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Proceedinas - - - - - - -of the Analytical Division ofThe Chemical SocietyCONTENTS49 SAC GoldMedal50 SAC Silver Medal52 AD Distinguished Service Award52 Reports of Meetings53 Summaries of Papers53 'Standards'54 'Training Graduates in Analytical57 Safety in Analytical Laboratories:Chemistry'Code of Practice for Use of GasCylinders61 Equipment News65 Rank Hilger Spectroscopy Prize66 Fourth SAC Conference68 Society for Analytical Chemistry68 Courses68 Conferences and Meetings70 Analytical Division DiaryEGMVolume 14 No 3 Pages 49-70 March 197March 1977 PADSDZ 14(3)49-70(1977)ISSN 0306-1 396PROCEEDINGSANALYTICAL DIVISION OF THE CHEMICAL SOCIETYOF THEOfficers of the Analytical Divisionof the Chemical SocietyPresidentD. W.WilsonUon. SecretaryP. G. W. CobbSecretaryMiss P. E. HutchinsonUon. Treasurer Hon. Assistant SecretariesJ. K. Foreman D. 1. Coomber, O.B.E.; D. C. M. Squirrel1Editor, ProceedingsP. C. WestonProceedings is published by The Chemical Society.Editorial: The Director of Publications, The Chemical Society, Burlington House, London, W1 V OBN.Telephone 01 -734 9864. Telex 268001.Subscriptions (non-members): The Chemical Society, Publications Sales Office, Blackhorse Road,Letchworth, Herts., SG6 1 HN.Non-members can only be supplied with Proceedings as part of a combined subscription with The Analystand Analytical Abstracts,0 The Chemical Society 1977SCOTTISH REGION MEETINGIntensive Course onat theWolfson Liquid Chromatography UnitDepartment of Chemistry, University of EdinburghonThursday and Friday, 9th and 10th June, I977A two-day Intensive Course on the practice of modern liquid chromatography willbe run in association with Professor J.H. Knox and leading equipment manufac-turers. The principles, equipment and applications in clinical, pharmaceutical andindustrial analysis will be covered in lectures and discussion groups.Practical sessions on column packing and testing, with manufacturers' experi-ments using the most recently developed equipment, will be based on small groups,limiting the maximum number of participants to 48.If demand is sufficient, a second, identical course will follow on Tuesday andWednesday, 14th and 15th June, 1977.For application forms and further information contact: Dr J. E. Whitley, ScottishUniversities Research and Reactor Centre, East Kilbride, Glasgow G75 OQU.HIGH-PERFORMANCE LIQUID CHROMATOGRAPH

ISSN:0306-1396    

DOI:10.1039/AD97714FX009

出版商:RSC    

年代:1977

数据来源: RSC

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March, 19 77 ANALYTICAL DIVISION DIARY 69Analytical Division Diary, continued Thursday, 14th-APRILFriday, lst, 3.30 p.m.: CardiffWestern Region.“Advances in ESCA for the Determinationof Chemical Species and Oxidation States,”by Professor D. M. Hercules.UWIST, Cardiff.Friday, lst, 2 p.m.: ChorleyNorth West Region, jointly with the Associ-ation of Public Analysts, on “PracticalAnalysis of Carbohydrates .”“Novel Syrups in the Starch Industry andthe Problems they Present to the Analyst,”by G. Stafford.“New Approaches to Carbohydrates Analysisin Food,” by Professor S. A. Barker.“Analytical Implications of the EEC Direc-tive on Sugar Products,” by R. S. Kirk.Heskin Hall, Chorley, Lancs.Wednesday and Thursday, 13th and 14th:LondonElectroanalytical Group on “ElectroanalysisWednesday 13th-Plenary Lecture : “Polarographic Methodsfor Use in Biological Systems,” by P.Zuman.“Cathodic Stripping Voltammetry Studiesof Sulphur-containing Compounds in Bio-logical Fluids,” by I.Davidson.“Continuous Measurements of Blood GasTension-The Current Status,” by D.Parker.“The Uses and Limitations of Polarographyin Determining Plasma Drug Levels inPre-clinical Pharmacology,” by J. Clifford.“The Use of Non-invasive Methods in BloodGas Analysis,” by I. Fatt.in Biological Fluids.”Plenary Lecture : “The Virtues and Limita-tions of Ion-selective Electrodes forMeasurements in Biological Systems,” byR. P. Buck.“Measurement of Plasma Potassium UsingIon-selective Electrodes,” by D.Band.“Microelectronic Ion-selective Electrodes,”by D. Owen.“Ion-selective Electrodes for BiomedicalApplications,” by J. D. R. Thomas.“Problems of Redox Measurements in CellPhysiology,” by J. Chayen.‘‘Selective Electrodes in Clinical Chemistry,”by M. Brand.Chelsea College, Manresa Road, London,s.w.3.Thursday, 14th, 10.30 a.m. : CambridgeRadiochemical Methods Group on “IsotopesInorganic Laboratories, The University, Cam-in Inorganic Chemistry.”bridge.Thursday, 21st, 2.30 p.m.: LondonBiological Methods Group.Discussion on “The Compendium of Standardsfor Biological Medicinal Products,” pre-sented by a panel of speakers from theDepartment of Health and Social Securityand the National Institute of BiologicalStandards and Control, headed by J.A.Holgate.National Institute for Biological Standardsand Control, Holly Hill, Hampstead,London, N.W.3.Friday, 22nd, 4 p.m.: PooleWestern Region.“Parts per Thousand Million,” by B. Poole.BDH Staff Club, Poole, DorsetAnalytical Division DiaryMARCHFriday and Saturday, 25th and 26th:Pitlochr yScottish and North East Regions on “TheMeasurement and Toxicity of Metallic andOrganic Species.”Friday, 25th, 9.30 a.m.-Plenary Lecture : “Metal Specific Detectors forChemical Speciation Studies,” by J. E. VanLoon.“Detection, Identification and Estimation ofOrganochlorine Compounds in the Environ-ment,” by A. V. Holden.“Determination of Trace Metals in Single CellProtein,” by S. G. Farrow and G. B. Fish.“Industrial Toxicity with Particular Refer-ence to Lead and Organic Compounds,” byC.Toothill.“The Transport and Storage of Trace Metalsin Animals,” by I. Bremner.“Uptake and Storage Mechanisms of HeavyMetals in Marine Organisms,” by T. L.Coombs.“The Measurement and Effect of Sub-lethalLevels of Some Heavy Metals on MarineLife in Simulated Marine Ecosystems,” byG. Topping.“Determination of Gold in Biological Fluidsand Tissues by Atomic-absorption Spec-trometry Using Carbon Furnace Atomisa-tion,” by H. Kamel, D. H. Brown, J. M.Ottaway and W. E. Smith.“The Application of Mossbauer Spectroscopyto Environmental Studies,” by B. Goodman.Scotland’s Hotel, Pitlochry.Saturday, 26th, 9.30 a.m.-Visit to the Freshwater Fisheries Laboratory,Faskally .Monday, 28th, to Friday, April 1st: LondonWednesday and Thurs-day, 30th and 31st: Analytical DivisionSymposia.Wednesday, 30th, 9.30 a.m.: History ofA nalytical Chemistry-“History of American Analytical Chemistry,”by R.Belcher.“From Essaying to Analytical Chemistry,How an Art Became a Science,” byF. SzabadvAry. .CS Annual Congress.“PAS of the Past,” by Miss J. D. Peden.“The Origin and Initial Development ofChemical Microscopy,” by R. H. Nuttall.“Irish Contributions to Analytical Chem-istry,” by D. Thorburn Burns.“Three Hundred Years of British Contribu-tions to Atomic Spectroscopy for ChemicalAnalysis,” by T. S. West.“William Crookes’ Chemical News andAnalysis,” by D. Betteridge.“The History of Organic Reagents,” byW.I. Stephen.Thursday, 31st, 10 a.m.-Sixth Theophilus Redwood Lecture : “Analy-sis with a Purpose,” by D. R. Deans.Modern Methods of Speciation-Chnracterisa-tion of Chemical Sfiecaes-“Metal Specific Detectors for ChemicalSpeciation Studies,” by J. C. Van Loon.“Characterisation of Catalyst Surface Speciesby Electron Spectroscopy,” by D. M.Hercules.“Molecular Emission Cavity Analysis,” byA. Townshend.“FTNMR Spectroscopic Analysis Through thePeriodic Table,” by I. K. O’Neill.“The Application of Electrochemical Meth-ods to the Study of Metal Species in Water,”by B. Fleet.“Characterisation of Materials by X-RayDiffraction,’’ by I. H. Scobey.University College, London.Particle Size Analysis Group, jointly with theMaterials Testing Group of the Institute ofPhysics on “Characterisation of Particles inMatrices .”“Analytical Electron Microscopy,” by G. W.Lorimer.“Microphase Polymer Systems,” by M. J.Folkes.“Measurement with the Quantimet 720,” byA. R. Davey.“Some Technological Applications of AugerElectron Spectroscopy Involving ParticleAnalysis,” by C. T. H. Stoddart.Department of Metallurgy, University ofManchester Institute of Science and Tech-nology, Grosvenor Street, Manchester,M17HS.Wednesday, 3Oth, 2 p.m. : ManchesterWednesday, 30th, 11 a.m.: LondonElectroanalytical Group, jointly with theElectrochemistry Group of the FaradayDivision, on “Students’ Research Papers.”Imperial College of Science and Technology,South Kensington, London, S.W.7.[continued inside back coverPrinted by Heffers Printers Ltd Cambridge Englan

