摘要:

Proceedings of the Society for Analytical Chemistry CONTENTS Reports of Meetings . . .. 41 Annual General Meeting . . 41 Annual Report of the Council . . 45 Summaries of Papers “Scanning Techniques” . . . . 58 “Amplification Reactions” . . 61 “Special Techniques in Analytical Chemistry” . . . . . . 63 “Thermal Analysis” . . . . 64 “Evolved Gas Analysis and Detec- tion” . . . . . . . . 65 Membership Changes . . . . 67 Papers Accepted for The Analyst 67 Publications Received . . . . 68 Forthcoming Meetings Back cover ?roc. SOC. Analyt. Chem. VoI. 7 No. 3 Pages 41-68 March 1970 Voi. 7 No. 3 PROCEEDINGS OF March 1970 THE SOCIETY FOR ANALYTICAL CHEMISTRY President of the Society T. S. West Hon. Secretary of the Society W. H. C. Shaw Hon. Treosurer of the Society G. W. C. Milner Hon.Assistant Secretaries of the Society D. 1. Coomber; D. W. Wilson Secretary Miss P. E. Hutchinson 9/10 SAVILE ROW LONDON W I X IAF Telephone 01-734 6205 Editor J. B. Attrill Assistant Editor Miss C. M. Richards Telephone 01-734 3419 Proceedings is published by The Society for Analytical Chemistry and distributed to all members of the Society and t o subscribers with The Analyst; subscriptions cannot be accepted for Proceedings alone. Single copies may be obtained direct from the Society’s Distribution Agents The Chemical Society Publications Sales Office Blackhorse Road Letchworth Herts. (NOT through Trade Agenu) price 0 The Society for Analytical Chemistry 5s. post free. Remittances MUST accompany orders. THE SOCIETY FOR ANALYTICAL CHEMISTRY The Eighth Annual Meeting on RESEARCH TOPICS IN ANALYTICAL CHEMISTRY will be held at The University of Birmingham on the afternoon of Friday May 8th 1970 The meeting will consist of twelve papers delivered by post-graduate students on a variety of topics in analytical chemistry.

ISSN:0037-9697    

DOI:10.1039/SA97007FX009

出版商:RSC    

年代:1970

数据来源: RSC

摘要:

THE SOCIETY FOR ANALYTICAL CHEMISTRY Forthcoming Meetings-continued IYednesday 15th NOTTIXGHAM Thursday 16th MIDLANDS SECTION jointly with the Toxicology Society. “Recent Advances in Toxicological Analysis,” by A. S. Curry. Nottingham ; BIOLOGICAL METHODS GROUP Full-day Meeting on “Pharmacological Screen- London. NORTH OF ENGLAND SmxroN jointly with the Sorth Lancashire Section of the “The Analysis of Plastics-Why and How?” by a%. G. Jones. Harris Technical College Preston ; 7.30 p.m. WESTERN SECTION Discussion Meeting. Discussion on “Analytical Problems of the Public Analyst,” to be introduced The George Hotel Chepstow; 6.30 p.m. SORTH EAST SECTION jointly with the Teesside Section of the Royal Institute “The Automation of Gas Chromatography,” by D. R. Deans. Constantine College of Technology Middlesbrough ; 8 p.m.MIDLANDS SECTION jointly with the Mid-Anglia Section of the Royal Institute “Automatic Analysis-An Industrial View-point,” by P. G. Jeffery. Luton College of Technology Luton; 6.45 p.m. CHROMATOGRAPHY AND ELECTROPHORESIS GROUP Meeting on “Comparison of Speakers to include P. Smith and Professor E. J . Shellard. Portsmouth Polytechnic Portsmouth ; 2.30 p.m. 6.30 p.m. ing for New Drugs 111.” T,orzno~ Friday 17th PRESTON Royal Institute of Chemistry. Friday 17th CH EPSTOW by L. E. Coles and W. Cassidy. Tuesday 21st ~II~)I>LESBROUGH of Chemistry. lycdnesday 22nd LUTON of Chemistry. Thursday 23rd PORTSMOUTH Chroma tographic Techniques. ’ ’ THE SOCIETY FOR ANALYTICAL CHEMISTRY Forthcoming Meetings March Wednesday 25th MANCHESTER KORTH OF ENGLAND SECTION joiiztZ2l with the Local Sections of the Chemical Society the Royal Institute of Chemistry the Society of Chemical Industry and the Society of Dyers and Colourists on “Recent Advances in Analytical Chemistry.” “The Use of GLC and TLC in the Structural A4nalysis of Organic Compounds,” by L. S. Bark. “Thermal Analysis,” by J. P. Redfern. “Atomic Absorption and Allied Spectroscopic Techniques,” by J. B. Dawson. “Mass Spectrometry and Electron Spectroscopy,” by M. Barber. Renold Building University of Manchester Institute of Science and Technology Sacltville Street Manchester 1 ; 10.00 a.m. April Friday 3rd and Saturday 4th SOCIETY jointZy with the Analytical Section of the Royal Dutch Chemical Society Symposium on “Accurate Methods of Analysis for Major Consti- LONDON tuents.” Imperial College of Science and Technology London S.\fr.7. ANGLO-DUTCH SYMPOSIUM AT the time of going to press there are still some vacancies for registration for this Symposium. Anyone who has not yet registered and who wishes to attend should telephone the S.A.C. office (01- 734 6205) asking for a registration form to be sent. This should be completed and sent back by return of post. Monday 9th to Friday 10th SLOUGH THERMAL ANALYSIS GROUP Second Thernial Analyis School. “Introductory Lecture,” by D. Dollimore. “Theoretical Basis for Thermal Analysis,” by R. A. IY. Hill. “Present Status and Future Development of the Techniques,” by J . P. Iiedfern. “Instruments,” introduced by R. C. hlackenzie. “Applications to Inorganic Materials,” by J. H. Sharp. “Applications to Metallurgical Problems ” by J . Mackowiali. “Applications to Organic Compounds Including Polymers,” by 13. C. Roberts. “Low-temperature Thermal Analysis,” by I. C. ITylie. “Quantitative Thermal Analysis,” by 5;. IY. Wilburn. Cement and Concrete Association Fulmer Grange Slough. AUTOMATIC METHODS GROUP Demonstration Meeting on “Semi-automatic or Automatic Instruments Other Apparatus Designed by Members and Kovel Assemblies of Component Instruments.” “The Role of the Instrument Manufacturer in the Development and Exploita- tion of Inventions,” by G. C. Collins. Rliddlesex Hospital Medical School Clel-eland Street London W. 1 ; 10.30 a.m. Thursday 9th LONDOX [continued on inside back cozrey Printed by W Heffer d( S o n s Ltd Cambridge England

ISSN:0037-9697    

DOI:10.1039/SA97007BX011

出版商:RSC    

年代:1970

数据来源: RSC

摘要:

March 1970 Vol. 7 No. 3 PROCEEDINGS OF THE SOCIETY FOR ANALYTICAL CHEMISTRY Annual General Meeting THE ninety-sixth Annual General Meeting of the Society was held at 5 p.m. on Friday March 6th 1970 in the Midland Hotel Peter Street Manchester 2. The Chair was occupied by the President Professor T. S. West B.Sc. Ph.D. D.Sc. F.R.I.C. The Financial Statement for the year ending October 31st 1969 was presented by the Honorary Treasurer and approved and the Auditors for 1970 were appointed. The Report of the Council for the year ending March 1970 (see pp. 45 to 57) was presented by the Honorary Secretary and adopted. The Scrutineers Mr. J. €3. Aldred and Mrs. H. I. Fisk reported that the following had been elected officers for the coming year- President-Professor T. s. West B.Sc. Ph.D. D.Sc.F.R.I.C. Past Presidents serving on the Council-A. J. Amos D. C. Garratt A. G. Jones and Vice-Presidents-H. J. Cluley C. A. Johnson and D. W. Wilson. Honorary Treasurer-G. W. C. Milner. Honorary Secretary-W. H. C. Shaw. Honorary Assistant Secretary-D. I. Coomber (Programmes). Other Members of Council-The Scrutineers further reported that 423 valid ballot papers had been received and that votes had been cast in the election of Ordinary Members of Council as follows-R. Belcher 352; D. Betteridge 249; E. Bishop 289; W. T. Elwell 340; D. Moore 230; J. M. Ottaway 233; G. E. Penketh 238; C. L. Wilson 305. The President declared the following to have been elected Ordinary Members of Council for the ensuing two years-R. Belcher D. Betteridge E. Bishop W. T. Elwell G. E. Penketh and C. L. Wilson.H. E. Brookes Mrs. D. Butterworth J . B. Headridge G. F. Kirkbright J. D. R. Thomas and C. Whalley having been elected members of the Council in 1969 will by the Society’s Articles of Association remain members of the Council for 1970. W. M. Lewis (Chairman of the Midlands Section) T. G. Morris (Chairman of the \Vestern Section) A. C. Docherty (Chairman of the North East Section) R. Sinar (Chairman of the North of England Section) C. E. Waterhouse (Chairman of the East Anglia Section) D. Ril. W. Anderson (Chairman of the Scottish Section) and W. J. Williams (Chairman of the Education and Training Committee) will be ex-oficio members of the Council for 1070. The Annual General Meeting was followed by a lecture given by F. L. Rose on “An Organic Chemist at Large. ” The presentation of the Society’s Gold Medal to Dr. R. C. Chirnside by the President was made a t the Informal Dinner held in the evening. A. ,4. Smales. 41

ISSN:0037-9697    

DOI:10.1039/SA970070041a

出版商:RSC    

年代:1970

数据来源: RSC

摘要:

