are examined in detail, and their theory is presented in a manner that will enable chem- ists to use the work as a practical guide to the use of two-dimensional techniques. The book includes a survey of the different two- dimensional experiments now available, to- gether with details of their applicability and practical limitations, followed by a short discus- sion of the spectrometer requirements necessary for performing two-dimensional experiments.

ISSN:0144-557X    

DOI:10.1039/AP9821900496

出版商:RSC    

年代:1982

数据来源: RSC

摘要:

October, 1982 CONFERENCES AND MEETINGS 503 Conferences and Meetings 1983 Pittsburgh Conference and Exposition on Analytical Chemistry and Applied Spectroscopy March 7-12, 1983, Atlantic City, NJ, USA The Symposia already organised for the 1983 conference will be on the following subjects: Science and Technology-Their Roles in Socio- logical Development ; Advances in Thin-layer Chromatography ; Chromatographic Instru- mentation ; Electroanalytical Methods and Materials ; Solving the Laboratory Data Management Problem ; Chromatography Tech- niques for the Industrial Hygiene Chemist ; Solid State Mass Spectrometry; Atomic Spectroscopy-Where Next ? ; Deconvolution and Resolution Enhancement in Instrumental Analysis; New Techniques in the Diagnosis of Cancer ; Advances in Laser Spectroscopy ; Practical Applications of Capillary Gas Chroma- tography Columns ; Surface Measurement Tech- niques on the Horizon; and Advances in Luminescence Spectroscopy.For information about the Conference write to Pittsburgh Conference, 437 Donald Road, Pittsburgh, PA 15235, USA. SAC 83 July 17-23, 1983, Edinburgh This conference, which is being organised by the Analytical Division of the Royal Society of Chemistry, is to be held at the University of Edinburgh. The Plenary Lectures will be as follows : “Capillary Separation Techniques : A Key to Future Improvements in Resolution and Sensitivity,” by Professor M. V. Novotny (Indiana University, USA) ; “Continuum Source Atomic-absorption Spectrometry : Past, Present and Future Prospects,” by Professor T.C. O’Haver (University of Maryland, USA) ; “Design and Application of Neutral Carrier- based Ion Selective Electrodes,” by Professor W. Simon (Eidgenossiche Technische Hoch- schule, Switzerland) ; and “Photoluminescence and Chemiluminescence Analysis : Recent Developments and Future Prospects,’’ by Professor J . N. Miller (Loughborough University, UK). In addition to these, the invited lecturers include F. Adams, L. S. Bark, J. Beynon, A. L. Gray, S. Greenfield, C. J. Keattch, A. C. Moffat, J. Ruzicka and D. R. Williams. Contributed papers and posters are sought on all aspects of analytical chemistry. The themes will include atomic spectrometry, automation, biochemical methods, chromatography, data processing, electroanalysis, electrophoresis, enzyme techniques, historical, immunoassay, industrial, mass spectrometry, microanalysis, microcomputers, microprocessors, molecular spectroscopy, photoacoustic spectrometry, probe methods, process control, quality control, radiochemistry, sample pre-treatment, separa- tion processess, thermal methods and X-ray methods.Lectures will last for 20 min (with 5 min more for discussion) while posters will be on display all day (author to be present for a speci- fied period of 1 h). Those wishing to present a lecture (on unpublished original work) should send a title and 200-word abstract to Dr. A. M. Ure, SAC 83 Scientific Secretary, c/o Analytical Division, Royal Society of Chemistry, Burlington House, London, W 1V OBN, by November 30, 1982. The remainder of the scientific programme consists of small group symposia (organised by special interest groups), update courses and workshops. In addition there will be an exhibition and a comprehensive social pro- gramme. For further information on the conference contact Miss P. E. Hutchinson, Secretary of the Analytical Division, Royal Society of Chemistry, Burlington House, London, W1V OBN.