ISSN:0306-1396    

DOI:10.1039/AD97714BX011

出版商:RSC    

年代:1977

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Vol. 14 No. 3 March 1977 of the Analytical Division of the Chemical Society Society for Analytical Chemistry Gold Medal As announced in the February issue of Proceedings (p. 19), the twelfth Society for Analytical Chemistry Gold Medal has been awarded to Professor T. S. West. Professor T. S . West was born in Peterhead, Aberdeenshire on November 18th, 1927, and received his secondary education at the Royal Academy, Tain, Ross-shire, where he developed an intense interest in the chemistry and physics side of science.As a winner of the 1945 Highlands and Islands Bursary competition he was able to go to Aberdeen University to study chemistry, mathematics, physics and geology. He graduated with 1st Class Honours in Chemistry in 1949 and proceeded to do his PhD work on analytical chemistry at the University of Birmingham under Professor R.Belcher, who had aroused his interest in this branch of chemistry during his period as lecturer on the staff at Aberdeen University. Following the completion of his PhD research programme on titrants based on (a) unusual valency states and (b) the determination of water, he was awarded a DSIR Research Fellowship to work with Professor Belcher on the ultramicro-analysis of organic compounds.He often reflects on how he was able to get married and start his family on the stipend of fI600 p.a. for the 3-year period concerned. During this time he undertook the construction of a quartz-fibre ultramicro-balance and the development of handling techniques. He was responsible, with Professor Belcher, for the direction of all of the first group of research students in this area.He was appointed Lecturer in Chemistry at Birmingham Univer- sity in 1955 and was awarded the Meldola Medal of the Royal Institute of Chemistry for 1956- an award considered each year for chemists aged 30 or below whose research work shows most promise. During his time in Birmingham he developed techniques of spectrochemical and electro- chemical analysis in addition to ultramicro- analysis and did a considerable volume of work on the development of chelating agents in trace analysis and chelatometry.He tends to look back on this period as the golden era of analytical chemistry. In 1963 he was appointed to the newly created Readership in Analytical Chemistry at Imperial College of Science and Technology of the University of London and in 1965 to the newly established Chair in Analytical Chemistry.At Imperial College he rapidly built up a large and intensively active research team specialising in the techniques of molecular absorption and fluorescence spectroscopy, elec- trochemistry and separation techniques, but especially in the analytical techniques of atomic spectroscopy, e.g., atomic-fluorescence spectroscopy, non-dispersive fluorescence, resistively heated (electrothermal) atomisation and spectral-line sources.The research group, 49led by Professor West and his team leaders, Drs. R. M. Dagnall, B. Fleet and G. F. Kirk- bright, established a pre-eminent international reputation for their work in analytical chemistry and attracted postgraduate (PhD) research students from all over the world, including Argentina, Australia, Bangladesh, Brazil, Can- ada, Czechoslovakia, Egypt, German Federal Republic, Hong Kong, India, Iran, Iraq, Japan, Kenya, Nepal, New Zealand, Norway, Pakistan, Poland, Singapore, Sri Lanka, South Africa, Spain, Sudan, Syria, Turkey, USA, USSR, Venezuela and Yugoslavia, as well as MSc students from these and other countries. Professor West served on most committees of the Society for Analytical Chemistry and was President of the SAC from 1969 to 1971.He played a decisive role in the forma- tion of the new Chemical Society and in 1972 he became the first Secretary of The Chemical Society and Chairman of its External Relations Board until he resigned the post in 1974 due to protracted visits abroad during that year and other responsibilities.In 1974 he was the third Theophilus Redwood Lecturer of the CS Analytical Division and in the following year he was the recipient of the 1975 Chemical Society Award in Chemical Analysis and Instrumentation. In 1967 he toured South Africa at the invitiation of the SA Chemical Institute and in 1968 he was the CS Travelling Lecturer to Australia and New Zealand.He was the NRC -Nuffield Visiting Lecturer to several Canadian Universities in 1974, and for a short period during the same year held the post of Distinguished Visiting Professor at the University of Florida. In 1976 he was appoin- ted by the Japan Society for the Promotion of 50 SAC MEDALS PYOC. Analyt.Div. Chem. SOC. Science as a visiting lecturer to five Japanese Universities. On the International scene Professor West has served on the Nomenclature Commission of the Analytical Division of IUPAC for many years, eight of them as Secretary. He was elected as the UK representative of the Analytical Division of IUPAC in 1971 on an international vote and was elected Vice-president of the Division in 1975.At the General Assembly of IUPAC in Warsaw in August, 1977, he will become President of the Analytical Division for a period of 4 years. He has also served on five occasions as one of the UK delegates to the IUPAC Council and has been Chairman of the Analytical Sub-committee of the Royal Society’s British National Committee for Chemistry for several years and ex ojicio a member of the main BNC committee.In 1975 he resigned the Chair of Analytical Chemistry at Imperial College to assume the Directorship of the Macaulay Institute for Soil Research in Aberdeen. His association with Imperial College continued through his appoint- ment as Honorary Professor for a further period of 2 years, during which time his respon- sibilities as supervisor for London University registered students is being phased out. Professor West, as twelfth SAC Gold Medallist, says he is very pleased to join such a dis- tinguished company, but particularly to follow in the footsteps of his former supervisor, Professor Ron Belcher, and his eminent spectroscopist predecessor at the Macaulay Institute, Dr. Bob Mitchell. He lives just outside Aberdeen and, although he confesses to missing some aspects of life in London, is very glad he no longer has to commute through its crowds every morning and evening.

ISSN:0306-1396    

DOI:10.1039/AD9771400049

出版商:RSC    

年代:1977

数据来源: RSC

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50 SAC MEDALS PYOC. Analyt. Div. Chem. SOC. Society for Analytical Chemistry Silver Medal As announced in the February issue of Proceedings (p. 19), the fourth Society for Analytical Chemistry Silver Medal has been awarded to Dr J. S. Hislop. John Hislop was born in 1940 in Kirkcaldy, Fife. The majority of his secondary schooling was a t the McLaren High School, Callander, Perthshire, with a short period at Tain Royal Academy.He entered Glasgow University in 1958 and graduated with a BSc in Pure Science (Honours Chemistry) in 1962. This was followed by postgraduate research in the Chem- istry Department of the same University, leading to graduation with the degree of PhD in 1965. The topic of his research, under the supervision of Dr. K. C. Campbell, was radio-tracer studies of catalysed chemical reactions, in particular the poisoning of certain hydrogenation reactions.This initial interest in radio-techniques resulted in his subsequent acceptance in 1965 of a post as Assistant Research Chemist in the Activation Analysis Research Laboratory of Texas A & M University. There, under the leadership of Dr. R. E. Wainerdi, he worked as a member of an international team involved in the development and application of neutron activation analysisMarch, 1977 SAC MEDALS 51 techniques.Dr. Hislop’s main interests were in the application of 14-MeV neutron activation and he was involved in development of a system designed for analysis of the lunar and other planetary surfaces. The experience and oppor- tunities he received during this period have proved invaluable during his subsequent career.In 1967 Dr. Hislop returned to the UK to take up a post as an SSO in the Analytical Sciences Division at Harwell. This Division, headed by Dr. A. A. Smales, conducted research and development into a wide variety of analyti- cal techniques for the atomic energy programme and, more recently and on a commercial basis, for industry and Government.In 1968 Dr. Hislop succeeded Dr. C. A. Baker as head of the team developing y-photon activation analysis. The technique was applied to a wide range of problems originating in the UKAEA and external organisations and successful applica- tions have included the determination of trace amounts of oxygen and carbon in very pure metals, including sodium, and in novel electronic materials.A unique application of the tech- nique was for the determination of fluorine in returned lunar samples. Analysis of this same material for certain other major, minor and trace elements by y-photon activation at Har- well illustrated that the technique had a wider range of applicability than solely for determin- ation of the light elements.This area has been further developed by Dr. Hislop’s team and they have shown that y-activation is particularly suited to determination of certain elements, such as lead and nickel, not readily measured by thermal neutron activation. In addition, in conjunction with high-resolution y-spectro- metry, the technique has been shown to be applicable to multi-element survey analyses of a wide range of geological, biological and environ- mental materials.Dr. Hislop has been invited to present a number of lectures both within the UK and abroad on the Harwell y-activation programme and he gratefully acknowledges the assistance he has received throughout the years from his colleagues in the y-activation section. In 1971 Dr. Hislop was given the additional responsibility of co-ordinating, within the Analytical Sciences Division , the various pro- j ects involved with determination of trace ele- ments in biological materials.This is still one of his main areas of interest and gained increased relevance in 1974 when his section, as part of the Chemical Analysis Group under Mr. H. I. Shalgosky, was combined with the former Health Physics and Medical Division to form the Environmental and Medical Sciences Divi- sion.In 1974 Dr. Hislop’s duties were further extended to include responsibility for a total of seven professional scientists involved in provid- ing analytical support using such techniques as optical spectroscopy, X-ray fluorescence, mass spectrometry and y-activation. He was promo- ted to PSO in July 1976. Dr. Hislop has published about 30 papers on his work, many of which are Harwell research reports, and has lectured a t numerous inter- national conferences in the USA and Europe. He represents Hanvell at various inter-Govern- mental Laboratory Working Parties on analyti- cal methods. Married with two small sons, Dr. Hislop lives in Cold Ash, a small village in the wilds of rural Berkshire. His interests include do-it-yourself maintenance and improvement of his house, bee- keeping and keeping his 1Q acres of garden under control. When time permits he enjoys other outdoor pursuits, including walking and tennis.