Ma.rch 19701 ANNUAL REPORT OF THE COUNCIL 45 Annual Report of the Council March 1970 FOR the Society the 1960s were eventful years. Over a period that saw the continued growth and diversification of the analytical sciences and the consolidation of techniques introduced in earlier years the Society has undergone changes that have fully reflected these developments. The middle years of the decade saw the formation of two new Sections and a rapid expansion of the Group structure of the Society; this growth was continued into 1969 with the incorpora- tion of the Polarographic Society as the Electroanalytical Group which held its inaugural meeting in November and the formation of a Joint Pharmaceutical Analysis Group sponsored in association with the Royal Institute of Chemistry and the Pharmaceutical Society of Grcnt Britain.The Society with its Sections and Groups again organised a comprehensive programme of meetings covering the wide range of topics that the field of analytical chemistry now embraces. It is encouraging to see that many of these meetings are organised jointly by Groups and Sections sometimes in association with other scientific bodies. In the 1960s also came the recognition that the Society should hold regular major con- ferences to provide opportunities for the presentation of papers and general interchange of ideas within the many areas of interest to analysts. In addition to these conferences now held at 3-year intervals and increasingly international in character there is need for other or more specialised conferences organised by Sections and Groups of the Society.In July the Atomic-Absorption Spectroscopy Group in association with the Spectroscopy Group of the Institute of Physics and the Physical Society organised an International Atomic Absorption Spectroscopy Conference which was the first of its kind to be held in the United Kingdom and it is believed the largest in the world so far on this subject. Held at the University of Slieffield the Conference was attended by 405 delegates about half of whom were from 30 overseas countries and it included a scientific programme in which some 40 per cent. of the contributed and plenary papers were presented by overseas speakers. At the opening ceremony the President of the Society presented Dr. A. Walsh F.R.S. with the Certificate of Honorary Membership of the Society in recognition of his pioneering work in atomic-absorp- tion spectroscopy.The Conference programme included a manufacturers’ exhibition and full social activities. The Chairman of the Conference Dr. J. B. Dawson and the Organising and Local Committees are to be congratulated on arranging a most successful and truly inter- national occasion. In the week following this Conference the University of Birmingham was the venue of the International Symposium on Analytical Chemistry organised by the Midlands Section of the Society and held under the patronage of the International Union of Pure and Applied Chemistry. The Symposium President was Professor M. Stacey and the joint Honorary Presidents were Professor T. S. West and Professor W. Kemula President of the Analytical Division of I.U.P.A.C. The scientific programme included six plenary lectures by speakers of international repute and some 110 contributed papers covering many aspects of analytical chemistry.A full social programme was arranged. The Symposium was made the occasion for many presentations both formal and informal to Professor R. Belcher in honour of his 60th birthday and in recognition of his long and varied services to international analytical chemistry. The Lomonosov Medal was presented to Professor Belcher on behalf of the University of MOSCOW in recognition of his contribution to promoting goodwill amongst All the meetings are fully detailed in the accompanying list. 46 ANNUA41a REPORT OF THE COUNCIL [P?‘oc. SOC. Analyt. CheWZ. chemists throughout the world and the Mendeleeff Medal awarded by the Praesidium of the Mendeleeff All-Union Chemical Society was presented as a token of the respect of that Society for Professor Belcher’s scientific achievements.Other presentations were made on behalf of the Austrian and American Microchemical Societies and by the French delegation. The Technische Hochschule of Vienna presented him with its “Golden Pin.” During the Symposium the TaIanta Gold Medal was presented to Dr. A. Walsh and the Hevesey Medal to Dr. A. A. Smales. The Midlands Section is to be congratulated on the success of this its fourth International Symposium. The return meeting with the Analytical Chemistry Section of the Royal Dutch Chemical Society will take place in April the Second Particle Size Analysis Conference will be held at the University of Bradford in September and in the summer of 1971 the Society will hold its third Conference on this occasion a t the University of Durham.This is the first year that The Chemical Society has undertaken the distribution of current journals and the sale of back issues and as a result we have benefited financially. These financial savings together with increases in subscriptions to the journals have made the main contributions to the surplus reported for the year. The major part of this surplus has been allocated to the reserve fund far the future purchase of permanent office accommodation. A new reserve fund has been set up to finance future computer applications which the Society will require in preparing indexes for Analytical Abstracts. The reserve funds for cumulative indexes and conferences have been increased.In May the Society changed its brokers so that a complete re-organisation of the schedule of investments could be carried out. Many of the smaller holdings of shares have now been sold and the total number of investments has been reduced to about fifty. The administra- tion and management of the Society’s investments has been entrusted to a nominee company of W. I. Carr Sons & Co. In March the Society instituted a staff pension scheme for the benefit of the permanent staff. Early in 1969 the Society was invited to take part in discussions that may well have a profound effect on the future of the Society. The close association between The Chemical Society and the Royal Institute of Chemistry led to the idea of a single chemical society that would speak with one voice for all branches of chemistry in the U.K.and the Society was asked to consider its attitude towards joining an amalgamation of The Chemical Society the Faraday Society the Royal Institute of Chemistry the Society of Chemical Industry and the Society for Analytical Chemistry. This invitation was considered by the Council in June when a Sub-committee of Council was formed to discuss the initial proposals and to advise Council on the implications. The Sub-committee met frequently thereafter and sent delegates to a11 subsequent meetings of representatives of the five societies. Members of the Society were informed in the November issue of Proceediizgs of the progress of the discussions. An exemplary plan of the proposed structure of an amalgamation of The Chemical Society and the Royal Institute of Chemistry was published in Chemistry in Britain but it became clear to the Sub-committee that this structure was not well suited to an amalgamation of five Societies.In addition it was felt that the Society should place itself in a position to influence the decisions that were being taken so as to be in a good position to decide to join or stay outside any amalgamation that is eventually formed. Accordingly the Society submitted a revised plan for a five-body structure for discussion at a meeting of representatives of the Societies in December and it is most encouraging that this plan was accepted with minor modification as the basis for further progress. Under the proposed Divisional structure this Society would become the Division of Analytical Chemistry retaining much of its present organisation and continuing its established activities including those of publishing its journals.While Council is fully aware that in an amalgamation we might lose some of our present independence the prospect of becoming the official analytical division of the (integrated) chemical society of the U.K. is an attractive one that augurs well for the status future prosperity and vitality of analytical chemistry. In 1969 the Society continued to participate in the activities of the Consortium on Chemical Information. The Chemical Society acting for the Consortium entered into an Arrangements for future conferences are progressing well. March 19701 ANNUAL REPORT OF THE COUKCEL 47 agreement whereby The Chemical Society became the sole agents for the sale and distribution in the United Kingdom of the publications of the Chemical Abstracts Service and undertook to develop a computer-based Chemical Information Service (U.K.C.I.S.).PUBLIC ATIONS-The Analyst Editorial Board and Executive Committee completed its first full year of operation in 1969 a year in which the size of the journal increased by some 40 per cent. The number of new manuscripts offered for publication during the year was 243 compared with 270 during 1968 the latter figure included 30 papers presented at the SAC Conference 1968 and the current figures include approximatelv 10 from the Birmingham and Sheffield Con- ferences. The rate of receipt and acceptance of papers over the past two years appears to have stabilised at about 20 per cent. above the level of earlier years although at present the rate of publication in terms of pages of print is about 40 per cent.higher. The average length of papers has increased slightly from 5.0 to 5.6 pages. The audited circulation of The Aiznlyst for 1969 is only slightly less than in 1968 (7138 against 7334 copies of each issue). Proceediqs has continued its policy of recording the activities of the Society and of its growing number of Sections and Groups. The summaries of lectures given at meetings remain one of its most valuable features. Over the past years the requirement of readers for speedier and more frequent production of indexes to AwaZytical Abstracts has been a continuing problem but the situation has been recently improved by the publication starting in 1969 of two volumes of AizaZytical Abstracts per year each with its own comprehensive Subject and Author Index.The Society is however aware of the growing value of computerisation in the information field and investigations which have included a pilot experiment into the use of computer techniques to generate the Abstracts Indexes are now in hand. This could result in the more rapid production of the 6-monthly indexes and the publication of monthly indexes but the most valuable outcome would be the very considerable saving in time in the production of the cumulative indexes. The number of abstracts published during 1969 in Analytical Abstracts is disappointing 7420 items (on 1052 pages) compared with 7778 (on 1056 pages) in 1968. This decrease is due to shortage of staff the difficulties in recruiting suitable new assistants and the relatively long periods required in training them.The necessary steps have been taken to increase the throughput of abstracts in the coming year. The second cumulative Index (covering the years 1964-1968) is now being compiled and the target date for publication is a t the beginning of 1971. A change in the production of Analytical Abstracts is the resignation of Dr. Norman Evers from his work on the subject section of the Index. Throughout the time he was Editor of Abstracts (from its inception in 1954 until 1962) and during the succeeding years Dr. Evers supervised and was fully responsible for this part of the Index; latterly the whole of the compilation has been in his hands. Miss Sinclair who since 1966 has helped with the pre- paration of some of the subject section has also resigned.Future subject indexes will be compiled by Dr. Jean Macqueen. Mr. C. H. R Gentry who has been a member of the Committee since 1957 and has been responsible for part of the “Inorganic” section of the journal resigned at the end of 1969 and has been replaced by Dr. T. R. Andrew; and Dr. D. C. Abbott has been appointed as an additional member to be responsible for the “Agriculture” and “Air water effluents” sections. The audited figure for the monthly circulation in 1969 was 6630 compared with 6775 in 1968. Although the flow of suitable manuscripts has been less in 1969 the Book Depzrtment has had a second successful year of operation. Plans are in hand for the publication early in 1971 of the first of a series of Annual Reviews each containing some four to six critical reviews of selected areas of analytical chemistry.In addition several authors have been approached for manuscripts suitable for publication in book form; each book will cover a specific topic The 1969 volume contains 197 papers (157 in 1068) in 1168 pages (836). The Editorial Committee has had two changes in its constitution. 