ISSN:0144-557X    

DOI:10.1039/AP9821900503

出版商:RSC    

年代:1982

数据来源: RSC

摘要:

504 ANALYTICAL DIVISION DIARY Anal. Proc. Analytica I Division Diary OCTOBER Putting a Byte into Analytical Wednesday, 20th, 1.45 p.m.: Man- Chester North West Region. Advances in NMR Spectroscopy. "NMR in Solution: New Methods of Deter- mining Structure and Conformation," by J. K. M. Sanders. "High Resolution NMR in Solid Materials," by Professor R. K. Harris. "Topical NMR and Imaging," by D. Shaw. "Industrial Applications of Multi-nuclear NMR," by A. M. Chippendale. Research Department, ICI PLC, Organics Division, Blackley, Manchester. Registration is necessary. Cost f 4 to members of RSC/AD; f 5 to members of RSC; f 6 to non-members; free to full-time students and retired members. Contact; Dr. A. Mathias, ICI PLC, Organics Division, Blackley, Man- Chester, M9 3DA. Thursday, 21st, 4 p.m.: Belfast Northern Ireland Region. Ion Pairing : A Marriage of Analytical Convenience. Speaker: Professor D. Thorburn Burns. Annual General Meeting: approximately 5.15 p.m. Room 246, Chemistry Department, The Queen's University, Belfast. Registration is not necessary. Contact: Mr. W. J. Swindall, Department of Chemistry, David Keir Building, Queen's University, Belfast, BT9 5AG. (Tel. 0232-661 1 1 1, Ex. 4428). Friday, 22nd, 6 p.m. : Chepstow Western Region. Flow Injection Analysis. Discussion meeting introduced by Professor D. Two Rivers Hotel, Chepstow. Registration is not necessary. Contact; Mr. F. W. Sweeting, Wessex Water Authority, P.O. Box 95, The Ambury, Bath, BAI 2YP. (Tel. 0225- 31 3500) Betteridge. Tuesday, 26th, 4.30 p.m.: Edinburgh Scottish Region, jointly with the South East Scotland Section of the RSC and the Edinburgh University Chemical Society.Chemistry. Speaker: R. M . Smith. Chemistry Department, King's Buildings, The University, Edinburgh. Registration is not necessary. Contact: Dr. A. F. Fell, Department of Pharmacy, Heriot-Watt University, 79 Grassmarket, Edinburgh, EHI 2HJ. (Tel. 031 -225-8432, Ex. 225). Thursday, 28th, 11 a.m. : London Violet Spectrometry Group. Analytical Division, jointly with the Ultra Recent Advances in Absorption and Luminescence Techniques and Silver Medal Lecture. "Recent Advances in UV Spectrometry," by A. J. Everett. "Photoacoustic Spectroscopy and Imaging," by Professor G. F. Kirkbright. Silver Medal Lecture: "Sensitive and High Resolution Analytical Techniques in Clinical Chemistry," by L.J. Kricka. "Recent Advances in Chiroptical Spectroscopy," by Professor S. F. Mason, FRS. "Recent Advances in Luminescence Techniques," by Professor J. N. Miller. Scientific Societies Lecture Theatre, 23 Savile Row, London, W.1. Registration is necessary. Cost f 1 0 to members of RSC and UV Spectro- metry Group; f 1 3 to non-members. Contact: Miss P. E. Hutchinson, Analytical Division, Royal Society of Chemistry, Burlington House, London, WIV OBN. (Tel. 01 -734 9971 ). NOVEM BE R Wednesday, 3rd, 10 a.m. : Nottingham Midlands Region. Using Microcomputers in the Analytical Laboratory. The aim of the seminar is to provide participants with an indication of the use of micro- computers in the laboratory. During the afternoon there will be an opportunity to see working demonstrations, to discuss problems and applications with equip- ment suppliers and users who have utilised microcomputers for data collec- ting and processing or for control pur- poses.