ISSN:0306-1396    

DOI:10.1039/AD9771400050

出版商:RSC    

年代:1977

数据来源: RSC

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52 AD DISTINGUISHED SERVICE AWARD Proc. Analyt. Div. Chem. SOG. Reports of Meetings Special Techniques Group The thirty-second Annual General Meeting of the Group was held a t 2.30 p.m. on Wednesday, December lst, 1976, a t Imperial College, South Kensington, London, S.W.7. The Chair was taken by the Chairman of the Group, Dr. P. B. Smith. The following office bearers were elected for the forthcoming year : Chairman- Dr.P. B. Smith. Vice-Chairman-Dr. T. B. Pierce. Honorary Secretary and Treasurer-Mr. J. T. Davies, Research and Development Department, Metal Box Co., Twyford AbbeyMarch, 1977 STANDARDS 53 Road, Park Royal, London, N.W.lO. Members of Committee-Dr. D. H. Christopher, Mr. J. H. Glover, Dr. H. Hughes, Mr. P. Hurley, Dr. R. P. Mounce and Mr. L. Ruddle. Dr.G. Duff and Dr. J. Miller were re-appointed as Honorary Auditors. Atomic Spectroscopy Group The twelth Annual General Meeting of the Group was held a t 2.15 p.m. on Tuesday, November 30th, 1976, a t the Geological Society, Burlington House, London, W.l. The Chair was taken by the Chairman of the Group, Dr. R. Smith. The following office bearers were elected for the forthcoming year : Chairman- Mr. C. P. Cole. Vice-Chairman-Dr. W. J. Price. Honorary Secretary-Mr. D. J. Willis, Rank Hilger Ltd., Westwood, Margate, Kent, CT9 4 JL. Honorary Treasurer-Dr. G. B. Marshall. Honorary A ssistant Secretary-Mr. C. A. Watson. Members of Committee-Mr. R. P. Blakemore, Dr. L. C. Ebdon, Mr. D. L. Miles, Dr. E. J. Newman, Dr. L. Ranson and Dr. J. Warren. Mr. D. Moore and Mr. R. A. White were re-appointed as Honorary Auditors.

ISSN:0306-1396    

DOI:10.1039/AD977140052b

出版商:RSC    

年代:1977

数据来源: RSC

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March, 1977 STANDARDS 53 Standards The following is a summary of one of the papers presented at a Meeting of the Analytical Division held on October 6th, 1976, in London. The Community Bureau of Reference (BCR) W. van der Eijk Commission of the European Communities, Community Bureau of Reference, 200 m e de la Loi, B-1049 Brussels, Belgium Within the Scientific and Technological Policy Programme of the Commission of the European Communities , work is undertaken in connection with public, scientific and technological services for the member countries, and the Community Bureau of Reference (BCR) constitutes one of the sections involved in this field.The programme of the BCR is concerned with the multitude of problems encountered with measurement methods and instruments and their calibration with reference materials.The determination of intrinsic properties of materials, as executed at all levels of commercial, industrial and scientific processes, has to be carried out in such a way that the results of the measurements fall into a homogeneous and coherent system. This is the basic idea that justifies and necessitates the existence and use of reference materials.In recent years, close co-operation between all parties concerned in the member countries of the EEC has developed in the field of reference materials and methods and much current and future work in various technical sectors is being jointly executed and planned. This co- operation became possible only because of the work of the Advisory Committee on Programme Management (ACPM) and the central secretariat of the BCR.The activities of these two parts of the BCR are intended to ensure complete co-ordination of the work within the member countries and today goes much further than the simple execution of isolated research programmes. All national activities are being continuously harmonised with each other and whenever necessary completed by action from the EEC. This co-operation allows the rationalisation of a great number of national activities and their completion or stimulation by a limited number of joint activities, and this programme supports, groups, dovetails and supplements the efforts of member countries in this field.The BCR thus encompasses a large number of sectorial activities for which it serves as an over-all frame.The structure of the BCR consists of an Advisory Committee on Programme Management (ACPM) , a central secretariat and a multitude of participating laboratories. The means needed for the development and upkeep of this European co-operative system, as well as those needed for complementary research contracts, are provided for in the BCR programme. The central secretariat of BCR relies for much of its technical exppvrtise on support from the Joint Research Centre (JRC) of the EEC, in addition to its laboratory work.The JRC thus plays an important part in all BCR activities.54 TRAINING GRADUATES IN ANALYTICAL CHEMISTRY PYOC. Analyt. Div. Chem. SOC. The BCR programmes are based on these general ideas and the funds are allocated depend- ing on the development and the needs identified in the numerous sectors of activity.The programme is based on the assumption of continuous activity in previously opened areas and the gradual addition of activities in new areas. The exact allocation of funds to the various sectors and specialities will always depend on the needs of and proposals from member countries and is decided case by case on the basis of recommendations from the ACPM. The means provided will allow for the continuation and slow expansion of work in the sectors concerned with ferrous metallurgy, non-ferrous metallurgy, inorganic chemistry, physical and technological properties, organic chemistry (analysis, plastics and rubbers, petroleum and related products), clinical chemistry and environmental analysis, and for the start of work in new sectors such as food products, cosmetic products and pharmaceutical products.