4s ANNUAL REPORT OF THE COUNCIL [Proc. SOC. Analyt. Chenz. or technique and will be written by a specialist in the particular field. I t is hoped that the first book will be ready for publication in 1971. ANALYTICAL METHODS COMMITTEE-The Committee has enjoyed a year in which signifi- cant progress in much of its work has been achieved. Five reports from the A.M.C. Sub- committees and Panels of the Joint Committee with the Pharmaceutical Society were pub- lished in The Anal-yst and several further reports are being prepared for publication during the next year.The Analytical Standards Sub-committee which has now nearly completed its work on standards for use in acid - base titrimetry has formed a Joint Panel with the Microchemical Methods Group of the Society to revise the specifications for “Reference Substances for Use in Organic Micro-analysis” and “Reagents for Use in Micro-analysis,” which were last issued in 1962. This Joint Panel under the Chairmanship of Dr. G. Ingram has made rapid progress and it is possible that it will complete its work in 1970. After having been Chairman of the Fluorine Sub-committee since it was formed in 1965 Mr. T. R. F. 137. Fennell has found it necessary to retire owing to the pressure of other commitments.The Committee is however pleased to record that Mr. Fennell is remaining as a member of the Sub-committee and Dr. E. J. Newman has been appointed Chairman in his place. The Joint Committee with the Pharmaceutical Society has formed three new Panels during the year and all three have begun work. Full details of the Committee’s work will be published later in the separate Annual Report of the Analytical Methods Committee. It is with deep regret that Council records the death of the Honourable Mr. Justice Lloyd- Jacob an Honorary Member of the Society and Chairman of the Trustees of the Analytical Methods Trust since its formation in 1956. His wise counsel and guidance will be greatly missed. The Committees of Council and their Chairmen during the year were as follows Abstracts Editorial Committee Analyst Editorial Board and Executive Committee Analytical Methods Committee Finance Committee Group Liaison and Policy Committee Honours Committee Programmes Committee Publications Policy Committee SAC Conference Executive Committee Education and Training Committee Dr.H. J. Cluley Dr. A. A. Smales Dr. D. C. Garratt Hon. Treasurer Mr. D. W. Wilson The President Mr. A. G. Jones The President The President Dr. W. J. Williams For service on these Committees and their various Sub-committees the Society relies heavily on the voluntary work of its members. In addition there are many who serve the Society by organising Group and Section activities by refereeing papers by representing the Society on outside bodies and in a variety of other ways. To them all and to the permanent staff for their continued support the Council expresses its thanks.In March 1969 Dr. P. G. Jeffery retired from his position as the Society’s first Public Relations Officer and Mrs. D. Butterworth was appointed to succeed him. To both of them Council extends its warmest thanks for their energetic promotion of the publicity accorded to the Society and its activities. On the recommendations of the Honours Committee Council decided unanimously to award the Society’s Fourth Gold Medal to Dr. R. C. Chirnside in recognition of his long and distinguished service to analytical chemistry. In 1927 he joined The General Electric Company Limited at Wembley and was appointed Chief Chemist in 1948. When in 1960 the Wembley Laboratories became the Hirst Research Centre he was appointed head of the newly created Chemistry and Technical Services Division a post from which he retired last year.Dr. Chirnside has many times been a member of Council was the first Chairman of the Physical Methods Group and of the Abstracts Editorial Committee and was President in 1959-61 He has throughout maintained a keen interest in educational matters and in 1967 he was awarded an Honorary D.Sc. by the University of Bath in recognition of his services to chemistry and education. The Society is proud to welcome him as its Fourth Gold Medallist. March 19701 ANNUAL REPORT OF THE COUNCIL 49 Membership of the Society now totals 2291 an increase of 54 on the year. The present membership of Sections and Groups is North of England Section . . . . .. .. Scottish Section .. .. . . . * .. Western Section .. . . . . .. .. Midlands Section . . . . . . .. . . North East Section . . * . .. . . .. East Anglia Section . . .. .. .. .. Atomic Spectroscopy Group . . . . . . * . Automatic Methods Group . . . . . . .. Biological Methods Group . . . * I ) . .. Electroanalytical Group . . .. . . . . Microchemical Methods Group . . * . . . Particle Size Analysis Group .. . . . . Radiochemical Methods Group . . . . . . Special Techniques Group . . . I . . .. Thermal Analysis Group . . * . . . . . Joint Pharmaceutical Analysis Croup . . . . Chromatography and Electrophoresis Group . . 436 97 140 277 109 127 650 694 354 726 156 699 256 248 637 250 380 HOXORARY MEMBERSHIP-COUnCi1 is very pleased to record that Dr. A. Walsh (C.S.I.R.O. Australia) has been elected as an Honorary Member of the Society.LONG MEMBERSHIP-The congratulations and good wishes of the Council are extended to Sir Ronald G. Baskett Dr. J. H. Bushill Mr. J. Butler Mr. H. Childs Mr. L. S. Davis Mr. J. C. Harrall Dr. G. U. Houghton Mr. A. 0. Jones Mr. E. Q. Laws Mr. R. Mallinder Xr. C. Paterson and Mr. J. B. E. Patterson who have completed 40 years of membership. DEATHS-The Council records with regret the deaths of the following members- A. E. Beet F. Major A. 0. Rlackhurst P. N. Mould F. H. Carr W. T. Kees G. W. Ferguson F. Robinson G. J. W. Ferrey 147. W. Robson A. C. Frazer C. W. Spiers P. Gouverneur R. G. Thin Sir George Lloyd- Jacob (Honorary Member) Chronological List of Society Section and Group Meetings 1969 January 1 rith London Microchemical Methods Group. Discussion on “The Micro Determination of Chlorine and Sulphur in Organic Materials,” introduced by S.Bance and R. Goulden. 17th Bath Western Section Annual General Xeeting preceded by a Joint Meeting with Bath University of Technology Student Chemical Society. “Analytical Aspects of Flame Chemistry,” by P. J - Padley. 22nd Loughborough Midlands Section. “ 14-MeV Neutron-activation Analysis,” by G. Oldham. 32nd Durham North East Section Annual General Meeting. “The Examination of Antiquities,” by A. E. Werner. 50 ANNUAL REPORT OF THE COUNCIL [Proc. Soc. A.I.taZyt. Chenz. 24th Edinburgh Scottish Section Annual General Meeting followed by a Meeting on “Geochemical Aspects of Analysis.” “Silicate Chemistry a t 2000°C and 20,000 Atmospheres,” by G. M. Biggar. “U - Pb Isotopic Stability in Zircons,” by R.T. Pidgeon. “The Geochemistry of Recent Manganese Nodules,” by N. B. Price. 25th Manchester North of England Section Annual General Meeting. Address of the retiring Chairman W. Cule Davies. February 5th London Society organised by the Special Techniques Group jointly with the Spectro- scopy Group of the Institute of Physics on “Radiofrequency Spectroscopy.” “Microwave Spectroscopy of Gases as an Analytical Technique,” by Professor J . Sheridan. “Electron Resonance-An Introductory Survey,” by Professor D. H. Whiffen. “Possible Analytical Applications of Electron Resonance,” by G. R. Luckhurst. 13th Manchester North of England Section and -4utomatic Methods Group on “Sewer Systems in Automatic Analysis.” “Automatic Chemical Analysis-An Industrial Viewpoint,” by P.G. Jeffery. “Some Special Problems in the Use of Automatic Analytical Systems in Clinical Biochemistry,” by A. H. Gowenlock. 14th London Society Special Meeting. 19th Stoke-on-Trent Midlands Section jointly with the Midlands Section of the Royal Institute of Chemistry. lf)th Manningtree East Anglia Section on “The Analysis of Plastics Formulations.” “The Impact of Physical Sciences on Polymers and Copolymers of Styrene,” by T. B. Gay. “The Identification and Determination of Some Phenolic Stabilisers in Polyolefins,” by L. H. Ruddle. “Determination of Certain Additives in Polyethylene and Polystyrene,” by J. T. Davies. 20th London Biological Methods Group on “Methods of Estimating Allergenic Properties Associated with Antibiotics. ” “Ion-selective Membrane Electrodes,” by Profcssor E.Pungor. “Techniques in Electrophoresis,” by G. F. Reynolds. “The Clinical Background of Penicillin Hypersensitivity,” by H. P. Lambert. “Control Methods for Allergenic Impurities in 6-APA and Penicillins,” by F. 11. Batchelor and 3liss “Correlation of Laboratory and Clinical Obseri-ations on Hypersensitivity to /3-Lactam Antibiotics,” J. Dewdney. by P. W. Muggleton. 22nd Liverpool North of England Section. 25th Newcastle Korth East Section jointly with the Newcastle upon Tyne and North East Coast Section of the Royal Institute of Chemistry. 26th London Atomic-Absorption Spectroscopy Group. “The Application of Newer Techniques in the Analysis of Food Flavours,” by D. \\‘eyl. “Forensic Science,” by S. Denton. Introduction by R. C. Thompson. “Developments in Atomic Fluorescence and Atomic Absorption,” by I<.M. Aldous. “The Application of Flames to Atomic Spectroscopy,” by M. Sargent. 27 th London Chromatography and Electrophoresis Group and Radiochemical Methods Group. “The Application of Gas - Liquid and Thin-layer Radiochromatography to Drug and Liquid Meta- “The Use of Thin-layer Chromatography in Checking the Purity of Labelled Compounds,” by D. A. “Low Background Systems for Radiochromatography,” by T. H. Simpson. bolism,” by P. Johnson and H. R. Hazelton. Lambie. March 19701 ANNUAL REPORT OF THE COUSCIL 51 March 5th Sheffield North of England Section and Particle Size Analysis Group on “Inertial Methods of Particle-size Analysis.” “Use of the Cascade Impactor for Particle-size Analysis,” by ?V. J. Megaw. “Particle-size Analysis with the Sharples Super Centrifuge,” by J.A. M. McLean. “Air Classification of Flour with the Bahco,” by N. I,. Kent. “Use of the Cyclosizer for Particle-size Analysis,” by C. G. L. Treasure. 