[continued on p. 505October, 1982 ANALYTICAL DIVISION DIARY 505 Analytical Division Diary, continued November, continued "Introduction to Microcomputers and Their Use "Interfacing Microcomputers to Analytical Instru- "Use of Low Cost Robot Arms for Automation "Interfacing a Microcomputer to an Atomic "Using a PET as a Chromatography Integrator," Trent Polytechnic, Clifton, Nottingham. Registration is necessary. Cost f12 to RSC members, f 2 0 to non-members and f 8 to students. Contact: Dr. A. Braithwaite, Depart- ment of Physical Sciences, Trent Polytechnic, Clifton, Nottingham, N G l l 8NS.(Tel. 0602-48248, Ex. 3252 or 31 74). in the Laboratory," by A. Braithwaite. ments," by D. J. Malcolme-Lawes. of Laboratory Processes," by T. B. Pierce. Absorption Instrument," by P. B. Smith. by M. Elphick. Thursday, 4th, 9.1 5 a.m. : London Automatic Methods Group, jointly with CoPharm (Pharmaceutical Industry and Schools of Pharmacy Co-operative Discussion Group). Automatic Methods in Pharma- ceutical Production and Analytical Laboratories. "On-line Data Capture," by K. Rutherford. "Automation of Physical Methods," by P. Cobb. "Automation of Dissolution Tests," by P. Gould. "Will Robots Ever Wear White Coats?" by M. "Production Documentation by Computer," by "Automation of Autoclaves," by B. Kirk."Automatic Sterilization Tech n iq ues," by a speaker from Beckton Dickinson. "Instrumental Process Control," by P. Ridgeway- Watt. London Tara Hotel, Scarsdale Place, London, W.8. Registration is necessary. Contact: Dr. C. J. Jackson, Health and Safety Executive, Occupational Hygiene Laboratory, 403 Edgware Road, London, NW2 6LN. (Tel. 01- Thursday, 4th, 10.30 a.m. : Bristol White. J. Goldsmith. Cost f 30. 450-891 1, EX. 227). Western Region and Atomic Spectro- Current Awareness Symposium on Electrothermal Atomisation in Analytical Atomic Spectroscopy. Although electrothermal atomization is a well established technique, it is subject to chemical interferences and other scop y Group. matrix effects when applied to a number of sample materials. This has stimulated considerable research in an effort to overcome many of the problems en- countered with 'first generation' instru- ments. As a result, developments have been made in the design and application of graphite tube atomisers in analytical atomic spectroscopy.Speakers at the symposium will review the current 'state of the art' and assess the importance of recent advances to practical analysis. Delegates will have the opportunity to discuss the relevance of these develop- ments to their own problems. "Electrothermal Atomisation Comes of Age," by J. M. Ottaway. " Developments in Background Correction," by J. B. Dawson. "The Modern Platform Furnace and Zeeman Background Correction," by W. Slavin. "Clinical Applications of Electrothermal Atomisa- tion," by H. T. Delves. "Electrothermal Atomization in the Chemical Industry," by R.C. Hutton. "The Future for Electrothermal Atomisation- Hybrid Techniques," by L. Ebdon. School of Chemistry, The University' Bristol. Registration is necessary. Cost f15 to RSC members, f20 to non-members and f5 to students. Contact: Mr. F. W. Sweeting, Wessex Water Authority, P.O. Box 95, The Ambury, Bath, Avon, BAI 2YP. (Tel. 0225-31 3500, EX. 385). Tuesday, 9th : London Biological Methods and Joint Pharma- ceutical Analysis Groups. Drug Delivery Systems. Pharmaceutical Society of Great Britain, 1 Lambeth High Street, London, S.E.I. Contact: Miss I. Ladden, British Pharma- copoeia Commission, Market Towers, 1 Nine Elms Lane, London, SW8 5NQ. (Tel. 01 -720-9844, Ex. 31 05). Wednesday, 10th : Sheff ield Electro analytical Group.Young Persons' Meeting. The Polytechnic, S heff ield. Contact: Mr. A. E. Bottom, Kent Industrial Measurements Ltd., EIL