ISSN:0306-1396    

DOI:10.1039/AD9771400053

出版商:RSC    

年代:1977

数据来源: RSC

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54 TRAINING GRADUATES IN ANALYTICAL CHEMISTRY PYOC. Analyt. Div. Chem. SOC. Training Graduates in Analytical Chemistry The following is a summary of one of the papers presented at a Meeting of the Education and Training Group held on October 20th, 1976, at the University of Birmingham. Recruitment and Training of Young Graduates for Analytical Laboratories-A Personal View from the Pharmaceutical Industry W.H. C. Shaw Glaxo Research Ltd., Greenford, Middlesex, UB6 OHE Two of the most striking aspects of the pharmaceutical industry are its international character and its large proportionate expenditure on research and development. The basic reason for the high level of world trade in pharmaceuticals lies in the high and increasing cost of de- veloping a new drug from the initial experimental stage to a marketable product.Except in the largest countries, domestic markets alone are insufficient to support the research effort needed. From this same reason stems the strong specialisation on the part of individual companies in a few selected therapeutic fields, rather than spreading their research more widely and less effectively over many classes of drugs. The development and sale of pharmaceuticals in most countries is subject to Governmental control, designed to ensure that products are safe and effective. In the UK, control is exercised under the Medicines Act 1968, and operated in relation to the examination of information, the granting of certificates to undertake clinical trials of new products and their subsequent licensing for sale, through the Committee for Safety of Medicines and the Depart- ment of Health and Social Security as the licensing authority.Over recent years, the amount of information required before approval of a new product can be obtained has increased greatly; it will include the proposed manufacturing process, analytical methods, specifications, batch and stability analyses, toxicity, pharmacology and therapeutic effectiveness.Most of the new drugs introduced to medicine are synthetic or semi-synthetic organic compounds of moderate complexity, usually with relative molecular masses in the range 200-1200. Produced initially on the laboratory scale, the compounds, after being checked for identity, will be subjected to a primary screening process operated by microbiologists if antibacterial activity is being sought or by pharmacologists when animal testing is needed, while toxicologists undertake preliminary safety testing.Most compounds will have lower activity than established drugs and be of no further interest. A compound that merits further study will be prepared on a larger scale and a possible commercial manu- facturing process developed.Pharmacists will make a range of experimental formulations and study their stability and a more detailed and extended toxicological study will be under- taken while earlier biological work is repeated and extended. Analytically, the purity of the material will be investigated, the amount and, whenever possible, the identity of im- purities will be established, methods for determining the compound in high and low con- centrations developed and the conditions under which the compound decomposes and the nature of the decomposition products will be studied. Assuming that all these and other studies show that we have a compound that is safe toMarch, 197 7 TRAINING GRADUATES IN ANALYTICAL CHEMISTRY 55 use and that biological tests indicate good potential therapeutic activity, the whole of the information is assembled in the form of a submission to the Committee for Safety of Medicines.If the Committee is satisfied with the completeness and validity of the information, it will advise the Licensing Authority to issue a Clinical Trial Certificate for the compound. The Certificate authorises the manufacturer to organise clinical trials, usually at teaching hospitals or under named consultants.The trials will extend over several months, sometimes much longer. If the trials are considered satisfactory, the results are submitted to the Committee together with an updated version of the remainder of the technical information. If the submission is accepted then, and only then, the manufacturer is authorised, through the granting of a product licence, to sell his product.The scientific environment in which a graduate entering the industry will find himself is essentially a multidisciplinary one where teamwork is of the essence. Much of the key in- formation is provided by analysis in one form or another, whether carried out by analytical chemists, microbiologists, biochemists or scientists of other disciplines.Against such a background, what training must be given to new graduates entering our analytical labora- tories and, when trained, what is expected of them? Over a period of several years, we would expect our trainees to have built up a thorough practical knowledge of the main analytical techniques operated and to have acquired the ability to produce trustworthy results on all instruments in the laboratory.Apart from general analytical procedures, most forms of chromatography (thin-layer, high-performance liquid, gas, ion-exchange and molecular exclusion) and spectroscopy (ultraviolet, infrared, nuclear magnetic resonance, atomic-absorption and -emission), together with the use of auto- matic analytical equipment, thermal and electrochemical methods of analysis, form the nucleus of the training programme.In parallel with the largely practical programme and background theory, there must be training in such related aspects as safety, laboratory documentation, the use of statistics and computer methods, while the ability to write reports of a reasonable standard should be acquired at an early stage.Specialist techniques such as microbiological assays, mass spectrometry, radiochemical methods and X-ray powder spectro- scopy may not form part of the practical training, but some knowledge is needed of the tech- niques, their capabilities and limitations and how the results are to be interpreted. By the end of their training period, graduates will have learned what techniques to apply in order to obtain the answers to problems in the most economical way and how to draw the correct conclusions from their laboratory work.They will be beginning to attend technical meetings and learning how to defend their conclusions, if necessary, in discussions with scien- tists of other disciplines. They will be developing one of the most important attributes of the analytical chemist-the ability to be critical of what information he is asked to believe and to put the right questions to satisfy himself on its validity.When we recruit graduates to be trained, what would we like to find when we interview them, and what, in practice, do we find? A few questions will soon reveal that the usual 3-year university degree course includes little that is directly relatable to analytical chemistry.Interpretation of molecular spectra in relation to molecular structure will have been well covered in organic chemistry. An ultraviolet and an infrared spectrophotometer may have been used, possibly also a nuclear magnetic resonance instrument, but of quanti- tative analysis, where their future careers, if in analytical chemistry, will mostly lie, practically nothing will have been taught.In contrast, the teaching of analytical chemistry in polytechnics is more identifiable, although often disguised as applied chemistry.l A 4-year sandwich-course graduate, in particular, will have spent two or three periods in an industrial laboratory; he will have some inkling of the practical problems facing such a laboratory and of the ways in which solutions to them are found.He will be a year older than the 3-year university-course graduate, he will certainly be better orientated and generally will show up better at interview. With a year’s training, however, the university graduate may well have caught up and perhaps reversed the position. The pharmaceutical industry is only a part of the chemical industry in this country; analytical laboratories in other parts of the chemical industry will have different requirements in mind when recruiting graduates.It could, in consequence, be argued that the function of our universities’ chemistry departments is to provide basic education with chemistry as the major subject. How far analytical chemistry, and particularly the attitude of mind56 TRAINING GRADUATES IN ANALYTICAL CHEMISTRY Proc.Analyt. Div. Chem. SOC. and practical approach it requires, should form part of that basic education is a matter of opinion. Let us examine the facts. The Analytical Division is the second largest Division of The Chemical Society. If the figures are any guide, the future careers of many chemistry graduates will lie in analytical chemistry.It would be easy to justify teaching the subject more widely to undergraduates on these grounds alone. If analytical chemistry is to continue to be inte- grated in chemistry degree courses, two possible ways of improving the situation come to mind, although both are in operation to some extent. As a practical exercise in organic chemistry, the student will prepare a particular com- pound, take the melting- or boiling-point of his product, run ultraviolet and infrared spectra and send a sample to someone else for elemental analysis and nuclear magnetic resonance spectrowopy and perhaps mass spectrometry.The probability is that the compound is the expected one, and that will be the end of the exercise. Let the student go on from that point, apply one or two forms of chromatography to his product, separate, identify and determine the impurities present.At least it will teach him to be critical of his own work, the beginnings of an analytical line of thought. Occasionally one interviews a graduate whose project had some analytical content, but it is rare to find that analysis is the major theme and there is clearly room for improvement in this direction.Such measures, though welcome, are, however, merely tinkering with the problem. The Commonwealth Universities Year Book2 lists 179 subjects for first-degree courses at British universities. Under Chemistry we find that the subject is offered by all but one of the universities. Industrial and applied chemistry may be read at 17, colour chemistry at 4, mathematical chemistry at 3, and technical chemistry at 2.Thus, analytical chemistry, of which there is no mention, cannot be taken as a main or subsidiary subject for a first degree at any British university. Only a minority of chemistry graduates go on to take a higher degree, still fewer a higher degree in analytical chemistry. How much longer must the formal and recognised teaching of our subject in universities be more or less confined to postgraduate courses? Are our academic friends so committed to research that they have forgotten to dig the very foun- dations for our science? No wonder there are difficulties in finding the right students’ to take up the SAC Studentship awards. No one of sufficient calibre with inventive ideas has yet come forward to justify the award of an SAC Fellowship.The reason is all too clear; the pool to be fished is too small and too shallow. Within the pharmaceutical industry there are biochemists, microbiologists, pharmacists, pharmacologists and others, all of whom will have been able to read their chosen subject from the time they entered university. Let our future analytical chemists be able to make a similar positive choice of career.One section of the chemical industry, at least, will welcome first-degree graduates in analytical chemistry. With such graduates no longer will there be doubt at interview, whether a candidate for a position in our laboratories is genuinely moti- vated towards analytical chemistry, or whether a year or two will be spent on his training, only for him then to discover a preference for some other branch of chemistry.Much has been said within the Analy- tical Division, and a little outside it, about the status of our science and the small number, of established university Chairs of Analytical Chemistry in this country3s4 and el~ewhere.~ So far these arguments seem to have been totally without effect. Let our universities take the crucial step of offering analytical chemistry in its own right, as a main subject for a first degree. If, in this way, analytical chemistry is given the academic coherence it so badly needs, there should be no fear of the consequences; full recognition as one of the major banches of chemistry will make the need for additional university Chairs in Analytical Chemistry clear for all to see. References Some kind of final-year project is a feature of many degree courses. Have we not here the key to the whole situation? 1. “Directory of Further Education,” Hobsons Press, Cambridge, 1975-76, p. 662. 2. “Commonwealth Universities Year Book,” Volume 1, Association of Commonwealth Universities, 3. Belcher, R., Chelny Brit., 1976, 12, 131. 4. Headridge, J . B., Chemy Brit., 1976, 12, 204. 5. Smythe, L. E., Chemy Brit., 1976, 12, 362. London, 1976, p. 200.