7th London Society Annual General Meeting. 1 lth Glasgow Scottish Section Special Meeting. “Complexometric Titrations,” by R. Pribil. l l t h London Microchemical Methods Group. 12th Xottingham Midlands Section and Special Techniques Group jointly with the East Midlands Section of the Royal Institute of Chemistry and the Nottingham Section of the Society of Chemical Industry on “Pyrolytic Gas Clirornatography.” “Pyrolysis - Gas Chromatography in the Vapour Phase,” by S. G. Perry. “Analytical Techniques with Curie-point Pyrolysis,” by N. B. Coupe. “The Application of Pyrolysis - Gas Chromatography to the Analysis of Polymeric JIaterials,” by “Scope and Limitations of Polymer Pyrolysis,” by C.E. Roland Jones. “Pyrolysis - Gas - Liquid Chromatography Applied to Study Kinetics and Mechanisms,” by R. S. “Pyrolysis - Gas Chromatography of Biological Macromolecules,” by ill. V. Stack. Address of the retiring President entitled “Our Publications-Present and Future,” by A. G. Jones. Discussion on “Specific Ion Electrodes,” introduced by G. J. Kakabadse. P. E. Arnold. Lehrle. 12th Nottingham Midlands Section Annual General Meeting. ZOth Middlesbrough North East Section jointly with the North East Metallurgical Society and the Teesside Section of the Royal Institute of Chemistry. “Emission Spectroscopy in the Steel Industry and its Application to the Analysis of Steel-making Slag,” by P.S. Bramhall. 20th Birmingham Midlands Section Special Meeting. 21st Leeds North of England Section jointly with the Leeds University Union Chemical Society. Zlst Glasgow Scottish Section on “Recent Progress in Voltammetry.” “Complexometry its Recent Progress and Influence on Analytical Chemistry,” by R. Pribil. “Automatic Sampling and Analysis,” by A. C. Docherty. “Principles of Voltammetry,” by E. Bishop. “Voltammetry as a Theoretical Basis of Electrolytic Analytical Methods and a Tool for the Investigation “Recent Developments in Analytical Voltammetry,” by R. C. Rooney. of Electrode and Chemical Reactions,” by K. Stulik. 21st Swansea Western Section jointly with the South Wales Section of the Royal Institute of Chemistry. “Recent Progress in Metallurgical Analysis with Particular Reference to the Iron and Steel Industry,” 28th and 29th Bangor Microchemical Methods Group on “Microanalytical Methods in Agricultural Chemistry.” by B.Bagshawe. “Microanalytical Methods in Agricultural Chemistry,” by H. Egan. “Residues Information-Purpose and Requirements,” by J. A. R. Bates. “The Use of Microanalytical Methods in Studies of the Control of Insect Pests of Stored Products,” “The Use of Ion-exchange Resins in Residue Analysis,” by A. Calderbank. “Microanalytical and Radiochemical Methods in Studies of Plant Growth and Nutrition,” by E. R. “The Determination of Nitroxynil in Meat by Polarography,” by M. Parnell. “Automated Enzymic Analyses of Hypoxanthine in Flesh Foods as Quality Indices,” by N. R. Jones. “Some Microchemical Methods Associated with Pest Control,” by S.Bailey and A. Taylor. “Microanalysis in Some ,2spects of Horticultural Chemistry,” by J. T. Martin. by D. F. Horler. Mercer. 52 ANNUAL REPORT OF THE COUNCIL [Proc. Soc. Analyt. Chew. “Microanalytical Methods in the Study of Plant Surfaces,” by P. J. Holloway. “Microanalysis of the Trace Metals in Biological Materials,” by C. F. Mills. “Methods of Examining the Distribution of Micro Nutrient Elements in Soil,” by R. I. Davies. “The Determination of Trace Elements in Fertilisers,” by J . M. Skinner. “Some Methods in Use in the Study of the Utilisation of Protein by Animals,” by R. A. Evans April lst London Society Demonstration Meeting organised by the Automatic Methods Group. “The R61e of the X.R.D.C. in the Development and Exploitation of Inventions,” by G.M. Blunt “Automatic Radiofrequency Titrator,” by G. Svehla W. J . Scott and R. K. Quigg. “Motorised Rack for Multiple Fusions in Test-tubes,’’ by P. J . Moore G. R. Brumby and G. T. Gook. “Automatic Determination of Alcohol,” by R. Sawyer and P. B. Stockwell. “A Simple Trace Reader with Digital Print-out,’’ by J . B. Dawson and K. Milner. “Determination of Potassium by an Automatic Ultraviolet Absorptiometric Method,” by J. M. Skinner. “Flexible Electrophoresis Applicator for Use with an AutoXnalyzer in Routine Protein Analysis,” “Automatic Sample Loader,” by G. W. Goodman. “Automatic Digester Sample Changer and Semi-automatic Work Aids,” by J . Hunt. “Automatic Diluter,” by J . S. Wragg D. F. C. Crawley and D. F. Spooner. “Semi-automatic Method for the Determination of Crystallising Point,” by G.W. Girling and J. “Automatic Ion-exchange Separation in Radiochemistry,” by H. J . M. Bowen. “Reaction Coil for Automatic Amino-acid Analysis,” by S. Jacobs. “A Differential Enthalpimetric Titrator. “A Compressed-air Hand-controlled Valve for Filling Burettes with Titrant ” by W. Sebborn. “Automatic Determination of the pH Value of Soil Samples,” by J . L. 0. Jones. “Automatic Dumas Nitrogen Analyser,” by J. B. Hamilton. “Macromolecular Models,” by I. Smith. “Cool Diffusion Flames ; Spectral Line Sources ; Separated Flames,” by Professor T. S. ?Vest. “Rapid Determination of Water-immiscible Liquids,” by T. Kennedy. “Continuous Polarography,” by B. Fleet. “The Dialysis of Small Volumes (5 to 50 p1) of Fluid,” by N. G. Heatley. “A Simple Cutting Holding and Back-flushing Arrangement for Dual-flame Ionisation Chromato- by M.E. Carruthers. Pentelow. An Enthalpimetric Analyser for the Continuous Measure- ment of Macro Amounts,” by R. P. Taubinger. graphs,” by N. Mellor. 1st and 2nd Leeds Thermal Analysis Group jointly with the Clay Ninerals Group of the Mineralogical Society on “Thermal Analysis in Clay Mineralogy.” “Investigation by Differential Thermal Analysis of Reactions During Hot-pressing,” by T. G. “The Determination of Quartz in Clays by Differential Thermal Analysis,” by 1. G. White and R. W. “Thermal Decomposition of Flocculated Clay Samples,” by D. Dollimore G. R. Heal and T. Horridge. “The Role of Thermal Analysis in the Evaluation of Impure Clay Deposits as Mineral Raw Materials,” “Structural Formulae of Hectorite Derived from Thermogravimetry,” by B.S. Neumann. “The Application of Gas Evolution Analysis to the Determination of Structural Hydrogen in Layer “The Kinetics of Dehydroxylation of Silicates from Thermogravimetric and Isothermal Experiments,” “Mossbauer Studies of the Thermal Reactions of Kaolinites,” by K. J. D. Mackenzie. “Methods and Techniques Used in the Study of the Poorly Ordered Components of Soil Clays,” by 16th Luton Midlands Section jointly with the Mid-Anglia Section of the Royal Institute of Chemistry . 18th Preston North of England Section jointly with the North Lancashire Section of the Royal Institute of Chemistry. 18th Chepstow Western Section. Carruthers. Grimshaw. by J. A. Bain and D. J. Morgan. Silicates,” by A. C. D. Newman. by J. H. Sharp. J. M. Bracewell A. S. Campbell and B.D. Mitchell. “Non-dispersive X-ray Fluorescence Analysis,” by T. W. Packer. “Chromatographic Methods of Pesticide Residue Analysis,” by J. O’G. Tatton. Discussion on “Electrical Methods of Analysis,” introduced by G. W. C. Milner A. J . Wood G. Phillips and R. H. Davies. 22nd Middlesbrough North East Section jointly with the Teesside Section of the Royal Institute of Chemistry. “The Work of a Textile Chemical Consultant,” by W. Garner. March 19701 ANNUAL REPORT OF THE COUNCIL 24th London Biological Methods Group. “Recent Advances in the Assay of Vitamin B, and its Co-enzymes,” by L. Mervyn. 53 25th Edinburgh Scottish Section and Chromatography and Electrophoresis Group on “Chromatography.” “Laminar Chromatographic Studies of the Wool-epicuticle and Amino-acids,” by E.I-. Truter. “Thin-layer Chromatography of Plant Phenolics,” by J. M. Philp. “Non-aqueous Ion Exchange of Weak Organic Acids,” by J. D. R. Thomas. “The Application of Gas - Liquid Chromatography to the Detection of Pollutants in Rivers,” by A. W. “The RM Concept,” by L. S. Bark. “Molecular Sieve Chromatography,” by D. M. W. Anderson. Davies. 29th London Radiochemical Methods Group on “The Uses and Measurement of Tritium.” “Problems Peculiar to the Use and Misuse of Tritium Compounds,” by E. A. Evans. “The Measurement of Tritium,” by R. D. Stubbs. “Tritium in Autoradiography,” by S. R. Pelc. “Low Level Tritium Measurements,” by R. L. Otlet. “Industrial Uses of Tritium,” by D. S. Glass. “The Uses and Measurement of Tritium in Steroid Biochemistry,” by I. Sommerville. “The Use of Tritium in Investigating the Origin of Milk Fat,” by R.I?. Glascoclr. 30th London Microchemical Methods Group. Discussion on “The Use of Instruments in the Analysis of Organic Materials,” introduced by A. G. Jones. May 7th London Particle Size Analysis Group on “Why Particle-size Analysis ?” “Particle-size Aspects of Cement Technology,” by R. G. Rlezard. “Particle-size Analysis in Powder Metallurgy,” by V. T. Morgan. “The Importance of Particle-size Analysis in Studies on the Rheological Properties of Emulsions,” by “Size Analysis and the Effects of Dispersion,” by W. E. Craker. “Particle-size Analysis in the Pharmaceutical Industry,” by N. A. Armstrong. “Particle-size Analysis of Pigments,” by V. T. Crowl. P. Sherman. 8th Belfast Society meeting on “Research Topics in Analytical Chemistry.” “The Analytical Chemistry of Bithionol and its Metal Complexes,” by A.Gray A. G. Fogp and D. “A Highly Sensitive Method for the Determination of Arsenic,” by C. A. Watson “Some Coulometric and Volumetric Acid - Base Titrations in Semi-aqueous Media,” by D. \IT. Whymark “The Applications of the Chemiluminescence of Benzazoles,” by A. Rixon and L. S. Bark. “What Happens When Solutions of Dithizone Deteriorate,” by D. C. Rupainwar and Professor “A Study of Salicylideneamino-2-thiophenol Some Related Compounds and their Tin Complexes,” “The Determination of Trace Amounts of Calcium in Stainless-steels by Solvent Extraction followed “Analytical Utility of the Metal Complexes of Alizarin Fluorine Blue,” by M. A. Leonard and I;. I. n’agi. Thorburn Burns. and J. M. Ottaway.H. M. N. H. Irving. by Mrs. J. Kingshott. by Atomic-absorption Spectrometry,” by J . Richardson. 14th Colchester East Anglia Section on “Applications of Spectroscopy.” “Fluorescence Spectroscopy and its Applications,” by G. F. Moss. “Chemical Uses of Proton Magnetic Resonance,” by P. D. Ralph. “X-ray Fluorescence Analysis,” by G. D. Woodward. 22nd Beckenham Biological Methods Group Summer Meeting. Visit to the Wellcome Research Laboratories. 30th to June 2nd Scarborough North of England Section Summer Meeting. 31st Rode Western Section Summer Meeting. “Evolution of the Ice Cream Industry,” by K. A. Hyde. “Industrial Archaeology of the Cloth Industry,” by I<. Hudson. 51 XSXUAL REPORT OF THE COUNCIL [Pvoc. SOC. Analyt. Chem. July 14th to 18th Sheffield Atomic-Absorption Spectroscopy Group jointly with the Spectro- scopy Group of the Institute of Physics.International Atomic Absorption Spectroscopy Conference. 