摘要:

Proceedinas - ~ - - - wof the Analytical Division ofThe Chemical SocietyCONTENTS19 SAC Gold and~.Silver Medals19 AD Distinguished Service Award19 Reports of Meetings20 Geochemical Analysis21 Summaries of Papers212830 'Original Papers in Pharmaceutical40 Obituaries42 Conferences and Courses43 Chemical Society Library44 Publications Received46 CS Publications News48 Analytical Division DiaryCS Autumn Meeting: 'Data Usageby Analytical Chemists'CS Autumn Meeting: 'Justification ofComputers in Analytical Chemistry'Analysis'Volume 14 No 2 Pages 19-48 February 197PADS DZISSN 0306-13961 4 (2) 1 9-48 (1 977) February 1977PROCEEDINGSOF THEANALYTICAL DIVISION OF THE CHEMICAL SOCIETYOfficers of the Analytical Divisionof the Chemical SocietyPresidentD.W. WilsonHon. SecretaryP. G. W. CobbSecretaryMiss P. E. HutchinsonHon. 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.Nonmembers can only be supplied with Proceedings as part of a combined subscription with The Analystand Analytical Abstracts.Q The Chemical Society 1977SCOTTISH REGION MEETINGIntensive Course onat theWolfson Liquid Chromatography UnitDepartment of Chemistry, University of EdinburghonThursday and Friday, 9th and 10th June, 1977HIGH-PERFORMANCE LIQUID CHROMATOGRAPHYA 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.I f 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

ISSN:0306-1396    

DOI:10.1039/AD97714FX005

出版商:RSC    

年代:1977

数据来源: RSC

摘要:

Febrwary, 1977 ANALYTICAL DIVISION DIARY 47Analytical Division Diary, continuedMarch, continuedFriday and Saturday, 25th and 26th:PitlochryScottish 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 t o 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. GoodmanScotland’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 ,4rt Became a Science,” byF. Szabaddry.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 t o 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-Characterisa-tion of Chemical Species-“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.“Distinguishing ‘Dissolved’ and ‘Undissolved’Forms of Lead in Potable Waters,” byC. A. Edwards.‘University College, London.Wednesday, 30th, 2 p.m. : ManchesterParticle 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, ManchesterM17HS.Wednesday, 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. 7FEBRUARYTuesday, 22nd, 4.15 p.m. : LoughboroughMidlands Region, jointly with the Lough-borough University Chemical Society.“Approaches to Automation,” by J.K.Foreman.Lecture Theatre J O O l , Edward HerbertBuilding, University of Technology, Lough-borough.Tuesday, 22nd, 2.30 p.m.: ReadingSouth East Region, Microchemical Methodsand Electroanalytical Groups.“An Analyst Appraises Electroanalysis, ”by Professor E. Bishop.Discussion to be led by B. Fleet and P. 0.Kane.Chemistry Department, Palmer Building,Room G-02, The University, Reading.Maps are available from Dr. B. Birch,Port Sunlight Laboratory, Unilever Ltd.,Port Sunlight, Merseyside L62 4XN (Tel.051-645-2000).Tuesday, 22nd, 7 p.m. : SwanseaWestern Region, jointly with the South Wales“Two Hundred Years of Brewing,” by Pro-Chemistry Department, University CollegeWest Section of the CS.fessor R.Belcher.of Swansea, Swansea.Wednesday, 23rd, 10.30 a.m. : LondonRadiochemical Methods Group on “ResearchTopics. ’Chemistry Department, Queen ElizabethCollege, Atkins Building, Campden Hill,Kensington, London, W.8.Thursday, 24th, 4.15 p.m.: Old AberdeenScottish Region, jointly with the Aberdeen andNorth of Scotland Section of the CS and theAberdeen University Chemical Society.“Dithizone-A New Look at an Old Reagent,”by Professor H. M. N. H. Irving.Department of Chemistry, University ofAberdeen, Meston Walk, Old Aberdeen.MARCHTuesday, lst, 2 p.m.: LondonEducation and Training Group on “TeachingSpeakers: D. Pusey, S. Thorburn and S. J.Polytechnic of the South Bank, London, S.E.1.Chromatographic Techniques.”Moulton.Analytical Division DiaryPrinted by Heffers Printers Ltd Cambridge EnglandWednesday, 9th, 6.30 p.m.: MoretonNorth West Region, jointly with the Liverpooland District Section of the CS and theSouth Cheshire Branch of the Pharma-ceutical Society.“Pharmaceutical and Analytical Aspects ofBio-availability,” by N.E. Stevens andJ. R. Salmon.E. R. Squibb Laboratories, Moreton, Wirral.Friday, 1 lth, 6.30 p.m. : ChepstowWestern Region.Discussion on “Analytical Aspects of thePollution Control Act,” to be introduced byG. J. Dickes.Wye Room, George Hotel, Chepstow.Tuesday, 15th, 2.30 p.m.: LondonSpecial Techniques Group on “Remote Scann-Lecture Theatre A, Sherfield Building,ing Techniques.”Imperial College, London, S.W .7.Thursday and Friday, 17th and 18th: YorkThursday, 17th-Analytical Division : Annual General Meeting ;Meeting on “Pyrolysis Techniques for Analy-“Analytical Pyrolysis,” by C. E. R. Jones.“The Pyrolytic Identification of OrganicMolecules : Mass Spectrometry us. GasChromatography as the Analytical Finish,”by G. Ingram.“The Use of Thermal Degradation for theCharacterisation of Textile Materials :Pyrolysis GC and Thermogravimetry, ’’J. S. Crighton.2.30 p.m.sis”; 3.30 p.m.Informal Dinner; 7 p.m. for 7.30 p.m.Friday, 18th, 10 am.-“Automated Analysis of Tyre Rubber Blendsby Computer-linked Pyrolysis Gas Chroma-tography,” by G. L. Coulter and W. C.Thompson.“The Identification of Formulated Drugs byPy-GC-MS,” by W. J. Irwin and J . A.Flack.“Forensic Applications of Analytical Pyroly-sis Techniques,” by B. B. Wheals.Royal Station Hotel, Station Road, York.[continued inside back cove

ISSN:0306-1396    

DOI:10.1039/AD97714BX007

出版商:RSC    

年代:1977

数据来源: RSC

摘要:

Vol. 14 No. 2 Proceedings February 1977 of the Analytical Division of the Chemical Society Society for Analytical Chemistry Gold and Silver Medals On the recommendation of its Honours Commit- tee, the Council of the Analytical Division, at its meeting on December 14th, 1976, awarded the twelfth Society for Analytical Chemistry Gold Medal to Professor T. S. West Director of the Macaulay Institute for Soil Research, Aberdeen, and the fourth Society for Analytical Chemistry Silver Medal to Dr.J. S . Hislop of the Atomic Energy Research Establishment, Harwell. Analytical Division Distinguished Service Award On the recommendation of its Honours Com- mittee, the Council of the Analytical Division, at its meeting on December 14th, conferred the second Analytical Division Distinguished Service Award on Dr.D. C. Garratt Scientific *4dviser, Pharmaceutical Society of Great Britain, London. Reports of Meetings Scottish Region The forty-second Annual General Meeting If the Region was held a t 5 p.m. on Friday, November 5th, 1976, a t the University of Strathclyde, Glasgow. The Chair was taken by the Chair- man of the Region, Dr. J. M. Ottaway. The following office bearers were elected for the forthcoming year: Chairman-Dr.A. M. Ure. Vice-Chairman-Dr. G. C. Cochrane. Honorary Secretary-Dr. J. E. Whitley, Scottish Univer- sities Research and Reactor Centre, East Kilbride, Glasgow, G75 OQU. Ho9zorary Treasurer-Dr. J. M. Ottaway. Honorary Assistant Secretary-Mr. A. F. Fell. Members of Committee-Dr. P. Bowden, Mr. N. Cadzow Dr.G. S. Fell, Dr. M. Masson, Dr. G. Topping and Dr. D. E. Wells. Dr. B. W. East and Mr. J. S. Foster were re-appointed as Honorary Auditors. Midlands Region The twenty-second Annual General Meeting of the Region was held at 6.15 p.m. on Tuesday, November 23rd, 1976, a t the Boots Pure Drug Co. Ltd., Nottingham. The Chair was taken by the Chairman of the Region, Dr. A. Townshend. The following office bearers were elected for the forthcoming year: Chairman-Dr.A. Town- shend. Vice-Chairman-Mr. D. M. Peake. Honorary Secretary-Dr. R. S. Barratt, En- vironmental Protection Unit, Environmental Department, 120 Edmund Street, Birmingham, B3 2EZ. Honorary Treasurer-Dr. J. N. Miller. Members of Committee-Professor R. Belcher, Dr. R. K. Bramley, Mr. D. M. Evans, Dr. A.G. Fogg, Dr. G. C. Gidley and Mr. S. Greenfield. Mr. W. G. Harris and Mr. H. Pugh were re-appointed as Honorary Auditors. , East Anglia Region The ninth Annual General Meeting of the Region was held a t 2.15 p.m. on Thursday, November 25th, 1976, a t the Research and Technology Centre, Spillers Ltd., Cambridge. The Chair was taken by the Chairman of the Region, Mr. A. W. Hartley.The following office bearers were elected for the forthcoming year : Chairman-Dr. D. Simpson. Vice-Chairmun- Mr. J. Dutton. Honorary Secretary and Treasurer-Mr. A. G. Croft, Spillers Ltd., Research & Technology Centre, Station Roaci, Cambridge, CB1 2 JN. Members of Committee- Dr. D. Christopher, Mr. A. W. Hartley and 1920 REPORTS OF MEETINGS PYOC. Analyt. Div. Chem. SOC.Dr. R. Whiteoak. Dr. A. N. Worden and ant Secretary-Mr. D. G. Porter. Members of Mr. C. E. Waterhouse were re-appointed as Committee-Mr. C. L. Denton, Dr. B. Fleet, Honorary Auditors. Mr. S. R. Hill, Mr. J. Stevens and Mr. K. Swann. Dr. J. E. Page and Mr. W. H. C. Shaw were re- Chromatography and appointed as Honorary Auditors. The twelfth Annual General Meeting of the Group was held at 2.30 p.m.on Tuesday, The eleventh Annual General Meeting of the November 30th, 1976, at the BP Refinery, Group was held at 2.30 p.m. on Tuesday, Grangemouth. The Chair was taken by the November 30th, 1976, in the Geological Society Chairman of the Group, Dr. G. H. Jolliffe. The Lecture Theatre, Burlington House, London, following office bearers were elected for the W.l.The Chair was taken by the Chairman of forthcoming year: Chairman-Dr. G. H. Jolliffe. the Group, Dr. W. Carr. The following office Vice-chairmanMr. D. A. Elvidge. Honorary bearers were elected for the forthcoming year: Secretary and Treasurer-Dr. D. Simpson, Chairman-Mr. B. Scarlett. Vice-Chairman- Analysis for Industry, Factory 2, Bosworth Mr. R. W. Lines. Honorary Secretary and House, High Street, Thorpe-le-Soken, Essex, Treasurer-Mr.M. W. G. Burt, Atomic Weapons C016 OEA. Members of Committee-Dr. F. K. Research Establishment, Building B9C5, Alder- Butcher, Dr. C. E. R. Jones (co-opted), Mr. J. W. maston, Berks. Honorary Assistant Secretwy- Murfin, Mr. P. F. Wadsworth and Mr. V. C. Dr. R. Wilson. Members of Committee-Dr. W. Weaver. Dr. S. J. Purdy and Mr.J. S. Wragg Carr, Dr. M. J. Groves, Mr. J. E. C. Harris, Mr. were re-appointed as Honorary Auditors. J. L. F. Kellie, Dr. N. A. Orr and Dr. N. G. Stanley-Wood. Mr. P. W. Shallis and Dr. T. Allen were re-appointed as Honorary Auditors. Electrophoresis Group Size Analysis Group Thermal Methods Group The twelfth Annual General Meeting of the Group was held at 10 a.m. on Friday, November 19th, 1976, in the University Hall, University of Bath, Claverton Down, Bath. The Chair was taken by the Chairman of the Group, Dr.F. W. Wilburn. The following office bearers were elected for the forthcoming year : Chairman- Dr. F. W. Wilburn. Vice-Chairman-Dr. R. H. Still. Honorary Secretary-Mr. C . J . Keattch, Industrial & Laboratory Services, P.O. Box 9, Lyme Regis, Dorset.Honorary Treasurer- Dr. A. A. Hodgson. Members of Committee- Dr. L. s. Bark, Dr. P. A. Barnes, Mr. J. Bather, Mr. E. L. Charsley, Dr. S. A. A. Jayaweera, Mr. P. W. Lawson, and Dr. R. C. Mackenzie (co-opted). Dr. W. Boardman and Mr. P. J. Haines were re-appointed as Honorary Auditors. Radiochemical Methods Group The tenth Annual General Meeting of the Group was held at 1.45 p.m.on Thursday, November 18th, 1976, at Hoechst Pharmaceutical Research Laboratories, Milton Keynes, Bucks. The Chair was taken by the Chairman of the Group, Dr. P. Johnson. The following office bearers were elected for the forthcoming year: Chair- man-Dr. G. W. A. Newton. Vice-chairman- Mr. G. A. Sutton. Honorary Secretary- Mr. M. A. Crook, Department of Chemistry and Polymer Technology, Polytechnic of the South Bank, Borough Road, London SE1 OAA.Honorary Treasurer-Mr. D. A. Ginger. Hono- rary A ssistant Secretary-Mr. J. W. McMillan. Members of Committee-Dr. D. E. Bowyer, Dr. W. G. Duncombe, Professor J. H. Fremlin, Mr. J. A. B. Gibson, Dr. D. M. Taylor and Dr. A. R. Ware. Mr. G. Farmer and Dr. P. The Meeting Of the Johnson were appointed as Honorary Auditors. Group was held at 2p.m. on Wednesday, Automatic Methods Group December Sth, 1976, in the Chemistry Depart- ment, Imperial College, London, S.W.7. The Chair was taken by the Chairman of the Group, Mr. D. C. M. Squirrell. The following office bearers were elected for the forthcoming year: Chairman-Mr. D. C. M. Squirrell. Vice- ChairmanMr. J. L. Martin. Honorary Secre- tary-Dr. P. B. Stockwell, Laboratory of the Government Chemist, Cornwall House, Stam- ford Street, London, SEl 9NQ. Honorary Treasurer-Mr. K. H. Wall. Honorary Assist-