ISSN:0306-1396    

DOI:10.1039/AD9771400054

出版商:RSC    

年代:1977

数据来源: RSC

摘要:

March, 1977 CODE OF PRACTICE FOR USE OF GAS CYLINDERS 57 SAFETY IN ANALYTICAL LABORATORIES While safety in the chemical laboratory has been a matter of general concern for many years, interest in laboratory conditions and practices has been heightened by the recent introduction of the Health and Safety at Work Act. The laboratory concerned with analytical chemistry has, in addition to problems that occur in all laboratories, requirements that relate to its own particular work and the implications of these requirements have not been widely discussed in the literature.An occasional series of articles on aspects of safety of particular interest to analytical chemists is therefore to be published in Proceedings. It is hoped that these articles will provide a forum for further discussion, and correspondence on the individual articles and on all safety matters is invited.The first article, which takes the form of a code of practice for the use of gas cylinders in analytical laboratories, appears below. Code of Practice for the Use of Gas Cylinders in An a lyti ca I Laboratories About 2 years ago, the Analytical Chemist’s Committee (ACC) of Imperial Chemical Indus- tries Limited decided to set up a small team to study the use of gas cylinders in analytical laboratories and to recommend a code of practice.The team, comprising W. J. Cank (Mond Division), D. R. Deans (Petrochemicals Division), D. M. Peake (Imperial Metal Indus- tries) and L. F. C. Underwood (Petrochemicals Division), completed its task early in 1976 and, after taking account of comments from labora- tory managers and administration and safety officers in both the UK and Europe, the ACC approved the adoption of the code of practice for all of the Company’s analytical laboratories.The code evoked such widespread interest that it was decided to publish it in the belief that it would be of value to other analysts, and that it might stimulate constructive comment and discussion in what, for many laboratories, can be a difficult area.1. Scope The code covers the storage, transport, handling and use of gas cylinders in analytical laboratories only. Excluded from the code are the filling of cylinders, including the preparation of calibration mixtures, and pressure testing of cylinders and regulators. Also excluded is the transport of cylinders outside the laboratory.2. Gas Cylinder Hazards 2.1. Nature of the gas Gases should not be used without prior con- sideration being given to any hazards associated with them. If possible, use an alternative with a lower risk. The appropriate safety pre- cautions should be taken to safeguard personnel from any risk. Gases can be broadly classified as follows: 2.1.1.Inert asphyxiants (e.g., nitrogen, argon). This group of gases is non-toxic but can act as asphyxiants by displacing the air neces- sary to sustain life. 2.1.2. Toxic (e.g., sulpkur dioxide, Jzydrogen sulphide). Toxic gases in relatively low con- centrations may have adverse physiological effects. These effects will vary in form and degree depending on the gas.2.1.3. Flammable (e.g., butane, propane). The hazards associated with gases in this group are those of fire and explosion. Table I gives the flammability ranges (in air) of some of the more commonly used gases. There is a wide variation in flammability range for different gases. Ethylene oxide, for example, has explosive limits of 3-100% V/V in air, while butane has the relatively narrow range of Fire, possibly without explosion, will occur if a leak develops under conditions where the gas immediately comes into contact with a source of ignition (hydrogen escaping a t high pressure may ignite spontaneously).However, if igni- tion is delayed, an explosion (external to the 1.9-8.5% V/V.58 CODE OF PRACTICE FOR USE OF GAS CYLINDERS Proc. AnaZyt. Div. Chem.Soc. TABLE I FLAMMABILITY RANGES OF GASES IN AIR Gas Hydrogen . . Methane .. Acetylene . . Ethane . . Ethylene . . Cyclopropane . . Butane .. Butenes .. Carbon monoxide Ethylene oxide. . Methyl chloride Methylamine . . Ammonia . . Hydrogen sulphide Propane .. Explosive limits, yo V/V in air .. 4-75 .. 5-15 . . 3-52 . . 3-12.5 . . 3.1-32 . . 2.2-9.5 . . 2.4-10.4 . . 1.9-8.5 . .1.6-9.7 .. 12.5-74 , . 3-100 . . 10.7-17.4 . . 4.9-20.8 . . 16-25 . . 4.3-46 cylinder) will occur provided that the concen- tration of the gas in air, at the time of ignition, lies between the explosive limits of the particu- lar gas. Sources of ignition can include sparks from static discharges to or from cylinders. 2.1.4. Corrosive (e.g., chlorine, sulphur di- oxide). Gases in this category are usually toxic and corrosive.Most are lachrymatory and will irritate the skin, and some can be absorbed through the skin. 2.1.5. Decomposition. Some gases, particu- larly acetylene, can decompose spontaneously when stored under pressure. Above pressures of about 9 p.s.i.g., undissolved (free) acetylene will begin to dissociate (decompose) and revert to its basic elements, viz., carbon and hydrogen.Considerable amounts of heat are given off during dissociation and may result in explosions of great violence. For this reason, acetylene is dissolved in acetone contained in a porous material (massing) inside the cylinder. If a void should occur in the porous mass of a cylinder of dissolved acetylene, then the acetylene may decompose. This decomposition may be initiated by some mechanical shock, such as dropping the cylinder.The voids in the porous mass can occur through natural settling of the mass or through damage to the cylinder in the form of denting. 2.1.6. Others (e.g.. oxygen, compressed air). Small increases in oxygen concentration greatly increase the fire hazard. An oxygen-enriched atmosphere will permit the burning of sub- stances that are not readily combustible in ordinary air.Fluorine and chlorine trifluoride, both of which are toxic, are very reactive chemically; in contact with many substances these gases will cause spontaneous fires and very vigorous burning can occur. 2.2. Density of gases Gases heavier than air can travel considerable distances and accumulate at a lower level than the source of a leak, thus producing an explosive or toxic hazard at a remote point.Leaks of gases lighter than air tend to be self-venting but can be trapped at higher levels than the leak. Hydrogen in particular can present an explosive hazard in this way. 2,3. Liquefied gas Dangers can exist due to hydraulic pressure if cylinders are not filled to the correct ullage or if subjected to a temperature increase (above 45 “C is considered unsafe).Liquefied gas cylinders should not be placed close to the surface of radiators, steam pipes, ovens, etc. 2.4. Gas cylinder identification It is essential to know what gas is contained in a given cylinder. All cylinders must therefore be clearly labelled with regard to their contents. For normal industrial gases, labelling according to BS 349:1973 is recommended.Commercial industrial gas cylinders should normally be colour coded according to the above British Standard. Colour codes can be ambiguous ; “industrial” gas colour codes are different from those for “medical gases.” This ambiguity can present a considerable hazard when both types of cylinders may be in use. The colour coding of gas pipes and hoses, which may be supplied with gas from cylinders, is not standardised.Consequently, any colour- coded pipes that are to be connected through a suitable regulator to the cylinder are likely to be colour coded differently. The main hazard is that it is not necessarily correct to connect a cylinder of one colour code to a pipe of the same. colour code. As a further means of distinguishing between flammable and non-flammable gases, the cylin- der valve outlets are screwed left-hand and right-hand, respectively.The outlets of valves for oxygen cylinders are screwed right-hand, as oxygen itself is non-flammable. The valve outlets of American helium cylinders have left- hand threads, although the gas is non-flammable. Hazards can arise through the use of an incorrect regulator on a cylinder.For instance, acetylene regulators should not be used onMarch, 1977 CODE OF PRACTICE FOR USE OF GAS CYLINDERS 59 hydrogen cylinders, which are filled to a higher pressure. The gauge for hydrogen is up to 3 000 p.s.i. but for acetylene 600 p.s.i. 2.5. Accidental escapes of gas Accidental escapes of gas will give rise to the hazards outlined in Section 2.1.Hazardous conditions may also arise if the escaping gas comes into contact with a substance with which it is chemically reactive. Such escapes may be occasioned by, for example, a defective cylinder valve or failure to close the valve properly, non- tight gas connections and defective hoses, pipes or connected apparatus. - 2.6. Gas pressure Some hazards arise only because the gas in a cylinder is at a pressure greater than atmos- pheric.For example, there is the risk of bursting should a cylinder receive a severe mechanical blow, or as the result of a pressure rise following an increase in temperature, such as involvement in a fire. Should the cylinder valve be broken off, the contents of the cylinder will be discharged to the atmosphere in an un- controlled manner, creating the risk of fire, explosion, poisoning or asphyxiation (depending on the gas), and the cylinder could, in some circumstances, be propelled like a rocket, so causing considerable damage. A considerable amount of energy is stored in a gas cylinder.For example, a 5.7-m3 cylinder when charged to 172 bar (2 500 p.s.i.g.) con- tains the energy equivalent to the contents of a small high-explosive shell.It is important to ensure that fittings and apparatus (on the high-pressure side of an installation) will safely withstand the maximum pressure of the cylinders that are to be connected. 2.7. Cylinder masses Cylinders in common use weigh between 23 and 113 kg when fully charged but are also of considerable mass when empty. Personal injury could arise through mishandling or insecure positioning.The dropping of a cylinder could result in damage to the cylinder with the associated hazards (see Section 2.6). 3. Example of Instructions for the Use of Gas Cylinders in Analytical Laboratories These instructions are intended as a guide, and the actual instructions issued at any site should take into account any local conditions and in particular local emergency procedures, which may differ from those included.Specific start-up and shut-down instructions should be provided for each major analytical installation incorporating gas cylinders. 3.1 Storage No part of any working area should be used for the purpose of long-term storage of gas cylinders. The number of gas cylinders held in the laboratory should be kept to the minimum necessary to meet working requirements.If a cylinder of a little used gas, particularly if corrosive, is kept in a laboratory for a lengthy period, it should be inspected periodically by a “competent” person. 