21st to 25th Birmingham Midlands Section. International Symposium on Analytical Chemistry. August 7th’ Glasgow Scottish Section Special Meeting. “Some Current Research in Atomic Absorption,” by A. Walsh. September 17th London Eadiochemical Methods Group. Discussion on “Errors in Radiochemical Analysis ” introduced by H. J. &I. Bowen. 19th and 20th Portsmouth Microchemical Methods Group jointly with the Mid-Southern Counties Section of the Royal Institute of Chemistry on “The Application of Microchemical Techniques in the Petrochemical and Allied Industries.’ ’ “Recent Advances in the Application of Organic Elemental Analysis ” by P. Gouverneur.“Determination of Trace Components of Petrochemical Products,” by G. B. Crump. “Polymeric Analysis by Micropyrolysis Gas - Liquid Chromatography,” by G. Bagby. ‘‘A Gas-chromatographic System to Facilitate the Mass-spectrometric Analysis of Minor Deuterated “New Developments in the Chromatography of Petroleum Products,” by S. G. Perry. “Identification of Hydrocarbon Oils by Added Markers,” by K. Field. “Some Uses of Flask Combustion in the Analysis of Lubricants,” by 31. Lonsdale. “The Determination of Low Concentrations of Metals in Lubricating Oils by Spectrometric Methods,” “Research in Polytechnics,” by W. Davey. “Micro-analytical Techniques in the Analysis of Fuels,” by F. C. A. Killer. “The Determination of Trace Metals in Fuels by Atomic Absorption,” by J. Scott. “Quantitative Elemental Analysis of Small Liquid Samples (less than 1 nil) by X-ray Fluorescence,’’ Components in a Gas Mixture,” by D.Shepherd. by C. C. Washbrook and D. Pickles. by R. W. Williams. 24th Coventry Midlands Section. Discussion on “Membrane Electrodes,” introduced by R. A. Carter G. J. Icakabadse and A. M. G. Macdonald. 24th Bristol Western Section and A4tomic-Absorption Spectroscopy Group jointly with the Bristol and District Section of the Royal Institute of Chemistry on ‘Li4pplications of Atomic- absorption Spectroscopy. ” “The Use of Atomic-absorption Spectroscopy within the G.K.N. Group,” by R. M. Baldwin. “Some Applications of Atomic-absorption Spectroscopy to Agricultural Analysis,” by T. Williams. “Determination of Silver and Gold in Raw Materials and Products of Zinc and Lead Smelting,” by “A Consideration of Performance Capabilities of Atomic-absorption Spectrophotometers in Relation to “Aspects of Atomic-absorption Spectroscopy a t B.D.H.,” by R.Farrow. H. Edwards. Design Characteristics,” by R. J. Reynolds. 24th Bradford Particle Size Analysis Group. “Current Research in the School of Powder Technology a t the University of Bradford,” by J. C. Williams. “Surface Area Determination by the Diffusion of Air through Packed Beds of Powder,” by N. G. “Flow Microcalorimetry,” by R. M. Patel. “X-ray Sedimentometer,” by L. Svarovsky. “Particle Sizing by Automatic Image Analysis,” by A. C. Terrell. Stanley-Wood. 25th Motherwell Scottish Section. “X-ray Fluorescence and Emission Spectroscopy in Steelworks Analysis-Competitive or Complemen- tary?” by K.M. Bills. March 1970 ANSUAI REPORT OF THE COUNCIL 55 October lst London Society. “Computerised Titrations-l’nravelled Stoicheiometry and High Accuracy,” by Professor D. ‘IV Dyrssen. k d Cardiff Western Section. 4th Liverpool North of England Section. 7th Edinburgh Scottish Section jointly with the Edinburgh Branch of the British Computer Society. “Computerised Titrations-Unravelled Stoicheiometry and High Accuracy,” by Professor D. ‘IV. “Solvent Extraction,” by Professor D. TV. Dyrssen. “Industrial Aspects of Food Analysis,” by A. Turner. Dyrssen. 7th Belmont North East Section Social Meeting. “Close-ups in Colour,” by W. R. Lovesey. Hth London Microchemical Methods Group. Discussion on “The Micro Determination of Fluorine-specific Ion Electrodes versus Othcr Methods,” introduced by T.R. F. W. Fennell. 15th Birmingham Midlands Section on “Computer Applications.” “Introduction to Computers,” by R. K. Webster. “Computer Monitoring of Analytical Equipment Personnel and Samples,” by J. F. Becker. “Data Acquisition from Analytical Systems,” by J. A. Xewell. “‘The Use of Computers in Identification of Organic Compounds,” by W. Kelly. “An Automated Laboratory for Gas Chromatography,” by P. Mitchell. Wnd Ipswich East Anglia Section Annual General Meeting. Brd London Biological Methods Group. “:\mplification Reactions,” by Professor R. Belcher. “Interferon and its Antiviral Properties,” by R. D. Xndrews. November 5th London Society meeting on “Water Analysis.” “Water Sources and their Treatment,” by R. F. Packham. “Examination of Potable Water,” by A.T. Palin. “Analysis of Industrial Waters,” by T. D. Rees. “The Analysis of Aqueous Effluents and Polluted River Waters,” by H. -1. C. Montgomery. “On-line Analysis in Water Systems,” by A. A. Diggens. “Analysis of Water for High Pressure Boilers,” by W. G. Cummings. 7th and 8th Carlisle North of England Scottish and North East Sections and Microchemical Methods Group on “Recent Advances in Pharmaceutical Analysis with Special Reference to Microchemical Techniques.” “The Detection and Determination of Low-level Constituents in Pharmaceutical Products,” by C. A. “Problems Associatcd with the Detection of Impurities in New Drugs,” by \V. H. C. Shaw. “The Determination of Parts per Million of Mercury in Eye Drops by Atomic Absorption,” by W. H. “Analysis of Degraded Pilocarpine Solutions,” by J.B. Murray. “The Use of the Vitatron Integrating Densitometer for the Direct Measurement of Substances Separated “The Determination of Cephalosporin C in Fermentation Liquors with the Chrotnoscan Densitometer,” Johnson. Harper. by Thin-layer Chromatography,” by W. H. C. Shaw. bv P. Pulurrav. “Somi ExperienLes and Problems in Human Metabolic Research,” by A. Robertson. “The Application of Gas Chromatography to Official Monographs,” by J. C. Deavin. l2th Birmingham Midlands Section. “The Micro-coulometric Determination of Nitrogen Chlorine and Sulphur in Hydrocarbons,” by “Sonic Modern Electroanalytical Techniques,” by P. Zuman. F. C. A. Killer. 56 ANNUAL REPORT OF THE COUNCIL [PYOC. SOC. Analyt. Chew. 12th London Thermal Analysis Group Discussion Meeting on “Some Aspects of Tnstrumenta- tion.” “The Determination of Water,” by T.P. Lees. “Mass Spectrometry - Differential Thermal Analysis ” by M. Bracewell. “Low Temperature Differential Thermal Analysis,” by B. Treherne. 13th London Thermal Analysis Group Annual General Meeting followed by a meeting on “Evolved Gas Analysis and Detection.” “Studies of Polymer Stability and Decomposition Products by Thermal Volatilisation Analysis,” by “Evolved Gas Analysis of Hydrogen and Other Vapour Species from Hydrous Silicates,” by I<. J. D. “An Introduction to the Use of Mass Spectrometry with Gas - Liquid Chromatography and Differential “The Use of Partial Pressure Mass Spectroscopy in the Thermal Analysis Studies of Carbon and “The Use of Gas - Liquid Chromatography in Investigating Products Desorbed on Heating Organic 13th London Automatic Methods Group Annual General Meeting preceded by a meeting on “User Experience on Data Recovery Equipment in Automatic Analysis.” I.C. McNeill. Mackenzie. Thermal Analysis Systems,” by W. A. Wolstenholme. Graphite,” by J . Dollimore C. M. Freedman and B. H. Harrison. Compounds Chemisorbed on Oxide Surfaces,” by A. K. Galwey. “Computer Dependent Data Processing in Clinical Chemistry,” by L. G. Whitby. “Gas-chromatographic Data Recovery by Computer,” by J . G. Lyons. 14th Chepstow Western Section. 17th London Radiochemical Methods Group Annual General Meeting. 18th London Special Techniques Group Annual General Meeting. “Some Analytical Problems in Egg Research,” by T. L. Parkinson. Zlst London Microchemical Methods Group Annual General Meeting followed by a Group Dinner.25th London Particle Size Analysis Group Annual General Meeting followed by a meeting on ‘ ‘ Present a tion of Particle-size Distributions. ’ ’ Discussion on “Determination of Moisture,” introduced by C. Harris. “Theory and Practice of Scintillation Counting,” by J. B. Birks. “Graphical Presentation,” by Professor H. Heywood. “The Characterisation of Particulate Systems,” by B. Scarlett. 26th Eastham North of England Section jointly with the Carlett Park Chemical and Physical Society. 26th London Chromatography and Electrophoresis Group Annual General Meeting followed by a meeting on “Isoelectric Focusing.” “Steric Hindrance in Analytical Chemistry,” by Professor H. M. N. H. Irving. “Some Analytical Applications of Isoelectric Focusing,” by J.S. Fawcett. “Serum Protein Heterogeneity Studied by Isoelectric Focusing in Polyacrylamide Gel,” by A. R. 26th London Electroanalytical Group Inaugural Meeting followed by a meeting on “Selective Electrode Systems.” Williamson. “Glass and Solid-state Electrodes,” by K. Covington. “Liquid Ion-exchange Resin Membrane and Related Electrodes,” by €3. Fleet. “Galvanic and Related Electrode Systems,” by J. Tenygl. 28thJ Glasgow Scottish Section jointly with the Andersonian Chemical Society. “The Impact of Instrumental Methods on Organic Analysis,” by A. G. Jones. December 2nd London Atomic Spectroscopy Group (formerly the Atomic-Absorption Spectroscopy Group) Annual General Meeting. “Practical Aspects Involved in the Automation of Atomic-absorption Spectroscopy,” by J . Varley.International Atomic Absorption Spectroscopy Conference Sheffield 1969- “A Review of Theoretical Aspects,” by G. F. Kirkbright. “A Review of Practical Aspects,” by R. White. March 19701 ASNUAL REPORT OF THE COUNCIL 57 2nd London Biological Methods Group Annual General Meeting. Discussion on “Statutory Requirements for Biological Substances of the B.P.,” introduced by G. A. Stewart. 3rd London Society meeting on “Scanning Techniques.” “ X-Ray Micro-analysis Techniques,” by Miss P. J . Killingworth. “X-Ray Milliprobe Analysis,” by J . D. Wilson. “Examination of Surfaces by Scanning with Charged-particle Beams,” by T. B. Pierce. 3rd Huddersfield North of England Section jointly with the Huddersfield Section of the Royal Institute of Chemistry. 4th Gateshead North East Section jointly with the Newcastle upon Tyne and North East Coast Section of the Royal Institute of Chemistry and the Newcastle upon Tyne Section of the Society of Chemical Industry on “Trade Wastes and Industrial Effluents.” “Nuclear Methods in Trace Element Analysis,” by A.A. Smales. “Control of Pollution,” by R. J. H. Dyson. “Effluent Problems in the Chemical Industry,” by N. A. Dobson. “The Determination of B.O.D. C.O.D. and Total F b o n Content,” by G. M. Woodward. “Recent Advances in the Field of Water Pollution “Effluent Problems of a Modern Brewery,” by J. R. Simpson. “Automatic Monitoring and Control of Effluent Treatment,” by G. V. R. Mattock. by A. B. Wheatland. 5th Cardiff Western Section jointly with the Cardiff and District Section of the Royal Institute of Chemistry and the South Wales Section of the Society of Chemical Industry. 9th London Microchernical Methods Group. loth Birmingham Midlands Section. “Gel-permeation Chromatography,” by F. W. Peaker Discussion on “C.H.N. Automatic Analyzers,” introduced by H. G. Baxter. “Methods for the Determination of Fluorine (Other than Radiometric),” by J. K. Foreman. “The Determination of Fluorine by Neutron-activation Analysis,” by P. G. Jeffery. T. S. WEST President PV. H. C. SHAW Honorary Secretary