Analytical Instruments, Hanworth Lane, Chertsey, Surrey, KL16 9LF. (Tel. 093-28- 62671 ). [continued on p. 506506 ANALYTICAL DIVISION DIARY Anal. PYOC. Analytical Division Diary, continued November, continued Wednesday, 1 Oth, 10.30 a.m. : Graves- end Radiochemical Methods Group: Annual General Meeting; 2 p.m. Radiochemical Analysis. "The Advantages of Using Radioisotopes in Analysis-A Review," by G. W. A. Newton. "Computer Based y-ray Spectrometry," by L. Salmon. "Measurement of a- and /3-activity," by J. N. Barnes and K. J. Odell. "Applications of Radiochemistry in Analysis: A Review of Some Recent Work," by S.J. Lyle. "The Determination and Uses of Some Natural Radionuclides," by J. Eakins. l o u r of the CEGB Laboratories. CEGB, Canal Road, Gravesend, Kent. Registration is necessary. Cost f4. Contact: Dr. A. R. Ware, Scientific Services Centre, CEGB, Canal Road, Gravesend, Kent, DA12 2RS. (Tel. 0474-51 122). Thursday, 11 th, 5.30 p.m. : Liverpool North West Region, jointly with the Liverpool Polytechnic Students Chemi- cal Society. Archaeological Chemistry. Speaker: M. Hughes. The Polytechnic, Byrom Street, Liver- Registration is necessary; no charge. Contact: Mr. J. Aspinall/Dr. C. G. Taylor, Department of Chemistry, Liverpool Polytechnic, Byrom Street, Liverpool, Merseyside. pool. Thursday and Friday, 11th and 12th: StokePoges South East Region and Thermal Methods Group: Annual General Meeting of the Thermal Methods Group.Use of Microprocessors and Com- puters in Thermal Analysis. Guest speaker: Professor D. Betteridge. The meeting will include contributed papers and a visit to Perkin-Elmer as part of their anni- versary celebrations of 25 years in this country. Fulmer Grange, Stoke Poges, Bucks. Registration is necessary. Cost for resi- dents f60 to RSC members and f70 to non-members; non-residents f35 to RSC members and f40 to non- members. Contact: Dr. R. H. Still, Department of Polymer and Fibre Science, UMIST, SackvilleStreet, Manchester, M60 1 QD. (Tel. 061 -236-331 1 ). Friday, 12th, 7.30 p.m. : Scotch Corner North East Region: Annual General Meeting and Social Evening. Scotch Corner Hotel, Nr. Richmond. Contact: Mr.C. L. Denton, 20 Bedford Road, Nunthorpe, Middlesbrough, Cleveland. (Tel. 0642-31 5721 ). Friday, 12th, 5 p.m.: Edinburgh Scottish Region: Annual General Meeting. Catching Criminals with Chromato- graphy * Speaker: A. C. Moffat. Court Room, Heriot-Watt University, Edinburgh. Contact: Dr. A. F. Fell, Department of Pharmacy, Heriot-Watt University, 79 Grassmarket, Edinburgh, EHI 2HJ. (Tel. 031 -225-8432, Ex. 225). Wednesday, 17th, 10 a.m. : Liverpool Liverpool Section of the RSC. North West Region, jointly with the Recent Developments in Analytical Aspects of Chemical Oceanography. Chairman's introduction by Professor J. P. Riley. "Comparability of Analytical Data and Associated Problems," by G. Topping. "Trace Elements in Sea Water: Recent Work on Occurrence and Distribution," by J.D. Burton. "The Role of Electrochemical Techniques in Marine Chemistry," by M. Whitfield. "Metal Speciation in Sea Water," by C. M. G. van den Berg. "A Microcomputer-controlled Alkalinity Titra- tion-Methods and Results," by T. R. S. Wilson. "Determination of Very Small Concentrations of Radioisotopes in Sea Water," by C. W. Baker. Lecture Theatre 'D', University Lecture Rooms Building, The University, Liver- Registration is necessary. Cost f10 to RSC/AD members, f12 to RSC mem- bers, f 15 to non-members and f5 to retired members and students. Addi- tional cost : lunch f 5. Contact: Mr. G. Davison, Kodak Ltd., Chemical