3.2. Movement Cylinders should always be handled carefully and should not be allowed to receive blows likely to damage them or their valves, e.g., by being dropped on to unyielding surfaces.The mass of large cylinders makes it essential that they should always be moved in a cylinder carrier or trolley, which are available com- mercially. Staff should have instruction in kinetic handling and lifting, to avoid the risk of personal injury through mishandling. A film3 is available on kinetic handling, which includes the lifting of cylinders. Cylinders should not be handled with greasy hands, gloves or rags.When provided, valve covers should be kept in position in order to protect the valve during handling operations. 3.3 Correct use of cylinders 3.3.1. Size of cylinders. Whenever possible the size of cylinder should be such that the contents are used up within a reasonable time.3.3.2. Siting. Cylinders may be located in shelters outside the facility where the gas is required and the supply piped in. Any pipework should be designed by or approved by an engineer and include an isolation valve which can be operated from inside the laboratory. Cylinders may also be located in the laboratory. In both instances care must be taken to protect the cylinder from any source of heat likely to increase its temperature much above ambient.Care must also be taken to avoid contact with corrosive materials or dirt. Cylinders used in the open for lengthy periods should be protected from rain, snow and ice and consideration must be given to the effect that a decrease of the temperature to below ambient will have on the contents of the cylinder.Entrances, exits and passages must not be blocked by gas cylinders. 3.3.3. Care ‘and use of cylinder valves and fittings. Cylinder valves should be kept clean.60 CODE OF PRACTICE FOR USE OF GAS CYLINDERS PYOC. AnaZyt. Div. Chem. SOC. Loose dirt lying within the valve socket must be removed either by “snifting,” i.e., momen- tarily opening the valve to allow a small volume of gas to blow through, or preferably by blowing the dirt out with a compressed air-line if available.“Snifting” must not be carried out in confined spaces when toxic and/or flammable gases are involved, and in the latter instance not where there is any possibility of ignition. The operator should stand clear of the outlet while performing this operation. The cylinder valve must be cleared of loose dirt before fitting the regulator in order to allow it to seat properly.Only the standard key should be used to operate the valve spindle. Leverage must not be increased by any means, nor must excessive force be used. Valves should always be opened slowly. Some valves are fitted with non-captive spindles and care must be taken not to unscrew them too far (normally a half turn is sufficient).Cylinder valves and fittings should not be lubricated, except under specific advice from the gas supplier. On no account should oil or grease be used on oxygen cylinders, because of the risk of fire or explosion. Gas cylinders, valves and safety valves must never be repaired or modified by unskilled people. Cylinders, their valves and fittings should not be handled with greasy hands, gloves or rags.3.3.4. Use of regulator. With permanent, i.e., non-liquid, gases, the cylinders must be fitted with a pressure-reducing valve and the gas distributed at a reduced pressure. A regulator of the correct type (with respect to the pressure and nature of the gas) must always be used when gas is required from a cylinder. The cylinder valve must not be used to regulate the flow of gas.With liquefied gases, control of the gas flow should be arranged in accordance with the supplier’s instructions, which may or may not advise the use of a regulator. When a cylinder is not in use the cylinder valve must be closed. 3.3.5. Stability of cylinders. Cylinders must be secured against unintended movement. Cylinder stands, clamps or cylinder trolleys can be used for this purpose.3.3.6. Special precautions f o r cylinders of acetylene, liquefied gas and ammonia. Acetylene cylinders and cylinders of liquefied gas must be used upright in order to avoid outflow of liquid (acetone in the case of acetylene) into the regulator. Joint fittings or piping made of copper or of an alloy that contains more than 70% of copper must not be used with acetylene cylinders.Acetylene in contact with copper can form copper acetylide, which will readily explode when subjected to friction, heat or impact. Fittings used to connect ammonia cylinders must not be made of copper or copper alloys because of their susceptibility to chemical attack. 3.3.7. Testing for leaks. Joints in fittings and piping can be tested for leak-tightness by applying a soap solution.With fluorine, use a filter-paper soaked in potassium iodide solution, when a brown stain will appear at the leak. There are commercially available leak detectors for specific gases and explosion meters to detect leaks of hydrogen, etc. Leaks can also be detected by closing all exits, pressurising the system and isolating the inlet, then observing any pressure drops in the system with time.When particularly hazardous gases are to be used, the advisability of installing continuous leak detectors should be considered. 3.3.8. Pressure gauges. Pressure gauges for use with oxygen should be permanently and plainly marked “Oxygen.” They should be used as supplied and not allowed to become contaminated with oil, as an explosion may result from contact between oil and oxygen under pressure.The maximum scale reading of any pressure gauge connected to a gas installation should be at least one third greater than the greatest pressure to be applied to that gauge. This includes gauges used to indicate cylinder pressure (unless the gauge is specifically marked for full-scale operation).3.3.9. Miscellaneous. Cylinders should not be allowed to come into contact with electrical apparatus. Cylinders, whether charged or empty, must not be used as rollers for moving equipment. Personnel responsible for the acceptance of gas cylinders should satisfy themselves that the cylinders supplied are undamaged and that the contents are readily identifiable. When in doubt the cylinder should not be used and the supplier should be notified. The valve on an empty gas cylinder must be closed, and any protecting valve cover replaced.Also, the cylinder must be marked “empty.’J Air and moisture should not be allowed to enter cylinders (air would present a decontamina- tion problem to the supplier, and moisture would present a corrosion risk). This could occur if a cylinder was emptied and the valve left open.For these reasons, cylinders should not be completely blown down, but a slight pressure should always remain in them.March, 1977 CODE OF PRACTICE FOR USE OF GAS CYLINDERS 61 3.4. Emergency firocedures 3.4.1. Fire. In all instances of fire, raise the fire alarm locally, which should immediately bring into operation local procedures; if neces- sary call the Fire Brigade; don breathing apparatus. When fire has originated in other material, try to extinguish the fire.If it is safe to do so, remove from the area cylinders not yet involved in the fire; ensure valves are properly closed. Cylinders that have become heated should be left where they are pending the arrival of the Fire Brigade. If safe to do so, they should be cooled by copious hosing.When flammable gas leaking from a cylinder is burning at or near the source of the leak, try, to close the valve. Try to remove any material being burned by the flame, using tongs for this purpose. If neither of these actions is possible apply a suitable extinguishing agent to any burning material, but never try to extinguish the gas flame itself other than by closing the valve.Do not spray water on to a cylinder of liquefied petroleum gas where the escape of gas is burning, as this could increase the output of gas where the cylinder has become cooler than ambient. When flammable gas is leaking from a cylinder but not burning, try to close the valve. Extinguish any means of ignition. Remove the cylinder into the open if possible. If not, evacuate the building and inform the site emer- gency service. When a cylinder of acetylene is thought to be “burning” internally (i.e ., the acetylene is undergoing decomposition), as evidenced by a hot spot on the cylinder wall, close the valve, .warn persons in the vicinity and tell them to leave the area.Call the Fire Brigade, then inform the suppliers as soon as possible-do not wait until the cylinder is thought to besafe.The Fire Brigade should deal with the cylinder until the supplier’s representative arrives. When any fire incident is over, never attempt to examine, use or tamper with a cylinder that has been involved; always inform the suppliers and allow them to take appropriate action. 3.4.2. Toxic gas leaks.If no respiratory protection is available, evacuate the area and inform the site emergency service. If canister-type gas respirators (“gas masks”) of a type specifically approved for the gas con- cerned are readily available, don a respirator and, if the leak is small, try to stop i t ; if not immediately successful, leave the area. If the leak is large, leave the area at once and inform the site emergency service.Warning. Canister-type gas respirators will not give protection against high concentra- tions of gas. Generally, 30-min protection will be available provided the gas concentration does not exceed 1 yo. The use of self-air sets is preferable provided that another person similarly equipped is standing by to effect rescue if necessary. NOTE: There may be a need to wear pro- tective clothing, e.g., against chlorine trifluoride. 3.4.3. Inert asphyxiant gas leak. If the leak is small, try to stop it, but if it is large leave the area and inform the site emergency services. 3.4.4, Shearing off of cylinder valve. If a gas cylinder valve is sheared off, there will be an uncontrolled outflow of gas, and there is a possibility of the cylinder becoming jet propelled. Evacuate the area and inform the site emergency service. 4. Statutory Requirements following Government Regulations : Cylinders of gases are covered by parts of the 1. Petroleum (Consolidation) Act 1928, CH 2. The Petroleum (Compressed Gases) Order 3. The Highly Flammable Liquids and Liquefied Petroleum Gases Regulations Explosives Act 1875, Order in Council No. 32. 1930. 1972. 30. 4. 5. Bibliography 1. UK Atomic Energy Authority, “Safety in the Use of Gas Cylinders,” A.H.S.B. Rep., A.H.S.B. ( S ) R-84, 1965. 2. ‘*Identification of Contents of Industrial Gas Containers,” BS 349 : 1973. 3. “Make Light of Lifting,’’ ICI Film Library, London. 4. “Matheson Gas Data Book,” Fourth Edition, Herst Litho Inc., New York, 1966.