ISSN:0037-9697    

DOI:10.1039/SA9700700045

出版商:RSC    

年代:1970

数据来源: RSC

摘要:

58 SCANNIKG TECHSIQC-ES [Proc. SOC. Analyt. Clzem. Scanning Techniques The following are summaries of two of the papers presented at an Ordinary Meeting of the Society held on December 3rd 1969 and reported in the December 1969 issue of Proceedings Electron Probe X-ray Microanalysis A General Review (p. 203). BY MISS P. J. I<ILT.ISG\VORTH (Canzbi4dge Scieizti3c Instruments Limited Electyoit-Probe Dicisioiz Cawzbridge CB4 3A W ) THE use of electron-beam excited X-radiation as the basis of a quantitative analytical tech- nique was first proposed by Castaing,l who used a stationary electron beam of about 1pm diameter incident upon the specimen. The limitations of this instrumentatioii were quickly appreciated in particular the time-consuming operations required to obtain concentration profiles and led to the development a t the Cavendisli Laboratory Cambridge of an instrument incorporating beam-scanning facilities.1 S FOR N AT I 0 I\; PR E SE STATION- Present day microanalysers are generally able to present information in one of t h e e forms . Qualitative distribution images are formed by deflecting the electron beam in a square raster over the surface of the specimen with the X-ray spectrometer set to detect X-rays from the element under investigation. In this mode the intensity of X-ray signal varies with the position of the electron beam and can be used to modulate the brightness of a cathode-ray tube scanned in synchronism with the beam building up an element distribution display. A comparison of element concentration in neighbouring areas (obtained by such a method) will be purely qualitative and can usefully be augmented by scanning more slowly across a single line on the specimen and recording the integrated intensity output as y-deflection curve either on the cathode-ray tube superimposed upon the distribution image or on a pen recorder for more accurate evaluation.Finally fully quantitative analysis can be achieved by positioning a stationary electron beam upon the area of interest and recording the X-ray intensity from each of the constituent elements. The intensities are compared with those from standard materials which are usually pure elements. To a first approximation the concentration C,4 of element A can then be T expressed as CA = 2 speci*nen x 100 where I A specimt.n is the recorded intensity from the speci- men and I pure is the recorded intensity from a standard of pure A.IA pure QUASTITATIVE CORRECTION PROCEDURES- If a more accurate evaluation is required some consideration must be given to the mech- anism of X-ray production within the specimen and to the interaction of the emergent X-ray beam with the specimen material. This leads to the derivation of a number of correction factors. The atomic number eflect-This is compounded of two opposing functions dependent upon the back-scatter coefficient and the electron-stopping power of the specimen. Several methods for determining these effects have been proposed much of the original work having been carried out by Thomas.2 For practical purposes this effect can be considered to increase with increasing atomic number difference of the constituent elements.An absorption correcfion-This is generally required to compensate for the difference in absorption of the measured X-rays during passage through the specimen compared with those emitted by the standard. Several correction procedures have been proposed but it is now generally accepted that the proposals of Philibert3 provide the best compromise between scientific accuracy and a workable formula for everyday use when certain parameters are modified in accordance with Heinrich* or Duncumb Shields-Mason and da C a ~ a . ~ As the mathematical process involved is iterative it lends itself particularlv to computer evaluation. March 19701 SCANNING TECHNIQUES 50 FLuorescence efects -These arise from excitation of secondary X-radiation and take two forms the more significant of these being excitation by the characteristic primary X-rays resulting in enhanced intensity of the detected low energy radiations at the expense of those of high energy.Correction for K and L series radiation has been described by Reed,6 but no satisfactory procedure is yet available for systems involving M series spectra; and for most purposes the minor component of radiation due to the continuum must be ignored. Until now it can reasonably be said that the accuracy of quantitative analysis has been limited by correction procedures rather than instrumentation. Use of the best correction procedures now available in conjunction with most recent values of the relevant coefficients indicates that for some elemental systems at least this is no longer the case and further instrumental development will again lead to improved results.XEW TECHNIQUES I S M1CROA4NALYSIS- Development now hinges around improved facilities peripheral to the technique. The use of servo-operated controls has already reduced the number of precise setting operations required during a quantitative analysis and is capable of further extension. The combination of X-ray spectrometry with transmission electron microscopy allow the identification of particles well below the normal mini1nur-n size although the analysis is no longer strictly quantitative. Finally with the development of detection systems for the wavelength range 1 to 10 nni it is now possible to determine with a suitable spectrometer the wavelength shifts and peak shape variations due to valency bonding for the lighter elements.Research on these semi- optical spectra opens up new forms of microanalysis. REFEREXES 1. Castaing R. Ph.D. Thesis University of Paris 1951. 2 . Thomas I?. M. Brit J . AppZ. Phys. 1963 14 397. 3. Philibert J. “X-Ray Optics and X-Ray Rlicroanalysis,” \‘olumr 3 Llcade~nic Press 1963 p. 379. 1. Heinrich K. F. J . “Abstracts of the 2nd National Conference on Electron Probe hIicroanalysis 5. Duncumb P. Shields-Mason P. I<. and da Casa C. “Proceedings of the Vth International 6. Boston Mass.,” Paper 7 1967. Congress on S-Ray Optics and Microanalysis,” Springer-I-erlag Heidelberg In the press. Reed S. J. B. Brit. J . AFpl. Phys. 1965 16 013. The Examination of Surfaces by Scanning with Charged-particle Beams BY T. R. PIERCE (Analytical Sciences Division Atomic Enevgy Heseavch Establishtneizt Harwell Near Didcot Bevkshive) XUCLEAR interactions induced by charged particles which are used as the basis for activation- analysis procedures can be broadly divided into two major categories those resulting in the production of radioactive isotopes and those producing prompt events that are suitable for measurement.The former normally require particle energies of at least a few million eV the latter need lower particle energies varying from a few hundred lteV to a few MeTr. ,4s charged particles lose energy relatively rapidly on passage through matter interaction of low-energy charged particles will be restricted to the surface layers of a thick target and only a limited volume of sample will be irradiated if the diameter of the primary incident particle beam is small. Thus analytical methods based on charged-particle irradiation can be readily adapted to scanning operation provided that prompt radiation emitted during the irradiation can be measured.’ Compared with established methods of small-volume analysis such as the electron microprobe charged-particle microprobe techniques have until recently received little attention from the analyst and are therefore a t an early stage of development.Rut their ability to provide analytical methods for the determination of light elements such as carbon and oxygen has prompted recent investigation. 60 SCASSISG TECHNIQUES [Yroc. SOC. Analyt. Chem. Analytical methods have been based on the measurement of three different types of radiation that are emitted as a result of nuclear interaction these are prompt y-radiation,2 particle groups produced as the result of nuclear reaction3 and particles scattered elastically from the sample during irradiation.* In addition X-rays are produced during charged- particle irradiation and can be used in positive-ion microprobe techniques,5 but X-ray methods are not considered here.Prompt y-radiation is produced by the de-excitation of excited nuclear states produced as a result of nuclear reaction. As prompt y-radiation can be excited during stable to stable transitions it is not necessary for a radioisotope to be produced for analysis to be possible. For example irradiation of carbon with deuterons of about 1 MeV will result in the reaction 1% (d,p) 13C producing carbon-13 in its first excited state which then decays promptly with the emission of a 3-09-MeV y-ray even although both carbon-12 and carbon-13 are stable nuclei.As by careful choice of both particle and energy prompt y-lines can be excited from most of the light elements this method is generally applicable to the determination of light elements in surfaces. When several elements contribute lines to the accumulated y-spectrum conventional methods of y-ray spectroscopy can be used to distinguish con- tributions from the different elements. Neasurement of particle groups for example protons emitted from the l2C (d,p) 13C reaction instead of prompt y-radiation is sometimes preferable to follow the progress of a nuclear reaction. As particle peak shapes are sensitive to the thickness of the layer from which the particles are produced the method is well applied to the examina- tion of thin films of light elements present on surfaces.The energy of particles scattered elastically from target nuclei can also be used to provide information about surface com- position. Most sensitive results are obtained when a thin film of a heavy element present on a light element matrix is being examined as under these conditions the contribution from the thin film is free from any background caused by particles scattered from the substrate. Any of the three analytical methods summarised above can provide information about a small volume of sample in suitable cases and can be used in scanning techniques provided that the diameter of the incident particle beam is restricted and that the region of the sample from which the radiation yield is emitted is known. Particle accelerators capable of producing particles and energies suitable for analysis are usually designed for general-purpose operation and little attention has so far been paid to thc possibility of providing small-diameter ion beams suitable for microprobe work.How- ever it has been shown that by combination of four specially designed quadrupole lenses in a Russian quadruplet arrangement beam diameters of less than 4 pm can be achieved (J. A. Cookson and I;. D. Pilling unpublished work). Restriction of beam diameter limits the total beam current available for use but 6 nA of 3-MeV protons have been obtained with a 3-MeV electrostatic generator. Scanning of the particle beam across the sample can be carried out by moving the position of the sample with respect to the beam either mechanically or by electrostatic beam deflection.In the work carried out within the Analytical Sciences Division A.E.R.E. scanning is usually discontinuous the position of the beam on the sample being changed between irradiations. So far positive-ion microprobe techniques have found their main application in the determination of light elements such as boron carbon nitrogen oxygen fluorine magnesium and aluminium distributed in surfaces or for examination of thin films of light elements present on sample surfaces for example films containing carbon and oxygen present on metal substrates. However elastic scattering has been used to investigate thin films of some heavy elements for example contaminant films of heavy elements present on the surfaces of alumina insulators and gold films on silicon slices. REFERENCES 1. 2. 3. 4. 5. Pierce T. B. Peck P. F. and Cuff D. R. A. Nucl. Inst. Meth. 1969 I 67. Pierce T. B. and P?Fk P. F. i p z Shallis P. W. Editor “Proceedings of the S.lC Confcrcncc W. Heffer & Sons Ltd. Cambridge 1965 p. 159. Amsel G. and Samuel D. Phys. Chem. Soc. 1967 23 1707. Rubin S. in Kolthoff I. M. and Elving P. J. Editors “Treatise on Alnalytical Chemistry,” Poole D. M. and Shaw J. I,. U.K. _4tomic Energy Authority Repovt A.E.R.E. R5918 1968. Nottingham 1965 Part I Volume 4 Interscience Publishers Inc. New York p. 2075.