Division, Research Depart- ment, Acornfield Road, Kirkby, Mersey- side. (Tel. 051 -546-21 01, Ex. 127). pool. [continued on p.507October, 1982 ANALYTICAL DIVISION DIARY 507 Analytical Division Diary, continued November, continued Wednesday, 17th, 6.30 p.m. : London Microchemical Methods Group: Annual The Integrity of the Sample During A na I ysis . Discussion to be introduced by J. F. Savoy Tavern, Savoy Street, London, Registration is not necessary. Contact: Mr. P. R. W. Baker, Department of Physical Chemistry, Wellcome Research Laboratories, Langley Court, Beckenham, Kent, BR3 3BS. (Tel. General Meeting . Wool ley. w.c.2. 01 -658-221 1, EX. 357). Friday, 19th, 7.30 p.m. : Preston North West Region, jointly with the Preston Polytechnic C hem ica I Society. Concurrent talks for the Ladies and for scientific members. "Microwave Cooking," by Mrs. J. Outlaw. "Electricity for the Future," by C.A. Stoddart. The Polytechnic, Corporation Street, Registration is necessary. Contact; Dr. J. D. Hepworth, Department of Chemistry, Preston Polytechnic, Corporation Street, Preston, Lancs. Preston, Lancs. Cost f 4. Wednesday, 24th, 10 a.m. : Leeds North East Region. Applications of Chromatography in Water Analysis. Speakers to include: R. Newton, Dr. Crathorne, Leeds. Contact: Mr. C. L. Denton, 20 Bedford Road, Nunthorpe, M iddlesbroug h, Cleveland. (Tel. 0642-31 5721 ). G. Wardell, I. Wilson and C. Hays. Thursday, 25th, 10 a.m.: Sharnbrook Midlands and East Anglia Regions with the Microchemical Methods and Joint Pharmaceutical Analysis Groups: Annual General Meeting of the East Anglia Region; 1.45 p.m. Modern Techniques and Applica- tions in Immunoassay.lmmunoassays are widely used for sensitive analyses in clinical chemistry, and are increasingly being applied in veterinary medicine, forensic toxicology, sports medicine and agricultural chemistry. This meeting will cover the fundamental aspects of modern isotopic and non-isotopic immunoassays and describe a wide variety of interesting applications. It will be of interest to students of analytical chemistry as well as to users of immunoassay methods. "The Background to Immunoassay," by Professor J. N. Miller. "The Production of Antisera for lmmunoassay," by B. A. Morris. "Aspects of ELISA," by A. Crimes and Professor C. H. S. Hitchcock. "Chemiluminescence Immunoassay," by J. S. Woodhead. "Radioimmunoassay in Forensic Science," by R. N. Smith. "Radioimmunoassay and Steroid Drugs in Sport," by Professor R. V. Brooks. Unilever Research, Colworth House, Sharnbrook, Bedford. Registration is necessary. Cost f 1 0 for RSC members, f15 for non-members. Contact: Mr. G. M. Telling, Unilever Research, Colworth House, Sharn- brook, Bedford. (Tel. 0234-781 781 ). Thursday, 25th, 4 p.m. : Glasgow Scottish Region, jointly with the South West Scotland Section of the RSC and the Andersonian Society. Chemistry of the Firth of Clyde. Speakers: B. Miller and A. J. Newton. Staff Centre, University of Strathclyde Glasgow. Contact: Dr. A. F. Fell, Department of Pharmacy, Heriot-Watt University, 79 Grassmarket, Edinburgh, EHI 2HJ. (Tel. 031 -225-8432, Ex. 225). Thursday, 25th, 5 p.m. : Cardiff Western Region, jointly with the South East Wales Section of the RSC and UWIST Student Chemical Society. The Analysis of Additives and Resi- dues in Plastic Materials. Speaker: D. C. M. Squirrell. UWIST, Cardiff. Contact: Mr. F. W. Sweeting, Wessex Water Authority, Bristol Avon Division, P.O. Box 95, The Ambury, Bath, BAI 2YP. (Tel. 0225-313500, Ex. 385).

ISSN:0144-557X    

DOI:10.1039/AP9821900504

出版商:RSC    

年代:1982

数据来源: RSC