ISSN:0306-1396    

DOI:10.1039/AD9771400057

出版商:RSC    

年代:1977

数据来源: RSC

摘要:

March, 1977 CODE OF PRACTICE FOR USE OF GAS CYLINDERS Equipment News Balances Gallenkamp have announced a new range of Mettler top-pan electronic balances, with easy to read LED digital displays. The PT320 is a “stretched” version of the current PT200, with a range of 0-320 g, readable to 1 mg. In the PL series two ranges are available: 0- 320 g readable to 0.01 g (PL300 and PL301) and62 EQUIPMENT NEWS Proc.Analyt. Div. Chem. Soc. 0-3200 g readable to 0.1 g (PL3000 and PL3001). The simple, single control bar of the earlier models is retained. Although the new balances are considerably smaller, a large seven- segment display is incorporated. Second mem- ories in the PL301 and PL3001 allow the running net total of weighed substances to be displayed. A second touch displays the mass of substance being added.This feature is valuable if inter- ruptions to the weighing procedure are likely to occur. A further addition for general weighing pur- poses is the dual-range PR1200. This has two selectable ranges: 0-120 g (readable to 0.01 g) and 0-1 200 g (to 0.1 g). Facilities for connec- tion to a recorder are incorporated, thus per- mitting direct transfer of weighing data.All of these balances are fully electronic and thus do not require vibration-free environments for reliable operation. A. Gallenkamp & Co. Ltd., P.O. Box 290, Christopher Street, London, EC2P 2ER. Programmable Data Logger The Aepex 810, designed and manufactured by AEP-International, is a programmable data logger which incorporates important features not normally found in data logging systems.The master control unit (MCU) accepts both analogue and digital inputs and can control up to 16 satellites, each with a 200-channel capacity. The satellites are data-gathering centres linked to the MCU by single cables, and can be either remote or local to the MCU. A crystal-controlled calendar clock in the MCU displays date and time.Integral battery back-up ensures that there is no data loss in the event of mains failure. Digitisation of analogue level inputs is by V to F converter. Linearis- ation is by PROM with up to four different con- figurations per system selected by pre-pro- grammed function store. Data printout is by fully alpha-numeric matrix line printer with 16 characters per line and a standard speed of 20 lines per second. AEP-International Ltd., Victor House, Norris Road, Staines, Middx. Blood Lead Testing A new instrument for the rapid screening of lead in blood, the ESA Model 4000, uses fluorimetry to measure the amount of zinc protoporphyrin (ZnP) in a drop of blood (about 30 pl). ZnP is a metabolite that increases in relation to the amount of lead ingested and absorbed in soft body tissue.As each measurement takes only about 10 s, thousands of samples can be checked in a single day. The Model 4000 is portable and extremely easy to operate, so that it can be readily used in fie1 d conditions. A sister instrument, the ESA 3010, uses anodic-stripping voltammetry for specific analy- sis of lead, copper, cadmium and other metals in blood and urine.MSE Scientific Instruments, Manor Royal, Crawley, West Sussex, RHlO 2QQ. Eppendorf Pipettes The Eppendorf range of fixed-volume pipettes has been re-designed to incorporate several new improvements. A single button allows one to &pick up sample, to pipette and to eject the tip. The pipettes now have a slimmer nose-cone to permit entry into small-diameter test-tubes.Pipette 4700 is available in 31 different sizes from 1 to 1000 p1. New multi-volume pipettes incorporate similar features. A partial twist of the operat- ing button adjusts the pipette to one of three different volumes. Six models are available, from the smallest at 10 - 20 - 25 pl to the largest at 500 - 750 - 1000 p1. Anderman & Co. Ltd., Central Avenue, East Molesey, Surrey, KT8 OQZ.Laboratory Spill Kits A range of six individual “laboratory spill kits” to neutralise, clean up and safely dispose of common hazardous chemical spills is offered by Diamed Diagnostics. Devised by the Baker Chemical Co., the kits are available to deal with acids, caustics, flammable solvents, mercury, cyanides and hydrofluoric acid. Diamed Diagnostics, Queensland Street, Liverpool, L7 3JQ.Fraction Collector For general use the Buchi 660 fraction collector is now available. The 660 is an extremely com- pact unit offering a choice of four interchange- able turntables carrying 24 x 14, 24 x 18, 16 x 24 or 8 x 52 mm diameter collection tubes. A timer provides dual ranges of 0-60 s or 0-60 min . Orme Scientific Ltd., P.O. Box 3, Stakehill Industrial Estate, Middleton, Manchester, M24 2RH.Liquid Chromatography A new high precision bore stainless-steel tube for HPLC has been introduced by Accles andMarch, 1977 EQUIPMENT NEWS 63 Pollock, and provides a higher level of perform- ance compared with many of the tubes currently in use. The Apollo LC tube has a guaranteed mirror finish bore of 20 pin RMS CLA (0.5 pm) and offers increased column efficiency, a signifi- cant decrease in edge effects and greater uni- formity in reproducing columns.The column is available with three standard internal diameters of 4.5, 7.0 and 10.0 mm, with special sizes on request. The Apollo LC can be supplied in pre- cision-cut lengths of 10, 15, 25, 50 and 100 cm or in random lengths. Magnus Scientific, Alsager, Cheshire.Portable Conductivity Meter The Hach portable conductivity meter measures specific conductance for a wide range of applic- ations, from distilled water to industrial wastes. A 49-in analogue meter makes read-outs easy on any of the five ranges, from 0 to 20000 pmho ( p S ) . A thermistor network in the tungsten probe electrodes automatically compensates for sample temperature from 0 to 100OC.An accuracy of 1 yo f .s.d. is claimed. Hach Chemical Co., P.O. Box 907, Ames, Iowa 50010, USA, or Hach Europe, BP 51, 5000 Namur 1, Belgium. Air Monitor The Miran-201 ambient air monitor can be sensitised to measure any one of over 300 toxic vapours to OSHA compliance levels. The instrument sequentially monitors as many as 15 remote locations up to 400 f t distant, printing vapour concentrations in parts per million a t each location and time of sampling on a digital printer.These data enable time- weighted averages of the exposure of individual workers to be determined. An additional feature is an adjustable high-level alarm to give an immediate warning of unsafe toxic concentra- tions at any of the monitored sites. The single-wavelength infrared system per- mits a high degree of selectivity, thus reducing interference from other vapours that may be present in the atmosphere being monitored.For most applications the ability to measure a single pre-selected toxic gas is sufficient; how- ever, a multi-purpose installation is sometimes required and can only be achieved a t present by installing two or more instruments.Wilks Scientific Corp., P.O. Box 449, S. Nor- walk, Conn. 06856, USA. Computing Quantitative IR Analyser The Wilks Model 80 computing IR analyser permits measurement of up to 18 wavelengths in under 2 min, automatic data reduction of up to 11 components with interference correction and instant recall of 5 discrete analyses. A permanent record of all analytical data is pro- vided by the integral printer.Recall from memory is also easily achieved. Extremely accurate quantitative data are obtained owing to the high signal to noise ratio and low drift. Through signal averaging, 256 measurements are made a t each wavelength over a 1/180-s interval. A wide range of sample handling accessories can be accommodated. The total analysis time for a complex five- component mixture, with significant spectral interferences, is claimed to be 5 min; a similar analysis by manual methods would necessitate several hours of data reduction time.Wilks Scientific Corp., P.O. Box 449, S . Norwalk, Conn. 06856, USA. GC Carrier Gas Control Module A dual-channel carrier gas control module, primarily intended to upgrade control systems on existing gas chromatographs, has been intro- duced by SGE.The carrier gas supply pressure is stabilised by a precision regulator and the gas then passes to two digital flow controllers that provide constant mass flow-rates with changing downstream pressure. The actual flow-rate is displayed on a digital indicator over the range 10-90 cm3 min-l. Scientific Glass Engineering (UK) Ltd., 657 North Circular Road, London, NW2 7AY.Pollution Air Samplers A new range of air samplers has been introduced by Gelman Hawksley Ltd. All samplers have temperature control, flow meters and 24-h timer control. The automatic sequential sta- tions have the added facility of a temperature- measuring system coupled to a strip recorder. The flow-rate can be varied between 0.5 and 30 1 min-l. Samplers for monitoring airborne gas and dust are fitted with glass impingers, and for particulate contaminants Gelman open- ended filter holders or the new magnetic filter holder are used with the Gelman range of membranes.Gelman Hawksley Ltd., 12 Peter Road, Lancing, Sussex, BN15 8TH. Dissolved Oxygen Electrodes The Type 40/3M dissolved oxygen electrode is a laboratory model for applications requiring a compact probe and fast response.The Type 28/3M is a field model suitable for most indus- trial applications and BOD determinations ; the Type 30/3M is identical, but incorporates the64 EQUIPMENT NEWS Proc. Analyt. Div. Chem. SOC. Simac temperature compensator. All electrodes are supplied with a 3-m cable and DIN plug. The replaceable pre-mounted membranes are readily changed without tools and can be factory refurbished if required.Simac Instrumentation Ltd., Lyon Road, Hersham, Walton-on-Thames, Surrey, KT12 3PU. Retrofit Kit for Time-of-flight Mass Spectrometers The CVC MA-RK-5 electronics retrofit kit is now available for Model 12 and 14 time-of-flight mass spectrometers. The kit greatly improves the stability, sensitivity and reliability of these instruments and gives the user access to the full range of MA series output accessories, including multiple mass sequencer, four-channel monitor, dual rate scanner and total output monitor.CVC Scientific Products Ltd., Eastheath Avenue, Wokingham, Berks., RG11 2PW. Bench Power Supply Three commonly used voltage - current combin- ations for integrated circuits, both linear and digital, and microprocessors, are provided by the Kepco Model MPS 620M.The 5-V supply has a 0-6-V adjustable output, rated 0-5 Aat any voltage setting, and can be operated without de-rating to f50 "C. Error- sensing terminals are provided, with capacity to handle 1-V cable loss, and the output is protected by an adjustable crowbar. Control is by a high- resolution 10-turn rheostat.The f20 and -20 V outputs are controlled by a single 10-turn control in a tracking mode and provide a full 1-A output through their entire range. Large 24411 meters monitor both voltage and currents on all three outputs. Techmation Ltd., 58 Edgware Way, Edg- ware, Middx., HA8 SJP. Radioimmunoassay The LKB-Wallac Ultro RIA is a simple, versatile system for radioimmunoassays.Samples are prepared using either the LKB 2075 diluter or the LKB 2071 sample processor. The former, using a fast hand-operated pipette, permits the dispensation or dilution of pre- selected volumes from 10 pl to 3 ml at the rate of 20 per minute. The latter, designed for automatic operation, can be programmed to sample, dilute and dispense into racks of test- tubes.Nine special push-button programmes are suitable for most RIA requirements. The LKB-Wallac 1270 Rackgamma is the measuring station of the system and permits gamma-counting to pre-set parameters for most normal assays. The same racks as for sample preparation are used, and thus immediate counting is facilitated. The Rackgamma in- corporates a mini-computer, which not only controls all the measuring operations, but also evaluates the results.Use of the RIA evalu- ation pack permits calculation of the dose value and provides a printout for direct use by the physician. LKB Instruments Ltd., LKB House, 232 Addington Road, Selsdon, South Croydon, Surrey, CR2 9PX. Rheology The Rheometrics mechanical spectrometer is useful for the study of deformational response of materials under controlled stress.Viscoelastic measurements of fluid, molten, rubbery and solid-state materials, traditionally difficult and time consuming to perform, are now achieved in a few minutes. Thus information on process- ability and molecular characterisations of fluids, melts and rubbers, or thermodynamic transi- tions in solids, is readily available. The spectrometer consists of a transducer with a 20 g to 10 kg orthogonal force ( X , Y and 2) full scale and a 200 g cm-l to 100 kg cm-l torque.This, coupled with a precision air bearing, signal conditioner, sample thermo- couple, X , Y, 2 translation, constant angular velocity from 0.001 to 200 rad s-l and contin- uous and discrete speed selection, forms the fundamental drive unit. Precision environ- mental chambers permit rapid and accurate measurements from - 120 to + 320 "C for solids, melts and fluids.Dynamic oscillatory or vibrational motions can be provided through a low-frequency sinusoidal function generator with a frequency range of 0.001-30 Hz. Automatic printout of all rheological test data, paper punch units and X - Y plotters can also be incorporated. Rheometrics Inc., 2438 US Highway No.22, Union, N.J. 07083, USA. Microwave Plasma Emission Spectro - meter The EDT MPS 600 microwave plasma emission spectrometer system permits the determination of trace elements in small liquid samples. This instrumental system has been developed for the routine simultaneous determination of sub- nanogram amounts of both metals and non- metals in sample volumes of only a few micro- litres by atomic-emission spectrometry. It provides a discrete sampling system and excitation source and detection system capableMarch, 1977 EQUIPMENT NEWS 65 of precise and simple operation. The heart of the instruments is a microwave-excited argon plasma discharge ; emission from samples intro- duced into the plasma is analysed and detected via a multi-channel direct-reading spectrometer.This is an electronic signal recovery system which allows sensitive and precise analysis for up to eight elements simultaneously in pico- gram amounts in a single 5-pl sample solution. A fully programmable timer sequence permits sample desolvation, ashing and vaporisation. EDT Research, 65 Ivy Crescent, London, W4 5NG. Literature A new laboratory automation system for collec- tion and evaluation of real-time data from up to 30 analytical instrument interfaces is described in a 16-page brochure from Hewlett-Packard.An 18-page brochure devoted to the HP 5840A Series reporting chromatograph is now available. The HP 5840A is a second-gener- ation processor-based analytical system that features ease and speed of magnetic-card pro- gramming, an increased processor memory and a bidirectional link to laboratory computer systems.Quantitative trace component analysis, using a “purged splitless’ ’ gas chromatography tech- nique, is described in a 4-page application note. The technique is especially suited for chromato- graphers concerned with complex mixtures in environmental, flavour, fragrance and biomedi- cal investigations.Hewlett-Packard Ltd., King Street Lane, Winnersh, Wokingham, Berks., RGl 1 5AR. Process control instrumentation systems, which automatically analyse process streams or batches of specified compounds and then initiate action to maintain concentrations within desired limits, are described in a new brochure from Wilks. The MIRAN-1 system of mini- ature infrared analysers and accessories is also described in a 6-page brochure, outlining the three basic systems available. Wilks Scientific Corp., P.O. Box 449, S. Norwalk, Conn. 06856, USA. A 58-page catalogue of systems and methods for biochemical research is available from LKB Instruments Ltd., LKB House, 232 Addington Road, South Croydon, Surrey, CR2 SYD. The complete range of Chemplex XRF and XRD spectrochemical accessories is described in a new catalogue. Chemplex Industries Inc., 140 Marbledale Road, Eastchester, N.Y. 10707, USA. The 17th edition of the Kent Technical Review is devoted to articles on the Group’s measuring, analytical and process control instrumentation. Of special interest to analysts are descriptions of power station water analysis using electrochemical sensors and new uses for katharometers. George Kent Ltd., Luton, Beds., LU3 1AL.