ISSN:0037-9697    

DOI:10.1039/SA9700700058

出版商:RSC    

年代:1970

数据来源: RSC

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March 19701 AMPLIFICATION REACTIONS 61 Amplification Reactions The following is a summary of the paper presented a t a Joint Meeting of the Scottish Section with the Edinburgh University Chemical Society held on February 17th 1970 and reported in this issue of ProceediPzgs (p. 43). Developments in the Application of Amplified Reactions in Analytical Chemistry BY R. BELCHER (Department of Chemistry Frankland Building The Univevsity of Birmingham P.O. Box 363 Birmingham 15) AMPLIFICATION (or multiplication) reactions were first used more than a century ago but were not known by that particular name. They were given this name in the early days of microanalysis when they were used extensively (as they still are) in the determination of iodine and methoxy1.l They may be defined as reactions in which the normal equivalence is altered or circumvented in some way so that a more favourable measurement can be made.There are two kinds of amplification reaction direct and indirect. In direct ampli- fication reactions the constituent required is amplified directly and is measured as such whereas in indirect amplification an ion or radical associated with the desired constituent is amplified and measured. Most amplification reactions are based on indirect processes. There has been a revival of interest in these methods for it has been realised that by their application to trace analysis the lower limits of certain instruments can be extended. AMPLIFICATION OF HALIDES- One of the first reactions to be known as an amplification reaction was that used for the micro determination of iodine in organic compounds (Leipert in 1929).Iodide is oxidised to iodate and on acidification and addition of excess of iodide a 6-fold amount of iodine is liberated Reactions of this type had been known since the beginning of the century.1 Other methods of amplifying iodine have been described1; this is probably the element easiest to amplify. Possibly the most interesting is the method in which periodate is used. 310,- + I- = 4103-. It can be seen that a 24-fold amplification is possib1e.l Bromide can be amplified by oxidation to bromate but the reaction demands more stringent conditions than the corresponding iodide reaction. A 4 variety of reactions is also available for this amplification but oxidation with hypochlorite is undoubtedly the best. Hypochlorite also oxidises iodide to iodate so that it is possible to determine iodide and bromide in admixture by amplification reactions.Chloride cannot be amplified directly. When oxidised chlorine is produced which forms hypochlorite and some chloride ion ; the hypochlorite then forms chlorate and more chloride ion. Several other exchange reactions have been described.l Indirect amplification is possible by use of exchange reactions. For example- AgIO + C1- = AgCl + 10,-. A4PPLICATIONS O F THE IODIDE AND BROMIDE AMPLIFICATION METHODS- Alkoxyl groups are determined by a modification of Zeisel’s method; the alkyl iodide In the determination of oxygen in organic compounds the carbon is converted into iodate. monoxide formed reacts with iodine pentoside- 5CO + I,O -+ 5C0 + I,. The reaction is unfavourable for iodimetry but after amplification of the iodine3 a favourable measurement is obtained.Kirsten* amplifies the gravimetric method in an ingenious way. Both the iodine and carbon dioxide pass into an Askarite tube which is weighed. Traces of iodine or bromine in various forms are readily determined by amplification.1 62 AMPLIFICATION REACTIONS [Proc. SOC. Analyt. Cherii. IXDIRECT AMPLIFICATION OF METALS- When metals form complexes with organic ligands which can be separated in some way it is often possible to determine the metal via the ligand. For example metal 8-hydroxy- quinolinates can be precipitated and the 8-hydroxyquinoline determined by titration with bromate. As 1 mole of 8-hydroxyquinoline requires 4 equivalents of bromate amplification results; it is greater the higher the valency of the metal.An even greater amplification is obtained if cerium( IV) perchlorate is used. One mole of 8-hydroxyquinoline consumes 29-P equivalents of cerium(1V). MISCELLANEOUS DETERMINATION- One traditional method for the determination of phosphorus gives a remarkable amplifica- tion. After precipitation as ammonium phosphomolybate the latter is converted into lead molybdate. The final precipitate weighs about 140 times the weight of the original phosphorus. Titrimetric methods in which the yellow precipitate is titrated with alkali or the molyb- denum(V1) is reduced to molybdenum(V) or (111) are also indirect amplification methods. Colorimetric methods based on the molybdenum determination have also been used. Some unusual methods for the determination of metals have been proposed by Weisz.1 RECENT DEVELOPMENTS- Several investigators notably Kirkbright and West and their co-workers have described several interesting methods based on the formation of heteropoly acids.Phosphorus has been determined by extraction as the hetero-molybdic acid and the molybdenum determined spectrophotometrically.5~6 In alternative methods the molybdenum is determined titri- metrically7 and (also silicon) by atomic-absorption spectroscopy.8 ,4 double-amplification method has been described in which the molybdenum is converted into the 8-hydroxyquino- linate then determined with b r ~ m a t e . ~ Niobium,lo titaniumll and thoriumf2 have been determined by extracting the particular metal hetero-molybdic acid and determining the latter by atomic-absorption spectroscopy.Arsenic can be determined in a similar way followed by spectrophotometric determination of molybdenum by to1uene-3,4-dithiol.l3 The method is ten times more sensitive than the molybdenum-blue method. Selenium has been determined by formation of its complexes with 3,3’-diaminobenzidine.14 The complexes are separated at different acidities. Cobalt can be determined by formation of [Co(N02) J3- followed by precipitation with [Co(NH,) J3+ ; the precipitate is reconverted into Co2+ and recycled through the process.15 The same investigators determined trace iodide by using periodate oxidation and complexing the unreacted periodate with molybdenum(V1). A 24-fold amplification is obtained (K. Belcher J. Haniya and A. Townshend unpublished work). Fluoride in the range 0.4 to 8 mg has been determined by an exchange reaction with calcium iodate.16 The mean recovery is 99.69 per cent.1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15. 16. REFERESCES Belcher K. Talanta 1965 15 357. Roberts G. A. Ibid. 1968 15 277. Unterzaucher J. Ber. dt. chetiz. Ges. 1940 73B 391. Kirsten W. J. Microchevn. J . 1960 4 501. Luech C. H. and Boltz D. F. -4nalyt. Chenz. 1958 30 103. Djurkin V. Kirkbright G. F. and West T. S. Analyst 1966 91 66. Kirkbright G. F. Smith A. M. and West T. S. Ibid. 1968 93 224. -- Ibid. 1967 92 411. Belcher R’. and Uden P. C. Analytica Chirn. Acta 1968 42 180. Kirkbright G. F. Smith A. M. and West T. S. Analyst 1968 93 292. Kirkbright G. F. Smith A. M. West T. S. and Wood R. Ibid. 1969 94 754. Kirkbright G. F. Rao ,4. P. and West T. S. Analyt. Lett. 1969 2 69. Watson C. A. Proc. Soc. Analyt. Chern. 1969 6 185. Cheng I<. L. Analyt. Lett. 1968 1 447. Belcher Ti. Hamya J. and Townshend .$wad W. I. Hassan S. S. M. and Elsayes M. B. Mikrochiin. Acts 1969 688. Analytica Chinz. Actn 1969 47 149.

ISSN:0037-9697    

DOI:10.1039/SA9700700061

出版商:RSC    

年代:1970

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March 19701 SPECIAL TECHNIQUES I N ANALYTICAL CHEMISTRY 63 Special Techniques in Analytical Chemistry The following is a summary of the Address given by the retiring Chairman after the Annual General Meeting of the Special Techniques Group held on November 18th 1969 and reported in the February 1970 issue of Proceedings (p. 24). Some Analytical Problems in Egg Research BY T. L. PARKISSOX (Flour Milling and Baking Research Association Cliorleya~ood Rickmansworth Herts.) INYESTIGATION of the effect of heat pasteurisation on liquid whole egg required the develop- ment of a method of fractionating the very complex mixture of proteins in liquid whole egg. A combination of dialysis centrifuging at high speed and then fractionating the soluble and insoluble portions separately by chromatography on diethylaminoethylcellulose was found to be a suitable procedure for revealing differences between raw and pasteurised whole egg and it was used to study the influence of staling and freezing in addition to the effects of time and temperature of pasteurisation.lV2 There was some evidence that association of some of the white and yolk proteins occurred when these components were mixed together in whole egg.Examination of the fractions by electrophoresis in starch and polvacrylamide gels and on cellulose acetate strips demonstrated that most of them contained a number of different proteins and efforts have been made to effect further resolution of the components of two particular fractions of the soluble proteins it having been found that these fractions were consistently quantitatively reduced as a result of pasteurisation.Some success has been achieved by dialysing them against acetate buffer and then sub-fractionating on carboxy- metliylcellulose. Zone electrophoresis showed that a particular protein band in one of the sub-fractions derived from raw egg was absent in the corresponding sub-fraction derived from pasteurised egg. This band had the same mobility as one of the ovalbumins but it has not been definitely identified. Fractionation on diethylaminoethylcellulose was less satisfactory for the insoluble proteins than for the soluble proteins as buffer solution of considerably higher ionic strength was needed to dissolve them. Consequently a large (“inert”) fraction of these proteins was not adsorbed on the column and was eluted immediately after the void volume of effluent had passed througli.Examination of these “inert” fractions by gel filtration on Sepharose 4B revealed that those derived from pasteurised whole egg contained a much greater proportion of high molecular weight compound than those derived from raw Zgg. Some of this material was isolated and shown to be a lipoprotein containing about r 0 per cent. of lipid and 30 per cent. of protein; the lipid portion is a complex mixture of several different groups and the protein moiety is an extremely insoluble material with an amino-acid composition that does not exactly match that of any egg protein reported in the literature but is closest to that of vitellenin. Another interesting finding in the gel-filtration experiments was that freezing and subsequent thawing of liquid whole egg resulted in the insoluble proteins containing a very much greater proportion of high molecular weight lipoprotein than had been found even in pasteurised unfrozen egg.Concentrations of thiol and disulphide groups have been determined in the soluble protein portions of raw and pasteurised liquid egg by allowing them to react with a known excess of methylmercury(II) iodide and measuring the unreacted excess by a polarographic method. With the object of making a similar study of the effect of pasteurisation on the lipid components of whole egg a published method for separating egg lipids into different classes by column chromatography on silicic acid is being evaluated. However examination of the different fractions by thin-layer chromatography has shown that some of them contain more than one class of lipid and consequently modification of the method is under investigation. The work described was supported by a grant from the British Egg Marketing Board. REFERENCES 1. -. -) Parkinson T. L.. J . Sci. Fd Agric. 1967 18 205. __ Ibid. 196S 19 552 and 590.