ISSN:0306-1396    

DOI:10.1039/AD9771400019

出版商:RSC    

年代:1977

数据来源: RSC

摘要:

20 REPORTS OF MEETINGS PYOC. Analyt. Div. Chem. SOC. G eochemi ca I Ana I ysis A meeting was held on December 13th, 1976, between representatives of the Mineralogical Society and the CS Analytical Division to discuss collaboration in the area of geochemical analysis. Those attending from the Mineralo- gical Society were Professor D. K. BaileyFebruary, 1977 DATA USAGE BY ANALYTICAL CHEMISTS 21 (Chairman of the Geochemistry Group), Dr.G. L. Hendry (Joint Honorary Secretary of the Geological Spectroscopy Group) and Mr. J. E. T. Horne (General Secretary), and those from the Division were the President, the Honorary Treasurer, the Chairman of the Group Liaison and Policy Committee and the Secretary. It was agreed that the interests of members of both Societies in the field of analysis could best be met by an effective exchange of information on meetings of common interest, whether arranged by the Mineralogical Society and its Groups, or by the Analytical Division and its Groups.Such meetings will be announced in Proceedings and in the Mineralogical Society Bulletin. The possibility of joint meetings was welcomed. For some meetings the Mineralogical Society will charge a registration fee for non-members. Members of the Analytical Division who have particular interests in this area may wish to know that membership of the Mineralogical Society costs LZ per annum (inclusive of their Bulletin, but exclusive of other publications). Enquiries for membership should be addressed to the General Secretary, Mineralogical Society, 41 Queen’s Gate, London, SW7 5HR.

ISSN:0306-1396    

DOI:10.1039/AD9771400020

出版商:RSC    

年代:1977

数据来源: RSC

摘要:

February, 1977 DATA USAGE BY ANALYTICAL CHEMISTS 21 CHEMICAL SOCIETY AUTUMN MEETING The Chemical Society Autumn Meeting was held at the University of Sheffield from September 21st to 23rd 1976. Included in the programme was a session organised by the Chemical Information Subject Group and the Education and Training Group entitled Data Usage by Analytical Chemists, and another session entitled Justification of Computers in Analytical Chemistry.Summaries of papers presented at both sessions are published below. Data Usage by Analytical Chemists The following are summaries of three of the papers presented a t the CS Autumn Meeting on September 22nd. Computer-based Bibliographical Information for Analytical Chemists F. E. Wood and D. Bawden Postgraduate School of Librarianship and Information Science, University of Shefield, Western Bank, Sheffield, S10 2TN Vast numbers of scientific papers are produced each year (over 400000 in chemistry), and abstracting and indexing services have problems in handling this volunie of papers so all of the largest now use computer-based methods. The files of machine-readable bibliographic data thus created are available for computer seaching.Current Awareness and Retrospective Searches File producers or their agents offer SDI (selective dissemination of information) services that supply users regularly with references to recently published papers on subjects in which they are interested. These services are tailor-made; an individual search is matched against each file of new references for each user.Charges vary with the complexity of the search and may range from about i20 a year for a simple search to several hundred pounds for a very large search; the average is about 480 a year. A cheaper way to obtain a current awareness service is to subscribe to a standard “off the peg” service. There are a number available on topics of interest to analytical chemists from, for example, UKCIS (United Kingdom Chemical Information Service) the International Food Information Service and the Institute for Scientific Information.UKCIS call their “off the peg” service Macroprofiles and charge 438 a year plus postage. Current awareness searches are run against files that are the equivalent of the current issues of abstracting or indexing publications but these files accumulate and it is possible to search backwards through the records for several years.Retrospective searches are costly because the files to be searched are usually very large.22 DATA USAGE BY ANALYTICAL CHEMISTS Proc. Analyt. Div. Chew. SOC. On-line Searching Recently, there has been a great increase in the use of on-line interactive services (where the search is carried out live at a computer terminal and can be modified as it proceeds).Although the whole file can be searched, it is usually possible to limit searches so that only recent re- ferences are retrieved. In addition, most services allow searches to be stored from one month to the next for regular current-awareness use. There are four o,n-line services that offer telephone dial-up access from this country: Lock- heed, Systems Development Corporation (SDC), the European Space Agency through the Technology Reports Centre (TRC), and the National Library of Medicine (NLM) through the UK MEDLARS service.Between them, they offer over 40 different bibliographic files, many of which have some entries relating to analytical chemistry. This choice of files, covering a variety of chemically related fields, is valuable because of the wide range of applications of analytical techniques. With on-line searches payment is made for what is used: access to a number of files is no more costly than access to any one file.Files Obviously, for anyone working in the chemical field ChemicaZ Abstracts (CA) must be of prime importance. The records in this journal (but not the abstracts) are available on-line as CA Condensates from Lockheed, SDC and TRC.The dates from which the files run vary with the service (Lockheed from January 1972 onwards, SDC from 1970 and TRC from 1969), which is a point worth noting if older material is of importance. However, the choice of which service to use is not straightforward, particularly as TRC and Lockheed use one in- formation retrieval system and SDC another, each of which has advantages for particular types of search.l CA Condensates can be searched using natural language words (indexing is by words from the title of the paper plus natural language keywords so all synonyms have to be used), author’s name, country of patent application, patent classification number, patent assignee, patent number, language, journal title and CA Publication Section.Two additional files are available only from the Lockheed service: CASIA, which can be searched using CA approved index terms, i.e., those which occur in the CA volume indexes, and by CAS Registry Numbers for specific chemical substances; and CHEMNAME, which is a dictionary file giving CAS Registry Numbers, synonyms and systematic names for each substance.TABLE I SELECTED ON-LINE FILES POTENTIALLY OF INTEREST TO ANALYTICAL CHEMISTS No. 1 2 3 4 5 6 7 8 9 10 11 12 13 File Service CA Condensates Lockheed, SDC, TRC CASIA Lockheed CHEMNAME Lockheed NTIS (Reports) Lockheed, SDC, TRC SCISEARCH (Citations) Lockheed, TRC Comprehensive Disser- tatiori Abstracts Lockheed SSIE (Smithsonian Science Information Exchange, on-going and recently completed research projects) SDC TOXLINE (Toxico1ogy)NLM CHEMLINE NLM RINCDOC (Pharm- aceu ticals) SDC BIOSIS (Biological Abstracts and Bio- research Previews) Lockheed, SDC MEDLINE (Index Medicus) NLM CANCERLINE (Cancer Chemotherapy Abstracts and other materials) NLM No.File Service 14 15 16 17 18 19 20 21 22 23 24 25 PAPERCHEM SDC CAIN (Bibliography of Agriculture) Lockheed, SDC Pollution SDC Environmental Science Index TRC ENVIROLINE Lockheed, SDC GEOREF SDC APILIT.APIPAT (American Petroleum Institute : literature and patents) SDC METADEX (metal- lurgy) Lockheed, TRC World Aluminum Abstracts Lockheed, TRC Nuclear Science Abstracts TRC INSPEC (Physics Abstracts, Computer and Control Abstracts, Electrical and Electro- nic Abstracts) Lockheed, TRC COMPENDEX (Engineering Index) Lockheed, SDC, TRCFebruary , 1977 DATA USAGE BY ANALYTICAL CHEMISTS 23 There are a number of files that cover more than just chemistry which are worth considering because they specialise in sources other than papers in periodicals; these are items 4-7 in Table I.The main advantage of SCISEARCH is that it is possible to search for papers that have cited a known relevant reference, so working forward in time.Citation searching is especially useful if the subject is difficult to define. The remainder of the files listed in Table I cover subjects bordering on chemistry, which include some analytical work, or deal with equipment or techniques used in analysis. CHEM- LINE is an interesting and developing chemical dictionary file that is an aid to searching the TOXLINE (toxicology information on-line) file.CHEMLINE can be searched by CAS Registry Number, molecular formula, molecular formula fragments, CA preferred names, synonyms, name fragments, Wiswesser line notation and ring information. Running an On-line Search The search should be prepared in advance to save costs and so some alternative approaches are ready if the search needs refining.If similar searches are carried out frequently, it may be possible to devise standard searches in which terms can be substituted.2 A telephone call is made to the nearest point in the communications network (Orpington for TRC, The Hague or Paris for the other services) and so connection is made to the service operator's computer. Then the search can be carried out with the opportunity to check the results at each stage.In general, it is most effective if searches are carried out jointly by an information specialist, with a detailed knowledge of the systems' capabilities based on frequent use, and the enquirer, to evaluate the results of the search as it proceeds.Fig. 1 shows part of a search. Fig. 1. Part of a Lockheed search of CA Condensates. Sometimes on-line searching does not retrieve as many references as a thorough manual search but it is much quicker, easier and usually is sufficient to satisfy users.3 Access to On-line Services in the United Kingdom Some academic and industrial libraries already offer on-line searches as a service to their users, while more are actively considering their introduction.The Science Reference Library will run searches on request at a reasonable cost and publishes a useful guide to services4 Cranfield Institute of Technology also offers a service to outside users. The UK MEDLARS24 PYOC. Analyt. Div. Chew. Soc. service of the British Library Lending Division will carry out searches on the NLM files and UKCIS will do searches of the CA, BIOSIS and TOXLINE files.DATA USAGE BY ANALYTICAL CHEMISTS Cost of On-line Searching On-line searching costs vary according to individual circumstances, such as the amount of searching done, but E l per minute is a rough estimate; this would include running costs, maintenance and write-off on initial outlay.A simple search combining four terms can be done in about 5 min and four fairly complicated searches can be carried out in 1 h. In consider- ing these figures, it should be remembered that few scientists attempt to work out the true cost of the manual searches they do. Future Developments This is a rapidly growing area of information provision, and new files are added frequently and improvements are made regularly to the retrieval systems.Access to systems and their reliability are improving. Likely developments include the availability of the NLM and CA files on a computer in the UK, and the establishment of a European Information Network (EURONET), which should provide dial-up access to other files that are not available at present, References 1.2. 3. 4. Prewitt, B. G., J . Chem. I n f . Comput. Sci., 1975, 15, 177. Buckley, J. S., J . Chem. Inf. Comput. Sci., 1975, 15, 161. Michaels, C. J., J . Chem. Inf. Comput. Sci., 1975, 15, 172. Leigh, J. A., "Guide to Computer-based Literature Searching Services in Science and Technology Available in the UK," Science Reference Library, London, 1976. Data Compilations of Interest to Analytical Chemists Beryl Edmonds C"213HQ Physical Property Data Service, The Institution of Chemical Engineers, 165-171 Railway Terrace, Rugby, The scientific community has an increasing awareness of the need for good data.Analysts in particular have always recognised this, as witnessed by collections such as Beilstein, Landolt-Bornstein, Gmelin, etc. Certainly it is a field in which developing technology has produced a host of new analytical tools, necessitating the compilation of new sets of measure- ment parameters.The data required by the analyst will be determined by the techniques he uses and will range from the description of a well analysed sample (an index of suppliers of different sample types may be his most useful source) to a bank of spectral data for comparison with his unknown sample.The latter field has received a great deal of attention and it is details of spectral-data activities that will comprise most of this summary. Infrared Spectra The development of data activities in infrared spectra is fairly typical, involving several organisations. Initially spectra were supplied on sheets, with associated indexes, by the Thermodynamics Research Centre (TRC) for hydrocarbons and derivatives, by the Sadtler Research Laboratory for commercial organic compounds, including pharmaceuticals, and by the Coblentz Society for a range of pure compounds.The Documentation of Molecular Spectroscopy (Rutterworths and Verlag Chemie) and the Infrared Data Committee of Japan also supplied infrared spectral data, the former on inorganic as well as organic compounds but in these instances spectra were supplied on notched cards with coded classification in order to provide a means of identifying a certain substituent group, carbon skeleton or particular spectral feature.The methods of evaluation vary from selection on the basis of the investigator's competence and instrument quality to preparation of the spectra by quali- fied experts. Finally, spectra from all of these sources plus additional data from the scientific journals were collected and indexed by the American Society for Testing and Materials (ASTM).InFebruary, 1977 DATA USAGE BY ANALYTICAL CHEMISTS 25 addition to spectral-data cards an index was prepared on IBM cards and magnetic tape accord- ing to both a molecular formula and a serial number list. A computerised search system was also provided to permit identification of unknowns or spectra of particular interest.Several organisations have used this ASTM file as a data source in computerised search facilities. Current activities are the Infrared Data Retrieval Program of DNA Systems Inc. ; the Infrared Data Retrieval Programs of Chemir Laboratories; the Infrared Information System of Sadtler Research Laboratories ; and the Search Program for Infrared Spectra, a recent service introduced by NRC in Canada and only available there, Ultraviolet and Visible Spectra A similar picture emerges from an examination of data compilations for the ultraviolet and visible regions.TRC and Sadtler Research Laboratories provide spectra in hard copy and the Ultraviolet Atlas of Organic Compounds (Butterworths and Verlag Chemie) parallels the Documentation of Molecular Spectroscopy.Additional compilations are provided by Organic Electronic Spectra Inc. and Lang’s Absorption Spectra. Despite the collation of Over 25 000 spectra by ASTM no attempts appear to have been made to use a computerised search system.Atomic-absorption and Flame Spectroscopy A set of spectral-data activities parallel to those mentioned above are concerned with the basic data relating to atomic-absorption and flame spectroscopy. These data are dealt with by a number of data centres based at the National Bureau of Standards and supported by the Office of Standard Reference Data, compiling atomic energy levels, atomic transition proba- bilities, energy levels and atomic collision data.Useful handbooks include the MIT Wave- length Tables and Tables de Constantes Selectiondes. Nuclear Magnetic Resonance Spectroscopy In addition to the work of TRC and Sadtler Research Laboratories two commercial organisa- tions provide data on nuclear magnetic resonance spectroscopy, Varian Associates and the Japanese Electron Optics Lab.Co. Ltd. Both provide hard copy, the latter’s compilation being published by Sadtler. A Joint Committee on Atomic and Molecular Physical Data recommend criteria for the recording and use of nuclear magnetic resonance spectra and there is one computerised data activity, CNMR, which is a search of the carbon-13 spectra run by the Environmental Protection Agency.Mass Spectrometry Data compilations in mass spectrometry are provided by TRC, Centres d’Etudes Nucleaires de Grenoble, Atlas of Mass Spectral Data (Wiley), ASTM and the Atomic Weapons Research Establishment (AWRE) at Aldermaston. AWRE, in conjunction with the National Institute of Health and the Environmental Protection Agency in the US, provide the Mass Spectral Search System (MSSS), which is based on 39 500 spectra.A similar computerised activity is undertaken by McClaff erty at Cornell University. In addition to these major spectral activities there are several smaller ones, which are as follows: Raman spectra, TRC and the Joint Committee for Atomic and Molecular Physical Data; microwave spectra, NBS Microwave Spectra Data Activities and Landolt-Bornstein; activation analysis, NBS Centre for Activation Analysis ; Mossbauer effect, Mossbauer Effect Data Index.Of course analytical chemists use techniques other than spectral ones and these techniques have associated data centres. Some of the more recent computerised services that may be of interest are the Diffraction Data Tele Search (BDTS), which searches the powder diffraction data file of the Joint Committee of Powder Diffraction, and “Crysdata” run by the NBS, which covers many parameters concerned with the single crystal and can be used to identify crystals for which one or more of these parameters is known.In this connection there is also the Cambridge Crystallographic Data Centre. Another tool which must be mentioned is gas chromatography for which there are two main data compilations, the Gas Chromatographic Committee of Japan and the ASTM Committee on Gas Chromatography.Finally, many of these activities mentioned require the values of simple physical properties to be used in conjunction with the more specialised data peculiar to the technique. These26 proc. Analyt. Div. Chem.soc. values can be found in several places but a computerised source covering a wide range of such data is the Physical Properties Data Service (PPDS) of the Institution of Chemical Engineers. This summary contains a brief review of data compilations of possible interest to analytical chemists. DATA USAGE BY ANALYTICAL CHEMISTS Further details can be obtained from the author if required.Automatic Methods of Handling Chemical Structure and Property Information G. W. Adamson Postgraduate School of Librarianship and Information Science, University of Shefield, Western Baizlz, Shefield, S10 2TN The enquiries put to chemical information systems are often conveniently expressed in terms of chemical compounds and their properties. The information itself may also be organised in this way.For these reasons, much work has been put into developing methods of handling representations of chemical compounds in information systems.lg2 The representations are used to organise the information files and as index terms to access information associated with the compounds. This may be bibliographic information about documents containing refer- ence to the compounds, or the files may contain details of the properties of compounds, where samples may be located or purchased, and price.The automatic storage, analysis and retrieval of reaction information have also been investigated. Levels of Description of Chemical Compounds Perhaps the simplest useful representation of a compound would be its molecular formula, and this description has been used, and is still used in handling compound information.However, its usefulness is limited because it, alone, cannot distinguish between isomeric molecules. In- formation at this level is usually easily determined, coded and manipulated. An even more detailed level would be that of molecular dimensions as determined by diffraction or spectro- scopic experiments. However, the number of compounds whose molecular dimensions have been measured is of the order of a few tens of thousands, whereas the number of compounds which are known, and for which structure diagrams could be written, is of the order of several million.Thus, the structure diagram offers the best level of representation at present for general structure storage and retrieval purposes.However, the data base assembled by the Cambridge Crystallographic Data Centre is a valuable resource in its own right, as a data base of molecular dimensibns and crystal structures. The next level of description that has been widely used is the structure diagram. Coding Representations of Structure Diagrams Several methods of coding representations of structure at the level of a structure diagram have been used in information systems.An obvious method is by the use of nomenclature, either systematic or trivial. In another set of methods, fragmentation codes, the structures are broken into fragments, which could, for example, correspond to functional groups and skeletal fragments, and the structures are represented by lists of fragments. In this method, information about the relative positions of structural fragments is lost.The third of the main methods of coding structure diagrams is by means of linear notations, of which that originally devised by Wiswesser is the most widely used. In structures the features are represented by alphabetic or numeric symbols and the structure diagram is reduced to a short string of characters which can be read, manipulated and printed con- veniently.The last of the commonly used methods of coding structures is that which involves some kind of connection table. In its most explicit form, this table would be a square matrix with the same number of rows as atoms in the structure. The atomic symbols would appear on the diagonal, and the off-diagonal elements would indicate the type of bond between the atoms concerned. In this full matrix form, connection tables are very bulky but as theFebruary, 1977 DATA USAGE BY ANALYTICAL CHEMISTS 27 matrix is symmetric and most elements are zero, it can be condensed considerably.Connec- tion tables are only suitable for manipulation in a computer, whereas the other representations can be manipulated on punched card equipment or by hand, and can be used in printed indexes.The different methods of coding structure diagrams, with the exception of fragmentation codes, contain the same information and can be converted from one to another automatically. Fragment codes can be generated automatically from the other coded forms but, as an in- formation loss accompanies this process, it is not reversible.The large computer-based systems generally use more than one coded representation and may convert from one form to another automatically, in order to take advantage of particular, useful characteristics which one may have in a given application. A search may be for a single compound. Alter- natively, the search may be for a class of compounds which contain a specified substructure or combination of structural fragments.In this type of search, termed substructure searches, the questions may be very complicated and include alternative structural fragments, or specify that certain types of fragment should not be present. Searches for chemical structures fall into two main types. This type of search is commonly called a “registration” type search.Automatic Structure - Property (Structure - Activity) Correlation Recently, attention has been given to the investigation of automatic structure - property correlation. Methods and computer programs for manipulating the structural information have been developed for use in storage and retrieval, and program packages are available for the statistical analysis of large amounts of data.Over a number of years, large machine- readable files of structures and properties have also been built up. The availability of these three components means that for some organisations the extension of a structure - property storage and retrieval system to become a structure - property correlation and prediction system would be a relatively small step. A term recently suggested for the class of empirical structure - property correlation methods using machine-readable structure files is “substructural analy~is.”~ Most of these methods fall into two groups, one using classification methods and the other using regression analysis.Automatic Classification of Chemical Structure Information The classification of structural information is of interest both for possible application in information storage and retrieval and for structure - property correlation.The methodology and terminology of automatic classification are easily confused because of the partly inde- pendent development of similar methods by workers in different fields, numerical taxonomy by biologists, pattern recognition by computer scientists and automatic classification by information scientists.Pattern recognition and its terminology is probably the most widely used in chemistry. In supervised clas~ification,~ structures are placed into one of two or more pre-defined classes, whereas in the unsupervised methods5 the structures are placed in classes by procedures which need no information on class membership to start the process.These methods have been shown to produce classi- fications that are sensible from a chemical viewpoint, and which show some correlation with the properties of the compounds. However, it would be very costly at present to apply this kind of method to medium to large files of the order of 104-106 structures. Automatic classification methods fall into two main groups. Regression Analysis Several methods of structure - property correlation using regression analysis have been described.Connection tables6 and the Wiswesser Line Notation’ have been used and struc- ture has been directly correlated with biological activity and physical properties. The assumption underlying these methods is that the property value for a compound is a linear or simple non-linear function of contributions from the structural fragments present in the compound. The methods usually produce statistically significant correlations and estimates of the contribution which structural fragments make to the property. In favourable circumstances unknown property values can also be predicted.28 COMPUTERS IN ANALYTICAL CHEMISTRY Proc. Analyt. Div. Chem. SOC. Conclusions Chemical information systems including structural information are widespread in the chemical industry, especially in the areas of agrochemicals and pharmaceuticals, although they are not yet much used by chemists in academic institutions. If past trends continue their use will continue to increase and it will become more important for practising chemists to be aware of their uses and limitations. References 1. Lynch, M. F., Harrison, J. M., Town, W. G., and Ash, J . E., “Computer Handling of Chemical Struc- 2. Ash, J . E., and Hyde, E., “Chemical Information Systems,” Ellis Horwood, Chichester, 1975. 3. Cramer, R. D., 111, Redl, G., and Berkoff, C. E., J. Med. Chem., 1974, 17, 533. 4. Chu, K. C., Analyt. Chem., 1974, 46, 1181. 5. Adamson, G. W., and Bush, J . A., Inf. Stor. Retrieval, 1973, 10, 561. 6. Adamson, G. W., and Bush, J . A., Nature, Lond., 1974, 248, 406. 7. Adamson, G. W., and Bawden, D., J . Chem. Inf. Comput. Sci., 1975, 15, 215. ture Information,” Macdonald, London, 197 1.