ISSN:0306-1396    

DOI:10.1039/AD9771400061

出版商:RSC    

年代:1977

数据来源: RSC

摘要:

March, 1977 EQUIPMENT NEWS 65 Hilger S pect ro- scopy Prize The CS Atomic Spectroscopy Group invite appli- cations for the 1977 Rank Hilger Spectroscopy Prize. The successful candidate will receive a prize to the value of k75, part of which is to be used for the purchase of a book(s) for presentation at the AGM of the Group. The award will be judged on the basis of the candidate’s contribution to analytical atomic spectroscopy.Relevant tech- niques include atomic-absorption, atomic-fluores- cence, atomic-emission and X-ray fluorescence spectroscopy. The work need not be theoretical but could cover applications, instrumental modification, accessories, improvements in technique or data handling. The contribution need not have been published and candidates’ wishes with respect to publication will be respected.Intending candidates should (1) be under 30 years of age on December 31st, 1977; (2) be resident in the United Kingdom; (3) submit, before May 31st, 1977, a summary of about 500 words, describing their contribution to the theory or practice of atomic spectroscopy. The summary should be endorsed by a senior mem- ber of the establishment in which the candidate is employed. The Selection Committee would also be pleased to consider applications brought to their attention by senior members of an establishment on behalf of candidates who comply with the above criteria. Short-listed candidates may be required to submit a more detailed account of their work. Applications should be addressed to the Honorary Assistant Secretary, Atomic Spectro- scopy Group, Analytical Division, The Chemical Society, Burlington House, London, W 1V OBN.

ISSN:0306-1396    

DOI:10.1039/AD9771400065

出版商:RSC    

年代:1977

数据来源: RSC