ISSN:0037-9697    

DOI:10.1039/SA9700700063

出版商:RSC    

年代:1970

数据来源: RSC

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THERMAL AXALYSIS [Proc. SOC. Analyt. Chem. Thermal Analysis The following is a summary of the Address given by the retiring Chairman after the Annual General Meeting of the Thermal Analysis Group held on November 13th 1969 and reported in the February 1970 issue of Proceecliizgs (p. 25). Trends in Therinal Aiialysis BY J. P. REDFERN (Stanton Redcvoft Ltd. Coppev ,Ifill Lane London S . U’. 17) IN trying to assess the significant trends which there are likely to be in the coming decade it is advantageous first to look back. The position prior to 10 years ago was that thermal analysis was still essentially a specialist activity for a small but growing number of labora- tories. Certain well known schools both in thermogravimetry and in differential thermal analysis were firmly established in different parts of the world.Much of the equipment in use at that time was custom-built by the user and there were comparatively few manu- facturers of equipment and what was available was predominantly the thermobalance. Work had commenced on a simultaneous differential thermal analysis - thermogravimetric unit in Hungary in the early 195Os.l There were very few books in English on thermal analysis available that dealt in the main with specific aspects of the s ~ b j e c t . ~ ~ ~ The period 1960 to date may be labelled as the period of growth for thermal analysis. There has been a tremendous growth in the number of papers published on the subject and contained within this growth is the trend towards papers covering applications and theory and away from those covering aspects of instrumentation.The users now except in cases in which specialised applications are envisaged tend to purchase equipment from instrument manufacturers of whom there are now many. Nationally several thermal analysis groups have been set up and in 1965 an International Confederation for Thermal Analysis was inaugurated. The first conference was held in Aberdeen in that year and was attended by some 300 delegates from 30 different countries. The International Confederation established three specialist committees namely Nomenclature Standardisation and Publications each of which has been very active in the last 5 years. What will be the significant trends of the next 10 years? I t is unlikely that the period will see the same growth and it can probably be regarded as a period of consolidation.The last 10 years have thrown up several problems that need attention. (i) There is only just beginning to be a worthwhile and authoritative literature on the subject and there is a need for more literature of an introductory nature and covering certain applications in depth written by acknowledged experts in the field. (ii) Although some progress has been made in the introduction of instruction on thermal analysis in undergraduate courses there is considerably more that can be done in this direction. The Thermal Analysis Group of the S.A.C. ran a successful school in 1968 and a further one is planned for 1970. This school is intended for those working in industry to give an intro- duction to the subject. This need to educate scientists is further apparent by the slant adopted in advertising by certain manufacturers who feel it necessary not only to outline the equipment they have on offer but also to indicate the sort of information likely to be obtained from thermal analysis.It is likely that the next 10 years will see considerable progress in the use of thermo- analytical techniques in pilot plant on-line control and so on. In equipment the significant trends are likely to be towards miniaturisation and towards increasing ease of usage. The use of small samples high reproducibility of results and accurate control of atmosphere will be taken as a necessity. Other factors likely to emerge will be the increased use of low temperature differential thermal analysis and the development of linked techniques such as mass spectrometry - differential thermal analysis and thermogravinietry - differential thermal analysis. REFERENCES 1. Hungarian Patent 145,369 1955. 2. 3. Duval C . “Inorganic Thermogravimetric :‘inalysis,” Elsevier Publishing Co. Amsterdam London Mackenzie R. C. Editov “The Differential Thermal Investigation of Clays,” Mineralogical Society and New York 1963. London 1957.

ISSN:0037-9697    

DOI:10.1039/SA9700700064

出版商:RSC    

年代:1970

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March 19701 EVOLVED GAS ANALYSIS AND DETECTIOK 65 Evolved Gas Analysis and Detection The following are summaries of some of the papers presented at an Ordinary Meeting of the Thermal Analysis Group held on November 13th 1969 and reported in the February 1070 issue of Proceedings (p. 25). Studies of Polymer Stability and Decomposition Products by Thermal Volatilisation Analysis BY I. C. MCNEILL (Chemistry Defiartment University of Glasgow Glasgow) THERMAL volatilisation analysis was developed primarily as a tool for the investigation of polymer breakdown mechanisms and for polymer characterisation but the method is also suitable for a study of other substances that give volatile products on heating provided the sample does not sublime under vacuum. The sample is heated in a linear-temperature programmed oven (or isothermally) and evolved volatile products pass from the reaction tube through a vacuum system with a cold trap at -196" C some distance from the sample.An open system is used with continuous pumping. The volatilisation is followed by measuring and recording the small pressure in the vacuum system between the heated sample and the cold trap with a Pirani gauge the output of which is fed to a recorder. X single-line thermal volatilisation analysis system1 is useful in comparing stabilities of different materials or studying the effect of some form of treatment on the stability of a sample. Examples given were comparisons of mixtures of polymers with copolymers of the same over-all composition that give different thermal volatilisation analysis curves and the effect on poly(methy1 methacrylate) of ultraviolet irradiation.Considerable information is obtained in addition about the volatile products by thermal volatilisation analysis if an additional cold trap at a temperature between 0" and -100" C is inserted in the line before the Pirani gauge. The response then depends on whether or not the volatile product condenses in the initial trap. I t is convenient to have four such lines in parallel and to record four Pirani outputs simultaneously. Comparisons of these outputs can be very informative.2 Some examples were discussed. The involatile residue of polymer degradation may be of interest for example because of colour development but is often intractable because of insolubility. It may however conveniently be studied by thermal volatilisation analysis if the sample is initially cast as a film on the flat base of a silica thermal volatilisation analysis sample tube.The latter can then be inserted directly into the beam of an ultraviolet spectrometer before and after degradation without removal of the ample.^ REFEREKCES 1. 2. 3. McNeill I. C . Eur. Polym. J. 1967 3 409. ___ Ibid. in the press. Gardner D. L. and McNeill I. C. J . Thevrnnl Analysis in the press. Evolved Gas Analysis of Hydrogen and Other Vapour Species from Hydrous Silicates BY K. J. I). MACKENZIE (Ceramics Department The U+ziversity ShefJield) A MASS-SPECTROMETRIC technique has been developed for the analysis of high temperature gaseous reaction products of solids. The method is applicable to the study of mineral trans- formations in uacuo up to 1100" C and unlike the method of Freund and Gentsch,l is unaffected bv gettering phenomena on hot-metal filaments.66 EVOLVED GAS AS,4L\-SIS AND DETECTIOS [ Y V O C . SOC. Analyt. CheJlt. By this means studies have been made of the gaseous reaction products of hydrous minerals such as kandites and amphiboles. Molecular hydrogen has been confirmed as a decomposition product of amosite crocidolite micas and natural kaolinites but not synthetic kaolinite. A redox mechanism is proposed for hydrogen evolution and is supported by work on synthetic kaolinite. ,4t higher temperatures other gaseous species are evolved from kaolinite including oxygen and SiO. Deposition of silicon in the reaction tube has been confirmed by the electron microprobe. The thermodynamic implications of these results were briefly discussed.REFERENCE 1 . Freund F. and Gentsch H. Bey. dt. keram. Ges. 1967 44 51. An Introduction to the Use of Mass Spectrometry with Gas - Liquid Chromatography and Differential Thermal Analysis Systems BY J. R. CHAPMAN ( A . E.I. Scientific Apparatus Limited BavtoI.8 Dock Road Urmston ,Waizclcestev -1131 2LD) THE mass spectrometer provides a uniquely versatile and sensitive detector for ancillary techniques such as gas - liquid chromatography and differential thermal analysis. With these techniques it is usually necessary to provide some form of interfacing to remove carrier gas preferentially before the effluent enters the mass spectrometer. This is commonly accoiii- plished with a Llewellyn type of separator in wliich the effluent passes into the source through a membrane permeable to organics but impermeable to helium or nitrogen or with a Biemann separator in which the helium is preferentially removed by pumping it through afine glass frit.-Ilternatively some form of capillary link can be used. For example with a differentia1 thermal analysis carried out at pressures up to a few torr a direct capillary link is possible. If the pressure is increased because of the use of a carrier gas either a separator or a capillary link with a by-pass to a rotary pump is used although the latter is not an efficient method of sample transfer. The mass spectrometer can be used as a detector in three modes. By tuning in to an m / e value characteristic of a compound e.g. m / e 18 for water that compound can be monitored selectively with great sensitivity.Thus the trace at m / e 18 obtained from CuS0,.5H20 is almost exactly coincident with the differential thermal analysis trace. By means of peak switching techniques more than one peak can be monitored to extend the range of the method. A non-selective forin of detection is provided by tile total ion current monitor a plate which collects a fraction of the total ion beam before mass separation. This monitor provides a trace equivalent to that provided by a normal gas - liquid chromatographic detector. Most information can be provided by scanning the mass Spectrometer when peaks are sliown by the differential thermal analysis system or by the total ion current monitor. In this way it is possible to distinguish chemical from phase changes and to analyse the materials evolved.Examples presented by using a siniple mass spectroinetric - differential thermal analysis system include the pyrolysis of poly(viny1 alcohol) polystyrene and a monosulphide polymer. The Use of Partial-pressure Mass Spectrometry in the Thernial Analysis Study of Carbons and Graphite BY J. DOLLIMORE c. 31. FREEDMAN AND n. H. HARRISON (Department of Pure and Applied Pliysics University of Salford Salfovd 5 Lancashire) A VERS.4TILE partial-pressure mass-spectrometer system is described for measuring theriiially desorbed species from solid surfaces. The system evaluates not only the ratio of masses quantitatively present in the gaseous phase but also relates the specific mass (mg per gram of solid) desorbed or decomposed during thermal treatment. The extension of the method to oxidation studies is also described. March 19701 PAPERS -4CCEPTED FOR PUBLICATIOX 67 A study has been made of the initial evolution of gases from graphitic and non-graphitic carbons. These range in properties from a ground graphite of specific surface 103 m2 g-l to a nuclear-type graphite of 0.6 m2 g-l. ,4 study of a non-graphitic carbon Saran Charcoal of molecular sieve type is also included. The formation of surface oxide on a clean surface at pressures of about 0.2 mn of mercury is evaluated together with the resultant thermal decomposition of the surface oxide. The results from this paper together with other published work on graphites is reviewed and used to illustrate the application of the tliernial desorption results to oxidation studies on carbons and graphites.

ISSN:0037-9697    

DOI:10.1039/SA9700700065

出版商:RSC    

年代:1970

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March 19701 PAPERS -4CCEPTED FOR PUBLICATIOX Papers Accepted for Publication in The Analyst THE following papers have been accepted for publication in The ,4?znZyst and are espected to appear in the near future. “A Transistorised Radiofrequency Polarograph Its Use for the Determination of Tin “Some Further Analytical Applications of Perxenate,” by R. 1%’. Bane. ‘‘A Scheme of Qualitative Analysis for Twenty Common Cations,” by A. K. Ghose “Electronic Modulation of Electrodeless Discharge Tubes for Use in Atomic Spectro- “The Volumetric Determination of Alumina in Ceramic Materials with DCTA in Place “-4 Simple Colorimetric Method for the Determination of Iron in Serum,” by 1;. K. “Gas-chromatographic Determination of Clilorcholine Chloride Residues in Vegetable and Lead,” by M. Harrison C. L. Roughton and B. Surfleet. and A. K. Dey. scopy,” by P. C. Wildy and K. C. Thompson. of EDTA,” by H. Bennett and R. A. Reed. Guirgis and Y. A. Habib. Foods,” by I? Tafuri M. Businelli and P. L. Giusquiani. 68 PUBLICATIONS RECEIVED [Proc. SOC. Analyt. Chena. “The Determination of Aliphatic Ketones by Polarography of their Girard-T Hydrazone Derivatives,” by M. D. Booth and B. Fleet. “Rapid Determination of Small Amounts of Sulphate in Cellulose Nitrate by a Water- digestion Procedure,” by A. F. Dawoud and A. A. Gadalla. “Studies on the Analytical Chemistry of Hafnium and Zirconium. Part 1. A Review of Methods for the Determination of Hafnium and Zirconium in Admixture,” by A. Brookes and A. Townshend. “Flame-photometric Determination of Bromine in Urine,” by B. Gutsche and R. Herr- mann.

ISSN:0037-9697    

DOI:10.1039/SA970070067b

出版商:RSC    

年代:1970

数据来源: RSC