ISSN:0306-1396    

DOI:10.1039/AD9771400021

出版商:RSC    

年代:1977

数据来源: RSC

摘要:

28 COMPUTERS IN ANALYTICAL CHEMISTRY Proc. Analyt. Div. Chem. SOC. Justification of Computers in Analytical Chemistry The following is a summary of one of the papers presented at the CS Autumn Meeting on September 21st, 1976. Computer Systems in a Steelworks Laboratory L. Gwilliam British Steel Corporation, Port Talbot Works, Port Talbot, South Glamorgan, Wales During the past decade a number of computer systems have been designed and installed in steelworks laboratories. Three systems will be described, two of which have been installed and are in current use at the Central Laboratory, British Steel Corporation, Port Talbot Works.The third is being designed for the future steelworks laboratory. The new, central, production-control laboratory was designed in 1967 so that large numbers of samples could be analysed rapidly and accurately.The analysis systems were designed for a wide range of materials such as those used and produced in an integrated steelworks and the laboratory was equipped with a wide range of analytical instrumentation, including direct- reading optical emission spectrometers, X-ray fluorescence spectrometers, atomic-absorption spectrometers and a variety of smaller instruments used for the analysis of carbon and gases in iron and steel.A large, complex computer system based on a Myriad I1 computer, which had a 32K core, a 24-bit word, a 1.5-ps word time and a 2.4 million word disc, was designed for the BOS Plant development and the laboratory system was incorporated into the scheme. Each of the main instruments, i.e., the direct-reading emission spectrometer and the X-ray fluorescence spectrometer, is connected via an interface to the computer and the interface is used to identify samples and their source and to alert the computer with an enter pulse that the analyser is on-line.When the enter pulse is received the computer reads the sample identifi- cation and when the integration is terminated a pulse alerts the computer and reading of the element channels commences.The computer waits for an ADC balance pulse from the digital voltmeter, reads the channel and instructs the analyser to move to the next channel. This process continues until the final channel is read and a re-set pulse is given to the analyser and computer. The voltage readings are converted to percentage values from the calibration graphs stored in the computer and the analysis of the sample is displayed on the touch-wire television screen.The analysis is vetted by the chemist and the results, after acceptance, are transmitted by the computer to the correct customer teletype. When a new automatic X-ray fluorescence spectrometer was installed in 1975 it was fitted with a dedicated computer, PDP8M 12-bit word and 12K store so that results of an analysis could be produced more quickly and accurately.The instrument was fitted with 20 elementFebruary , 197 7 COMPUTERS IN ANALYTICAL CHEMISTRY 29 channels, 18 fixed and two variable, and was designed for the analysis of irons, steels and non- metallic materials. Methods of analysis need to be continually developed and updated in order to maintain efficiency and so the computer system was designed to give the maximum number of optimums and modes of operation.There are six methods of operation programmed into the computer system. Run Type 0-Intensity printout The system prints out the intensities of any combination of channels requested. Run Type 1-Concentration calculation and output The data are acquired from all channels and checks are made for error conditions.The intensities are converted to concen- tration by interpolation/extrapolation, applying the linear relationship The system asks for sample number and material identity. where C, = concentration for element X; I , = intensity for element X; C, = upper concen- tration limit ; I= = associated intensity; C, = lower concentration limit ; and I , = associated intensity.The element concentrations are corrected by applying the inter-element correction factors to all elements, starting with the lower concentration: Ccorrect = Capparent (1 + W l + K,C, + - - * +K,C,) where Ki is the correction factor for an interfering element i on a single element X, and Ci is the concentration of element i.The corrections are carried out in three phases: 1. 2. 3. Sort elements into ascending order of concentration. Apply the inter-element correction factors. Restore the elements to the original order for printout. Run Type 2-Concentration calculation and output with a n internal standard This system is similar to Run Type 1 but the intensity data for iron and cobalt are used t o give an intensity ratio, IFe/lCo, which is plotted against C,, to give the concentration of iron before applying the inter-element corrections.Run Type 3-Concentration calculation and output with repeatability from the sample. to give the mean analysis. Run Type 3 is similar t o Run Type 1 but allows the operator to input up to three sets of data The computer selects the two sets of data with least error for processing Run Type 4-Concentration calculation and output with internal standard and repeatability Run Type 4 is the same as Run Type 3 with the addition of the repeatability function.Run Type 5-Calibration The calibration data in this system are comprehensive and allow up to six calibration standards to be used for each material.The calibration data set up indicate one of the following: a negative value-it is required to update the lower standard intensity I(L); a zero value-ignore this channel; a positive value-it is required to update the high standard intensity I(H). Regardless of any drift error the concentration data I(H) or I(L) are updated with the latest intensity. The data held for the analysis system consist of concentration calibration and correction data for 14 materials and channel arrays for 5 combinations of elements.With the computer system described above it is possible to evaluate and use most of the current methods of X-ray fluorescence analysis for irons, steels and allied materials. The suggested system design of a future steelworks laboratory takes advantage of manufac- turers’ developments in equipment for analysis.Many of the newly designed instruments are computer controlled and have automatic monitoring and alarms for instrument malfunction.30 Proc. Analyt. Div. Chem. SOC. The computer systems provide a variety of functions such as automatic re-calibration; selection of programmes, i.e., number of elements, source conditions and other instrumental parameters ; averaging of results ; processing and transmitting information for production control ; and checking of specifications. The whole analysis, whether performed chemically or with small instruments, together with results obtained from the computer-controlled instruments, can be collated and output as shift or daily logs. Control check systems can be built in to alarm automatically when results deviate from normal. When these functions are linked together with a laboratory computer system more efficient management control is possible. ORIGINAL PAPERS IN PHARMACEUTICAL ANALYSIS

ISSN:0306-1396    

DOI:10.1039/AD9771400028

出版商:RSC    

年代:1977

数据来源: RSC

摘要:

30 ORIGINAL PAPERS IN PHARMACEUTICAL ANALYSIS Proc. Analyt. Div. Chem. SOC. Original Papers in Pharmaceutical Analysis The following are summaries of four of the papers presented at a Meeting of the Joint Phar- maceutical Analysis Group held on June 15th, 1976, at the Pharmaceutical Society of Great Britain, London. Use of Reversed- phase High -perf ormance Liquid Chromatography in the Analysis of Products Containing Halcinonide and Triamcinolone Acetonide G.Gordon and P. R. Wood International Development Laboratory, E. R. Squibb and Soms, Reeds Lane, Moreton, Wirral, Merseyside, L46 IQW Halcinonide (I) and triamcinolone acetonide (11) are corticosteroids marketed as anti- inflammatory agents in a number of topical dosage forms (creams, ointments and tinctures).In addition, triamcinolone acetonide is manufactured in an injectable form. CHzCI 1 c=o I Halcinonide I I Triamcinolone acetonide Halcinonide The development of formulations containing halcinonide coincided with the increase in use and importance of high-performance liquid chromatography (HPLC) as an analytical tool. Thus the assay development necessary to support formulations and stability studies was directed towards the use of this technique.Stability-indicating assay procedures were required for cream and ointment formulations containing halcinonide (0.1 yo m/m) in combination with neomycin and either nystatin or amphotericin B. Assay development was also required for a tincture formulation, essentially halcinonide and salicylic acid dissolved in aqueous ethanol.Conditions for the reversed-phase HPLC of halcinonide had been established previously1 and thus it was necessary to develop suitable extraction procedures for halcinonide and to extend the validation of the HPLC method to include an examination of its ability to indicate degradation of halcinonide in the above products. The conditions for the HPLC of halcinonide were as follows: instrument, a Varian 4000 dual-beam, 254-nm detector; column, 1 m x 2.6 mm i.d., stainless steel, dry packed with phenyl Corasil (37-50 pm); solvent, 200 ml of acetonitrile and 320 ml of methanolFebruary, 1977 ORIGINAL PAPERS I N PHARMACEUTICAL ANALYSIS 31 diluted to 1000 ml with water; sensitivity, 0.04; flow-rate, 0.8 ml min-l (700 p s i .) ; tem- perature, ambient.Initially, analysis of the tincture was carried out simply by dilution followed by HPLC. However, while satisfactory results were obtained for the analysis of a small number of sam- ples, analysis of large numbers of samples gave rise to an increasingly erratic base line. This effect was attributed to the presence of large amounts of salicylic acid relative to steroid (20: 1) in the formulation.A suitable procedure was found to be dispersion of the sample in 0.3 M sodium hydroxide solution and extraction of the halcinonide with chloroform followed by backwashing of the chloroform extract with distilled water. After removal of the chloroform, the residue was dissolved and diluted to an accurately known volume with methanol. The recovery and precision information obtained by using this procedure is given in Table I.Cream formulations are often the most difficult of pharmaceutical preparations for which to devise suitable assay procedures. The presence of oils, waxes and emulsifiers can cause difficulties in extraction and frequently result in interference in the final stages of the assay. In the halcinonide cream and ointment formulations there is the added complication of interference by the polyene antibiotics, especially for samples in which some antibiotic degradation may have occurred.Simple partitions between, for example, 2,2,4-trimethylpentane - methanol and acetonitrile - hexane were examined and found to be unsuitable, giving low recoveries of halcinonide. The procedure finally found to be suitable involved mixing a sample with Celite and eluting the halcinonide and some excipients directly on t o a chromatographic column (1.5 x 25 cm) packed with Florisil (log), using chloroform.Further washes with a mixture of chloro- form - hexane (60 + 40 V / V ) ensured complete extraction and eluted a large proportion of co-extracted excipients from the Florisil column. Halcinonide was then eluted from the colunin using 274, of water in acetone and, after removal of the solvent and dissolution of the residue in a known volume of methanol, was determined by HPLC.It was necessary, therefore, to remove the salicylic acid. TABLE I RECOVERY OF HALCINONIDE FROM PREPARATIONS Product (containing 0.1 yo m/m Coefficient Number of of halcinonide) Recovery, yo of variation, % determinations Nystatin Cream Amphotericin B Cream Nystatin Ointment Amphotericin B Ointment Tincture 100.3 100.3 100.0 98.3 99.1 0.8 0.7 1.2 0.3 1.2 7 7 8 7 11 These results were obtained by means of simple on-flow injection, using a repeater syringe and with no internal standard.Subsequent work has shown that testosterone propionate can be used as an internal standard. The validity of the HPLC assay as a means of detecting halcinonide losses due to degradation was confirmed by using the following techniques.It was assumed that, in the formulations under study, the most likely degradation route would be hydrolysis resulting in formation of the 21-hydroxy compound and possibly, in extreme instances, in elimination of the acetonide gFoup. Authentic samples of these compounds were shown to be well separated from hal- cinonide, eluting close to the solvent front.A degraded sample of halcinonide was prepared by refluxing the steroid in aqueous propylene glycol with a trace of copper(I1) acetate. The resulting product was assayed by HPLC and an established TLC procedure. Comparable results were obtained. Degradation zones observed on TLC were removed and examined using HPLC.Thus it was concluded that the HPLC system indicated stability. None of the peaks obtained overlapped with the halcinonide peaks. Triamcinolone Acetonide Investigations of the behaviour of triamcinolone acetonide in reversed-phase HPLC re- sulted in the development of stability assays for this steroid in cream, ointment and sus- pension products.32 Proc.AnaZyt. Div. Chem. SOC. The conditions for HPLC were as follows: instrument, home-made coil, nitrogen carrier gas, gas pressure solvent pump and a suitable 254-nm detector; column, 25 cm x 4.6 mm id., stainless steel, slurry packed with 10-pm Spherisorb ODs; solvent, methanol - water, 56 + 44 V/V, flow-rate 1.2-1.5 ml min-1; temperature, ambient ; internal standard, prednisolone. ORIGINAL PAPERS IN PHARMACEUTICAL ANALYSIS The recovery results obtained for the various products are given in Table 11.TABLE I1 RECOVERY OF TRIAMCINOLONE ACETONIDE FROM PREPARATIONS Coefficient of Number of Product Recovery, % variation, yo determinations Triamcinolone acetonide cream, Triamcinolone acetonide Triamcinolone acetonide 0.1% m/m 99.8 0.7 5 with halquinol cream, 0.025% m/m 99.2 0.94 10 2 mg ml-1 99.6 0.75 7 6 mg ml-1 100.5 0.5 7 suspensions : Details of the extraction procedures used for the triamcinolone acetonide products and the validation of the method as indicative of stability have been published elsewhere.2 Many papers have been published on the HPLC of drug substances and related compounds; however, few papers describe the application of HPLC to the quantitative analysis of pharmaceutical products.It was our intention to present our work as a quantitative appli- cation of HPLC, giving the relevant statistical data. These assay procedures have proved to be time saving and precise. The procedure for halcinonide has now been in use for about 3 years, during which time few problems have been encountered and over 2000 assays have been performed.References 1. 2. Petrie, G., and Poet, R., unpublished work. Gordon, G., and Wood, P. R., Aqzalyst, 1976, 101, 876. Comparison of Bioautography Using a Mycoplasma as Test Organism with Bioautography Using a Bacterium as Test Organism R. F. Cosgrove International Development Laboratory, E. R. Squibb and Sons, Reeds Lane, Moreton, Wiwal, Merseyside, L46 1Q W Bioautography is a well documented technique that is applicable to most antibiotics for the differentiation of biologically active components from biologically inactive components produced on chromatograms.It was first reported using paper chromatograms by Goodall and Lev9 in 1946 and using thin-layer plates by Fischer and Lautner2 in 1961.Many micro- organisms have been used for bioautography over the years, including bacteria, fungi, algae and protozoa. Formulation development work on a new antimicrobial compound that has antibacterial activity and antimycoplasmal activity necessitated a comparison being made of bioauto- grams produced using Staphylococcus aweus as test organism with bioautograms produced using Mycoplasma gallisepticum as test organism.To the author’s knowledge, mycoplasmas, the smallest known free-living forms of life that multiply in cell-free culture media, have not been used for bioautography. They differ from viruses and rickettsiae in that they do not require living cells for growth, and from bacteria in that they do not have a rigid cell wall nor cell-wall mucopeptide or its precursors.TheyFebruary, 197 7 ORIGINAL PAPERS IN PHARMACEUTICAL ANALYSIS 33 can generally pass through bacterial filters and may be as small as 125nm in diameter. They have very fastidious growth requirements in vitro and they are not generally used as routine microbiological test organisms. The bioautography of the compound with S. aureus as test micro-organism utilised standard procedures.For thin-layer chromatography, Merck F-254 silica-gel plates were used. There was a choice of two solvent systems : dichloroethane - ethanol - formic acid or butyl acetate - methanol - ammonia. Samples were prepared in 3 + 2 chloroform - methanol. The solvent was allowed to develop to a distance of 12 cm from the base line. There was a choice of two spray reagents for chemical detection : either 2 N sulphuric acid, which produces a yellow- ish brown zone on a white background, or anisaldehyde reagent, which produces a blue zone on a pink background.The plates were developed in duplicate : one was sprayed for chemical detection and the other used for bioautography. The S. aureus was grown for 16 h on an agar slope and washed into sterile saline to produce 60% transmission at 620 nm.A 2-ml volume of this suspension was used per 100 ml of antibiotic medium No. 4 (yeast beef agar). Inoculated agar was poured into a suitable flat-bottomed dish and allowed to solidify. The thin-layer chromatographic plate for bioautography was then inverted on lens tissue and placed on the inoculated agar surface for 30min.After removal of the thin-layer chromatographic plate and lens tissue, the agar plate was incubated for 16 h at 37 "C. In- hibition zones could be seen clearly against a translucent background of bacterial growth. Using M . gallisepticum, a thin-layer chromatographic system identical with that described above could be utilised but certain modifications had to be made to the bioautography procedure.Conditions for the growth of mycoplasmas in vitro are far more demanding than that of S. aweus and a complex agar medium containing Difco PPLO broth base, horse serum, yeast extract, glucose, nicotinamide adenine dinucleotide and arginine was required. A 100-ml volume of this medium was poured uninoculated into a sterile shallow glass- bottomed tray and allowed to solidify.The plate for the bioautogram was then inverted on lens tissue and placed on to the agar surface to allow diffusion from the thin-layer chromato- graphic plate to the agar plate. After 20min, the thin-layer chromatographic plate and lens tissue were removed. The surface of the agar was inoculated with 1.0 ml of a 24-h actively growing broth culture of M . gallisepticum, spread over the agar surface with the aid of a glass rod.After the culture had dried on the agar surface, the plate was sealed in a polythene bag, which produced the correct conditions of aeration and humidity for the growth of the mycoplasma. Differentiation of the zones was improved by spraying the plate with 0.1% phenol red solution. The mycoplasmal growth appears yellow with red zones of inhibition.To obtain reasonably sized zones of inhibition, the loading of antibiotic on the thin-layer chromatographic plate had to be much reduced, as mycoplasmas are far more sensitive to the compound than is S. aureus. Thus, a 150-pg loading with S . aureus 3s test organism had to be reduced to a 2.5-pg loading with M . gallzsepticum as test organism.This requirement presented some difficulties when monitoring accelerated stability samples of the compound for degradation. Degradation spots detected by thin-layer chromatography at a 150-pg loading were not detected at the 2.5-pg loading. This problem was overcome by using a 150-pg loading for the thin-layer chromatography. Then, by examining the developed plate under ultraviolet light, the main component spot could be located and re- moved.The thin-layer chromatographic plate could then be applied as before to the agar plate for bioautography of the remaining degradation spots. It is concluded that the use of mycoplasma species as organisms of detection in bioauto- graphy is feasible and that the method is reproducible and differs from bacterial bioauto- graphy only in the use of a more complex growth medium and an increased period of incubation.Incubation followed at 37 "C. After 48-72 h, zones of inhibition were visible. References 1 . Goodall, R. R., and Levi, A. A., Nature. Lond., 1946, 158, 675. 2. Fischer, R., and Lautner, H., Arch. Pharm., Weinheim, 1961, 294, 1 .34 Analysis of Candicidin and Related Polyene Antibiotics by Means of the Coil Planet Centrifuge ORIGINAL PAPERS IN PHARMACEUTICAL ANALYSIS Proc.Analyt. Div. Chem. SOC. J. W. Lightbown and Miss P. Newland Division of Antibiotics, National Institute f o r Biological Standards and Control, Hampstead, London, N W3 6RB 1. A. Sutherland and J. W. A. Dymond Division of Engineering, National Institute for Medical Research, Mill Hill, London, N .W.7 In considering the need for international standards for candicidin and trichomycin,l the WHO Expert Committee on Biological Standardization was concerned by a claim that the two materials were essentially the same.2 Collaborative studies of samples of candicidin and trichomycin being considered for use as international standards failed to distinguish one from the other on the basis of ultraviolet and infrared spectroscopy, chromatography and nuclear magnetic resonance and mass spectroscopy.Biological studies of relative activities against a range of sensitive organisms suggested, however, that the materials were different. Counter- current distribution studies, which had formed the basis of the original report of their near identity, were not considered to be satisfactory because of the necessary duration (several days) of the experiment and the known instability of these polyene antibiotics.The use of the coil planet centrifuge, which allowed counter-current separations to be carried out on a micro-scale, was described by Ito et aL3 This method was applied in our laboratories to an examination of candicidin and trichomycin, but methods of detection were insufficiently sensitive to allow quantitative analysis and the PTFE tubing used was per- meable to the solvents used, so that only encouraging but indefinite results were obtained.Later modifications* of the apparatus to a continuous process were also unsatisfactory in our hands. The further development of this technique and equipment has, however, allowed unequivocal results to be obtained.By identifying and controlling a number of previously uncontrolled variables, such as temperature, rotational speed and vibration, a procedure has been developed by Sutherland and Sharpe5 that allows reproducible separations to be carried out and a theoretical treatment of the data allows the calculation of partition coefficients of the separated compounds.240 180 120 60 Time from sample injection to collection/min Fig. 1. Separation of four polyene antibiotics using the coil planet centrifuge. Coil volume, 110 ml; sample load, 600 pg; solvent system, chloroform - methanol - borate buffer (4+4+3). Material completely soluble in mobile phase (P= 1.0) would be eluted at 60 min. A, Candicidin; B, levorin; C , trichomycin; and D, hamycin.Febviinvy, 1977 ORIGINAL PAPERS I N PHARMACEUTICAL ANALYSIS 35 The apparatus consists of a number of interconnected separation columns that are con- strained to rotate in a planetary fashion.In this way, tubes to and from the column do not twist, so that rotating seals are unnecessary. Each column is a helically wound tube that contains two immiscible solvent phases.The light phase is pumped through the columns while the heavy phase is held stationary under the opposing action of the inertia forces from the rotating acceleration vector and the drag forces from the mobile phase flow. A sample injected with the mobile phase will therefore partition between the retained stationary phase and the pumped mobile phase. Sample constituents retained in the column in the latter stages of a separation can be eluted quickly by pumping the heavier phase as the mobile phase. Using the system 4 + 4 + 3 chloroform - methanol - borate buffer (pH 8.2), a separation of candicidin components can be completed in 4 h, although the components of most interest are recovered in periods varying from 1 to 24 h.In this period, separations were achieved that would require 1 000-2 000 transfers in a conventional counter-current procedure.Fig. 1 shows separations obtained using the candicidin and trichomycin samples ; levorin and hamy- cin are included for comparison. Spectrophotometric examination of peak materials showed these to be polyene in nature. Fig. 2 shows the distribution of biological activity against Sacclznvomyces cerevisiae in relation to absorbance at 381 nm.Mixtures of candicidin and trichomycin were run and found to give the profile expected. The main biologically active peak of candicidin was collected and re-run after concentration ; a single peak was obtained. 60 100 140 Time from sample injectiodmin Fig. 2. Comparison of absorbance and biological activity for candicidin and trichomycin: (a) candicidin, 0.3 ml at 1 mg ml-I; and (b) trichomycin, 0.3 ml a t 1 mg ml-I.A, Absorbance; and B, biological activity. From the rate of movement of a peak, and the known proportions of the two immiscible phases, a value, P, can be calculated that represents the proportion of peak material in the mobile phase after correction to equal volumes.This value characterises the peak material as does K , the partition coefficient; the areas included by the various peaks would represent the proportion of that component if the absorptivity of each component was the same. Absorptivities have not yet been determined, but the proportional compositions have been calculated on the assumption that they are identical with that of the mixture, as a first approxi- mation.Table I shows the values obtained for the sample of candicidin being considered as36 Proc. Analyt. Div. Chem. SOC. possible WHO reference material, for the working standard of candicidin for the USA Food and Drug Administration and for seven different batches of candicidin from two different sources. The variation within the seven batches in the value of P for a given peak is shown as a range which varied approximately &5% about the mean. The variation in proportional composition was greater, but it appeared from this table that the proposed international reference preparation (PIRP) was a representative sample of currently available batches of candicidin.ORIGINAL PAPERS IN PHARMACEUTICAL ANALYSIS The separation of the components listed in Table I is illustrated in Fig.3. -Time Fig. 3. Separation of the components of candicidin listed in Table I. 30 20 10 0 40 30 20 10 0 & n 1 I I I 1 1 0.75 0.5 0.25 P = KI(K + 1) I l l 1 I I I I 10 5 2 1 0.5 0.25 Partition coefficient K Fig. 4. Comparison of four polyene antibiotics using the coil planet centrifuge : (u), candicidin, PIRP; ( b ) , levorin; (c), trichomycin; ( d ) , hamycin sample 1; and ( e ) , hamycin sample 2.Fig. 4 compares diagrammatically similar data obtained for candicidin, trichomycin, levorin It shows clearly that the PIRP candicidin was different in nature and com- and hamycin.Febridavy, 1977 ORIGINAL PAPERS IN PHARMACEUTICAL ANALYSIS TABLE I COMPARATIVE COMPOSITIONS OF CANDICIDIN PREPARATIONS P = K / ( K + 1) where K = partition coefficient. 37 Batches (7) from current production of two manufacturing sources PIRP FDA working standard A 1 Mean Range Mean Range -- P Content, yo Component * P Content, P Content, f-A-, & % % 20.0 8.8-29.2 1 0.91 17.5 0.93 15.4 0.96 0.91-1.00 2 -1 0.67 3.6 0.72 2.9 0.70 0.67-0.74 3.9 2.6-6.3 2B 0.55 16.0 0.56 14.6 0.56 0.53-0.59 17.7 13.9-23.2 4 0.29 14.4 0.28 20.4 0.28 0.27-0.30 14.4 7.9-21.1 Residue 0.22-0.04 12.7 0.19-0.02 17.9 0.23-0.02 0.25-0.01 12.6 7.9-19.4 3 0.41 36.1 0.40 28.8 0.40 0.38-0.42 31.4 23.6-44.5 *See Fig.3. position from trichomycin and hamycin. Two different batches of hamycin were available and differed markedly from one another. The sample of levorin resembled the candicidin much more closely, although the proportional composition was not included by the range of candicidin compositions noted ; whether this sample of levorin is typical of present-day material could not be determined.References 1 . 2. 3. 4. 5. WHO Tech. Rep. Ser., 1969, No. 413, 13. Kalasz, H., Gyimesi, J., Uskert, A., Magyar, K., and Horrath, I., Acta Chim. Acad. Sci. Hung., 1967, Ito, Y., Weinstein, M.A., Aoki, I., Harada, R., Kimura, E., and Nunogaki, K., Nature, Lond., 1966, Ito, Y., and Bowman, R. L., J . Chromat. Sci., 1973, 11, 284. Sutherland, I. A., and Sharpe, J. E. E., J . Chromat., 1976, 122, 333. 51, 431. 212, 985, Formation and Stability of lmidazole - Mercury Complexes with Some P-Lactam Antibiotics I. W. Macleod and B. J. Taylor Laboratory of the Governmed Chemist, Cornwall House, Stamford Street, London, SE1 9NQ The standard method of the British Pharmacopoeia for the assay of /3-lactam antibiotics is iodimetric titration.However, this method is subject to uncertain errors from iodine- absorbing impurities, so that for complex formulations it is normal to use microbiological assay. A chemical method for the determination of penicillins has been reported1 that in- volves the use of imidazole and mercury(I1) chloride to produce the stable mercury(I1) mercaptides of their penicillenic acids (Fig.1). The imidazole - mercury assay has been applied by the BP Penicillins Panel, and formally proposed to the European Pharmacopoeia Commission, after a successfully concluded com- parative study involving ampicillin, benzylpenicillin and phenoxymethylpenicillin.The general procedure is as follows. Prepare a solution to contain 50 pg ml-l of the penicillin or 200 pg ml-l of the cephalosporin in water, and pipette 2 ml of this solution into each of two test-tubes labelled “test” and “blank.” Dissolve 9.1 g of imidazole (recrystallised from toluene) in approximately 70 ml of water, adjust to the relevant pH shown in Table I using hydrochloric acid, and add water to 100 ml.Prepare the imidazole - mercury solution by adding dropwise, with continuous stirring, 1 ml of a 0.27% m/V solution of mercury(I1) chloride in water to each 10 ml of imidazole stock solution taken. Pipette 10 ml of this solution into the tube marked “test.” Prepare the imidazole working solution by adding 1 ml of water to each 10 ml of imidazole stock solution taken.Stopper both tubes, mix, place in a water-bath at the temperature and for the time stated in Table I, then cool to room temperature and measure the absorption of the “test” solution at the appropriate wavelength using the “blank” solution as reference. Pipette 10 ml of this solution into the tube marked “blank.”38 ORIGINAL PAPERS IN PHARMACEUTICAL ANALYSIS Proc.Analyt. Div. Chenz. SOC. TABLE I OPTIMUM CONDITIONS OF FORMATION, WITH THE ULTRAVIOLET ABSORBANCE DATA, FOR TWELVE P-LACTAM MERCURY (11) MERCAPTIDES H / \ CH CH HgC12 Antibiotic Temperature/"C Amox ycillin Ampicillin Benzathine penicillin Benzylpenicillin Penamicillin Phenoxymethylpenicillin Procaine penicillin Cephalexin Cephalonium Cephaloridine Cephalothia Cephoxazole 60 60 60 60 60 60 60 60 60 60 80 80 PH 6.8 6.8 6.8 6.8 6.8 6.8 6.8 6.8 8.0 8.0 6.8 6.8 Timelmin 15 20 25 25 20 20 25 25 45 60 30 30 Xmax./nm E X 105 at Am,,.311 19.4 31 1 19.6 325 26.6 325 26.6 325 24.4 325 25.5 325 26.6 322 12.9 345 6.2 345 5.1 345 6.0 363 10.4 In addition to the penicillins listed in Table I, it has been shown1 that carbenicillin, cloxa- cillin, dicloxacillin, methicillin, oxacillin , phenethicillin and propicillin yield assayable reaction products by heating at 60 "C for 20-30 min at pH 6.8.For substances such as benzathine and penamicillin, which are only sparingly soluble in water, the initial solution should be prepared in dimethylformamide and subsequent dilutions made with water.Ampicillin and amoxycillin react in a different manner from that of the other penicillins listed in Table I. Their reaction products exhibit maximum absorption at 311 nm, possess a lower molar absorptivity and are far less stable than the other penicillins investigated. However, by conducting the reaction at room temperature for 45 min, a more stable product with higher NH + lmidazole pH 6.8 R-C CH-CH C O //C-N-cH 0 coo0 / \ 2 \ / C H 3 R-C CH-CH c 11 I I I'CH3 c N-CH \coo0 6 jN H / \ II II CH CH d N \ R-C C=CH C \ I I 0-C N-CH l o \coo0 Fig.1. Normal mechanism for the formation of a mercury(I1) mercaptide from a penicillin. Fig. 2. Suggested reaction scheme (applied to ampicillin), which involves the formation of a 2,ti-piperazinedione.February , 1977 ORIGINAL PAPERS IN PHARMACEUTICAL ANALYSIS 39 absorptivity has been obtained.These results are inconsistent with the normal reaction mechanism (Fig. 1). Although no general pattern is apparent for cephalosporins, the reaction involving cephal- exin is exceptional in that the product absorbs at a wavelength significantly lower (322 nm) than those for other cephalosporins. The anomalous behaviour of ampicillin, amoxycillin and cephalexin, coupled with the structural similarity of an a-aminophenyl group in proximity to the p-lactam carbonyl group, suggests that in each instance a six-membered ring is formed in a simple process of closure (Fig.2). Support for this mechanism is obtained by acetylating the a-aminophenyl group prior to reaction. With ampicillin, the acetylated product gives a mercury(I1) mercaptide with higher absorbance at the normal maximum of 325 nm; by treating cephalexin in a similar manner, the amount of reaction product formed is drastically reduced (Fig.3). 270 30 0 350 Wave I e ng t t i /n rn Fig. 3. Comparison of ultraviolet spectra of: A, ampicillin; B, acetylated ampicillin; C, cephalexin; and D, acetylated cephalexin. Cephalosporins differ from penicillins by requiring stronger solutions exposed to more exacting test conditions (cf., Table I).This requirement often affects the stability of the reaction product. Consequently, the molar absorptivity values quoted are not absolute but are given for comparative purposes only. Each cephalosporin requires separate study in order to establish the optimum experimental conditions.Cephalosporin C so far has failed to give a reaction product. The claim of non-interference from degraded penicillin and from tested pharmaceutical adjuvants as made by Bundgaard and Ilverl has been upheld. Other drug substances occurring in penicillin formulations include chloramphenicol, ephedrine hydrochloride, lignocaine hydrochloride, streptomycin sulphate, sulphadiazine, suphadimidine, sulphamera- zine, sulphanilamide and sulphathiazole.2 No interference was observed when a ten-fold excess of each of these compounds over benzylpenicillin was used in turn. Benzathine and procaine were found not to interfere. The imidazole - mercury method, whether applied directly to Procaine Penicillin BP, or after preliminary precipitation of procaine in the manner described in the official method of assay,3 gave identical results. A standard deviation of 0.42% was obtained for ten determinations by the direct method. The imidazole - mercury method can therefore be used directly in situations where other current methods would require the preliminary removal of co-formulants. It is also applicable to the analysis of samples in which degradation is suspected. However, the use of mercury(I1) chloride introduces limitations : anions such as sulphide are incompatible, although this particular interference can be overcome by centrifugation and addition of further reagent. We thank the members of the BP Penicillins Panel for their advice and drug specimens. This paper is published with the permission of the Government Chemist.40 OBITUARIES Proc. Analyt. Div. Chem. SOC. References 1. Bundgaard, H., and Ilver, K., J . Pharm. Pharmac., 1972, 24, 790. 2. Blacow, N. W., Editor, “Martindale : The Extra Pharmacopoeia,’’ Twenty-sixth Edition, Pharma- 3. “British Pharmacopoeia 1973,” HM Stationery Office, London, 1973, p. 386. ceutical Press, London, 1972.

ISSN:0306-1396    

DOI:10.1039/AD9771400030

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年代:1977

数据来源: RSC

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40 OBITUARIES Proc. Analyt. Div. Chem. SOC. 0 bi tuaries Heinrich Kaiser Professor Dr. Heinrich .Kaiser, the eminent German spectrochemist, died in Dortmund on August 23rd, 1976. Born in Bochum in the Ruhr in 1907, he studied physics, mathematics and chemistry in the Universities of Munster, Freiburg and Cologne, from which in 1932 he received a PhD degree for work under Professor Rukop on oscillation frequencies in undamped electrical circuits.This provided the back- ground for later studies on spark-generator excitation in emission spectroscopy. On graduation he became assistant to Professor Karl Forsterling and was introduced to spectro- scopy. From 1934 until 1946 he was with the Carl Zeiss company, directing their spectrographic laboratories in Jena and Dresden during the war.He soon came to specialise in optical emission spectrochemical analysis, working on the analysis of alloys, the accuracy of spectral analysis, the application of spark emission methods and techniques of photographic photo- metry, devising a generalisation of the Seidel transformation to simplify the evaluation of spectral line densities. In 1945 the Zeiss works fell into US Army hands and Dr.Kaiser, after interviews with W. R. Brode and R. A. Sawyer, was transferred by truck from the prospective Russian zone to south-west Germany, with his family and his library, which took preference over scarce household articles. After two difficult years, he was appointed to the staff of the newly founded State Institute for Testing Materials in Dortmund, obtaining spectrographic laboratory facilities and becoming Privat Dozent in the Department of Physics in Bonn University, where Walther Gerlach was Professor.He advocated the establishment of an independent institute for the promotion of spectrochemistry in West Germany and was soon rewarded by the foundation of a society charged with the establishment of the Institute for Spectro- chemistry and Applied Spectroscopy in Dort- mund.This was inaugurated in 1952 with a staff of 20 under his direction. Ten years later commodious new premises were opened to accommodate a staff that had risen five-fold. Lines of work included atomic spectroscopy, atomic absorption, inorganic analysis, molecular spectroscopy, electronics and general physics, X-ray fluorescence and mass spectrometry.While the Institute was sponsored by Govern- ment and industry, Professor Kaiser was free to plan the research programme, in addition to which investigations and analyses for outside organisations were carried out on a contract basis. His own particular interests included limits of detection and accuracy of determina- tion in emission analysis. He retired from the Directorship shortly before his death, but remained active in other fields.Professor Kaiser was a familiar figure at scientific meetings in many countries. He first visited the USA in 1939, attending an MIT Summer Conference; after the war he seldom, if ever, missed an International Spectroscopy Colloquium and had planned to give a paper on analytical accuracy at the XIX CSI in Phila- delphia in November, 1976. He was a member of the Continuation Committee that ensured the perpetuation of the Colloquia along the lines established in Strasbourg in 1950.Those privileged to participate in one of the informal evenings that were a feature of these Colloquia will remember how, over a bottle of wine or a mug of beer, Dr. Kaiser would reminisce with Dr.Menzies, Professor Mandelstam, Father Salpeter and others, drawing from his stock of personal experiences. He had a profound sense of humour which often served in conjunc- tion with his wide knowledge of all branches of spectroscopy, to lead to a rational understanding over points that had given rise to heated discus- sion. His presidency of the Heidelberg Collo- quium in 197 1 revealed his appreciation of good music and his expertise in food and wine, as all those who attended the ancillary functions and excursions will agree.He liked to recall his misadventure on a visit to Harwell soon after the war, when his English was less proficient than it later became. He was to be met by an official car, but unfortu- nately a t Didcot there were two black cars withFebruary, 1977 OBITUARIES 41 uniformed drivers and he was driven off by the one awaiting an expert witness for local court proceedings. He spent several hours in a witness room (thinking it was not quite the welcome he had expected at Harwell, but saying nothing) before the local police, who had been alerted about his disappearance, found him on their own premises ! For many years he was a most active member of the International Union of Pure and Applied Chemistry.He twice represented the Federal German Republic on the Analytical Division Council of IUPAC and was in the final year of his present term of office at the time of his death. In Europe he was well known as a pan-European but a t IUPAC he became a superb inter- nationalist and took many a newcomer under his wing.Naturally he was the Chairman of the Commission on Spectrochemical and other Optical Procedures for Analysis for the maxi- mum period of office and under his guidance it made very notable contributions, particularly in unravelling the tangled skein of spectrochemical nomenclature. The stamp of his authority will remain in that area probably as long as spectro- chemical nomenclature is used.As always, even in IUPAC his work was overlaid by his sense of humour such as the time at Cortina d’Ampezzo when he slipped anchor and solemnly led the entire Commission up a mountain to hold their meeting there while “lesser” Commissions toiled in the summer heat of the valley a t their feet. Professor Kaiser, who is survived by his wife Ada, two sons, two daughters and four grand- children, was an Honorary Member of the Society for Analytical Chemistry and had received the Hasler Award of the Society for Applied Spectroscopy.Apart from publishing many scientific papers and serving as one of the Editors of Spectrochimica Acta from 1947 until 1958, he took an active interest in university education. At future spectrochemical gather- ings his scholarly presence will be sadly missed.R. L. Mitchell T. S. West George Frederick Smith Professor George Frederick Smith died in Urbana, Illinois, on September 23rd, 1976, in his 86th year; he must be ranked as one of the most distinguished analytical chemists of the present century. Professor Smith had a very varied career before he settled down to study chemistry seriously.He was a pianist in the silent cinema, he worked in the Kansas wheat fields and for the American Railway Express Co., was an infantryman in the First World War and taught music. He entered the University of Michigan at Ann Arbor and obtained his BS degree but his studies were interrupted by World War I. After the War he returned to Ann Arbor and completed his doctoral studies under the direction of the late Professor H.H. Willard. In 1921 he obtained an appointment at the University of Illinois, where he worked until his retirement in 1958. He still continued to work in the Department, probably until shortly before his death, and he retained a great interest in the activities of the Mid-West Universities Analytical Chemistry Association, which he helped to found.Smith’s researches in analytical chemistry covered a wide field; however, he is probably known best for his work on perchloric acid and on his studies of 1,lO-phenanthrolines and related compounds. In 1954, many older chemists will recall his memorable lecture with demonstrations to a packed hall in the Royal Institution. His skill would undoubtedly have been applauded by Michael Faraday himself. He played a great part in removing many of the general fears associated with perchloric acid reagent.In the course of his investigations of the 1, 10-phenanthrolines, more than 200 com- pounds were synthesised and their properties examined. As a result of this work, indicators and spectrophotometric reagents which are now widely used throughout the world were dis- covered.Probably his reagents for iron and for copper are those most widely used. His other studies included work on reductors, periodic acid, cerium (IV), primary standards, the determination of the alkali metals and various laboratory gadgets. In order to provide readily available reagents, Professor Smith founded the G. F. Smith Chemical Co.in 1928. The Company specialised in the manufacture of pure chemical reagents and this service enabled new methods to be put into practice without the usual delays caused by lack of availability of the necessary reagents. His Company also published a number of mono- graphs on various reagents, which were provided free of charge. Many people wrongly supposed that Professor Smith, who was very wealthy, acquired his riches from this Company, but it is doubtful if it was ever run on a profit-making basis, a t least in the early days.His personal fortune was acquired through his invention of a whipped-cream dispenser in 1934-the fore- runner of all subsequent aerosol dispensers. Professor Smith received many awards and honours, among which may be mentioned the42 CONFERENCES AND MEETINGS R o c .AnaZyt. Div. Chem. SOC. Fischer Award (1954) and the Anachem Award (1959). In 1966, the international journal of analytical chemistry Talantlz issued a G. F. Smith Honour Issue. Smith was one of the most likeable characters in analytical chemistry. He was generous in spirit, warmhearted and was always full of life. 4 t the SAC Conference held at St. Andrews in 1956, many of us remember him breaking scientific records for the longest after-dinner speech, which had previously been held by a well known carbohydrate chemist and who tried later, in vain, to recapture the record. The story be- came exaggerated with the passage of time, but the speech was said to last for 90 minutes. If one wrote to Smith on any subject he would in- variably reply with a 12-page letter written in his very legible script and in which he would dilate on many varied topics. Those of us who knew him intimately mourn his passing, knowing full well that the world is a poorer place without him. R. Belcher

ISSN:0306-1396    

DOI:10.1039/AD9771400040

出版商:RSC    

年代:1977

数据来源: RSC

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42 CONFERENCES AND MEETINGS ROC. AnaZyt. Div. Chem. SOC. Borough Road, London, S.E.l. The following will be presented : “An Integrated Foundation Course in Chromatographic Methods of Separation,” by D. F. G. Pusey. “Is GLC an Essential Component of the Science Curriculum ?” by S. Thorburn. “Practical Aspects of HPLC,” by S. J. Moulton. For further details contact the Honorary Secretary of the Group, Dr.N. T. Crosby, Labora- tory of the Government Chemist, Cornwall House, Stamford Street, London, SE1 9NQ. Conferences Orion Workshops on Electrodes February-March, 1977 and Courses Ion- selective MSE Scientific Instruments, the UK agents of Orion Research, are holding a further series of 1-day workshops, in which there will be demon- strations of the use of ion-selective electrodes in various applications.Direct methods, addition methods and potentiometric titrations will be carried out and there will be opportunity to discuss analytical problems. The workshops will be held as follows: Feb. 24, Aberdeen March 4, Birmingham Feb. 25, Glasgow March 7, Leicester Feb. 28, Teesside March 8, London March 1, Leeds March 9, London March 2, Liverpool March 10, London March 3, Manchester March 11, Bristol For details, contact Mrs D.Barton, MSE Scientific Instruments, Crawley, Sussex, RHlO 2QQ- Education and Training Group : Discussion Meeting March 1, 1977, London X discussion meeting on “Teaching of Chroma- tographic Techniques,” starting at 2 p.m., will be held at the Polytechnic of the South Bank, Courses on the Monitoring and Particle Counting of Asbestos March 7-9, 1977, London Two courses have been arranged on this subject by the McCrone Research Institute and they will be held on Monday and Tuesday, March 7-8 and Tuesday and Wednesday, March 8-9.Those interested should apply as soon as possible to The Registrar, McCrone Research Institute, 2 McCrone Mews, Belsize Lane, London, NW3 5BG. Joint Pharmaceutical Analysis Group : Discussion Meeting March 10, 1977, London A discussion meeting on “Preservation of Medicinal Products and Related Matters,’’ starting at 2 p.m., will be held in the Hall of the Pharmaceutical Society of Great Britain, 1, Lambeth High Street.Discussion will be led by an invited panel. For further details contact the Honorary Secretary of the Group, Miss I.Ladden, British Pharmacopoeia Commission, 8, Bulstrode Street, London W1M 5FT. CS Annual Chemical Congress March 28-April 1, 1977, London The Annual Chemical Congress of the Royal Institute of Chemistry and The Chemical Society will be based at University College London and will include the Centenary Celebrations of the RIC. Two analytical symposia will be held on Wednesday, March 30th and Thursday, March 31st.Symposium A will be on “The History of Analytical Chemistry” and will include lectures by R. Belcher, R. H. Nuttall, Miss J. Peden, W. I. Stephen, F. SzabadvAry, D. Thorburn Burns and T. S. West. Symposium B is entitled “Modern Methods of Speciation : Charac- terisation of Chemical Species’’ and will includeFebruary, 1977 CHEMICAL SOCIETY LIBRARY lectures by C.A. Edwards, B. Fleet, D. M. Hercules, I. K. O’Neill, A. Townshend and J. C. Van Loon. On Thursday morning, Dr. D. R. Deans will deliver the sixth Theophilus Redwood Lecture, “Analysis with a Purpose.” For titles of papers, see the Diary (p. 47). Further information, including application forms, can be obtained from Dr. John F. Gibson, The Chemical Society, Burlington House, London, W1V OBN.Gel Filtration and Electrophoresis March 28-April 1, 1977, Loughborough A course on this subject is to be held in the Department of Chemistry of the Loughborough University of Technology, and will cover the following topics : gel filtration in columns and on thin layers, including determinations of relative molecular mass and other applications ; related chromatographic techniques, including affinity chromatography, gel filtration - ion exchange, etc.; cellulose acetate electrophoresis and paper electrophoresis a t high and low voltages; gel electrophoresis on acrylamide, starch and agar gels ; isoelectric focusing and isotachophoresis ; immunological methods, including Laurel1 elec- trophoresis, electroimmunodiffusion and counter immunoelectrophoresis.Further details can be obtained from Mrs. P. A. Bartram, Chemistry Department, Loughborough University of Technology, Loughborough, Leicestershire, LEI 1 3TU. Spectrofluorimetry and Related Topics April 18-19, 1977, Loughborough This course is to be held in the Department of Chemistry of the Loughborough University of Technology and will cover the following topics : introduction to luminescence spectroscopy, instrumentation and practical techniques in luminescence spectroscopy ; fluorescence deriva- tisation and the analysis of derivatives by combinations of fluorimetry with thin-layer chromatography and high-performance liquid chromatography ; analysis of pharmaceuticals ; applications in biochemistry (both small mole- cules and macromolecules). Further details can be obtained from Mrs. P. A. Bartram, Chemistry Department, Loughborough University of Technology, Loughborough, Leicestershire, LE11 3TU. 43

ISSN:0306-1396    

DOI:10.1039/AD9771400042

出版商:RSC    

年代:1977

数据来源: RSC

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February, 1977 CHEMICAL SOCIETY LIBRARY 43 The Determination of Sulphur - containing Groups. Volume 2. M. R. F. Ashworth. Academic Press. 1976. Principles and Practice of X-ray Spectro- metric Analysis. Second Edition. E. P. Bertin. Plenum. 1975. Metal Carbonyl Spectra. P. S. Braterman. Academic Press, 1975. Biochemical Fluorescence : Concepts. Vol- ume 2. Edited by R. F. Chen and H. Edelhoch. Dekker.1976. Chemical Analysis of Organometallic Com- pounds. Volume 4. Elements of Group V. T. R. Crompton. Academic Press. 1975. Liquid Column Chromatography. A Sur- vey of Modern Techniques and Applications. Edited by 2. Deyl, K. Macek and J. JanAk. Elsevier. 1975. Molecular Spectroscopy of Dense Phases. Proceedings of the 12th European Congress on Molecular Spectroscopy held at Stras- bourg, 1975.Edited by M. Grossmann. Elsevier. 1976. A Guide to Laboratory Design. K. Everett and D. Hughes. Buttenvorths. 1975. Analytical Aspects of Mercury and Other Heavy Metals in the Environment. Edited by R. W. Frei and 0. Hutzinger. Gordon and Breach. 1975. Chemical Infrared Fourier Transform Spectroscopy. P. R. Griffiths. Wiley-Interscience. 1975. Thermal Analysis.Volumes 1, 2 and 3. Proceedings of the 4th International Confer- ence on Thermal Analysis held at Budapest, 1974. Edited by I. BuzAs. Heyden. 1975. Introduction to Computer Programming for Chemists. T. L. Isenhour and P. C. Jurs. Allyn and Bacon, Inc. 1972. Topics in Carbon- 13 NMR Spectroscopy. Volume 2. Edited by G. C. Levy. Wiley-Interscience. 1976. Aldehydes-Photometric Analysis.Vol- umes 1, 2 and 3. E. Sawicki and C. R. Sawicki. hemica' Society Library The following publications of analytical interest have been added to the Library since the last Academic Press. list appeared in Proceedings (1976, 13, 315). 1975-1976.44 PUBLICATIONS RECEIVED Proc. Analyt. Div. Clzem. SOC. Practical High Performance Liquid Chro- matography. Edited by C. F. Simpson. Heyden, in associa- tion with the Continuing Education Committee of the Chemical Society. 1976. High Pressure Liquid Chromatography in Clinical Chemistry. Proceedings of a Sym- posium held at Kings College Hospital Medical School, 1975. Edited by P. F. Dixon, G. H. Gray, C. K. Lim and M. S. Stoll. Academic Press. 1976. Modern Fluorescence Spectroscopy. Volume 1. Edited by E. L. Wehry. Plenum. 1976. Analytical Atomic Spectroscopy. W. G. Schrenk. Plenum. 1975. Trace Element Analysis. V. Valkovic. Taylor and Francis. 1975.

ISSN:0306-1396    

DOI:10.1039/AD9771400043

出版商:RSC    

年代:1977

数据来源: RSC