ISSN:0003-2654    

DOI:10.1039/AN95681FX025

出版商:RSC    

年代:1956

数据来源: RSC

ISSN:0003-2654    

DOI:10.1039/AN95681BX027

出版商:RSC    

年代:1956

数据来源: RSC

ISSN:0003-2654    

DOI:10.1039/AN95681FP053

出版商:RSC    

年代:1956

数据来源: RSC

ISSN:0003-2654    

DOI:10.1039/AN95681BP061

出版商:RSC    

年代:1956

数据来源: RSC

摘要:

MAY, 1956 THE ANALYST Vol. 81, No. 962 PROCEEDINGS OF THE SOCIETY FOR ANALYTICAL CHEMISTRY ANNUAL GENERAL MEETING THE eighty-second Annual General Meeting of the Society was held at 4.30 p.m. on Wednesday, February 29th, 1956, in the Meeting Room of the Royal Society, Burlington House, London, W.l. The Chair was occupied by the President, Dr. K. A. Williams, A.Inst.P., M.Inst.Pet., F.R.I.C. The financial statement for 1955 was presented by the Honorary Treasurer and approved, and the Auditors for 1956 were appointed. The Report of the Council for the year ending February, 1956 (see pp. 252-260), was presented by the Honorary Secretary and adopted. The Scrutineers, Messrs. P. S. Hall and R. E. Weston, reported that the following had been elected officers for the coming year- and had President-K.A. Williams, B.Sc:, Ph.D. , A.1nst.P. , M.Inst.Pet., F.R.I.C. Past Presidents serving on the Council-Lewis Eynon, D. W. Kent-Jones, J. R. Nicholls George Taylor. Vice-Presidents-D. C. Garratt, J. Haslam and H. M. N. H. Irving. Honorary Treasurer- J. H. Hamence. Honorary Secretary-N. L. Allport. Honorary Assistarct Secretary-R. E. Stuckey. Other Members of CozcnciG-The Scrutineers further reported that 458 valid ballot papers been received and that votes had been cast in the election of Ordinarv Members of Council as follows-R. C. Chirnside, 342; A. A. Smales, 314; D. D. Moir, 283; F.JC. J. Poulton, 275; S. G. Burgess, 266; A. F. Williams, 264; W. H. Stephenson, 256; W. H. C. Shaw, 192; A. L. Williams, 161. The President declared the following to have been elected Ordinary Members of Council for the ensuing two years-S. G.Burgess, R. C. Chirnside, D. D. Moir, F. C. J. Poulton, A. A. Smales and A. F. Williams. C. H. R. Gentry, W. C. Johnson, T. McLachlan, R. F. Milton, Miss M. Olliver and S. A. Price, having been elected members of the Council in 1955, will, by the Society’s Articles of Association, remain Ordinary Members of the Council for 1956. J. R. Walmsley (Chairman of the North of England Section), F. J. Elliott (Chairman of the Scottish Section), P. J. C. Haywood (Chairman of the Western Section), J. R. Leech (Chairman of the Midlands Section), G. F. Hodsman (Chairman of the Microchemistry Group), J. E. Page (Chairman of the Physical Methods Group) and K. L. Smith (Chairman of the Biological Methods Group) will be ex-oficio members of the Council for 1956.After the business outlined above had been completed, the meeting was opened to visitors, and Sir William Slater, K.B.E., D.Sc., F.R.I.C., delivered the Bernard Dyer Memorial Lecture (see pp. 276-283). At the close of the meeting the President presented Sir William with the Bernard Dyer Memorial Medal. ORDINARY MEETING AN Ordinary Meeting of the Society was held at 7 p.m. on Wednesday, May 2nd, 1956, in the meeting room of the Chemical Society, Burlington House, London, W.l. The Chair was taken by the President, Dr. K. A. Williams, A.Inst.P., M.Inst.Pet., F.R.I.C. The following paper was presented and discussed : “The Composition of Some Deposits and Muds in Estuaries, Rivers and Lakes,” by J.H. Hamence, M.Sc., Ph.D., F.R.I.C. 249250 PROCEEDINGS NEW MEMBERS [Vol. 81 ORDINARY MEMBERS Philip Arthur Andrews, B.Sc. (Dunelm.) ; Lloyd Edward Radcliffe Branch, B.Sc., B.Com. (Lond.) ; Leonard Joseph Hamilton, B.Sc. (Lond.), F.R.I.C. ; Stanley Hargreaves, B.Sc. (Lond.), A.R.I.C. ; Eric Leslie Heywood, B.Sc. (Lond.) ; Ian Johnston, A.R.I.C. ; Rowan Stanley Large; Robert Paterson McLintock, BSc. (Edin.), A.R.I.C. ; Howard Alfred Nicholls, A.R.I.C. ; Eric Barton Smith, B.Sc. (Nottingham) ; Francis Joseph Spillane; Ronald George Taylor, B.Sc. (Lond.), A.R.C.S. ; Stanley Williams, A.R.I.C. JUNIOR MEMBERS John Esam Fairbrother; Dorothy Adele Thomson, B.Sc. (Aberdeen) ; Ann Elizabeth Wardman. DEATHS WE record with regret the deaths of Philip Bilham George Herbert Butler.MIDLANDS SECTION AN Ordinary Meeting of the Section was held at 7 p.m. on Tuesday, March 27th, 1956, at the Gas Showrooms, Nottingham. The Chair was taken by the Chairman of the Section, Mr. J. R. Leech, J.P. The following papers were presented and discussed : “Pharmaceutical Aspects of the Analytical Chemistry of Mercury,” by G. J. W. Ferrey, B.Sc., F.R.I.C. (presented on his behalf by D. C. Garratt, B.Sc., Ph.D., F.R.I.C.) ; “The Microchemical Estimation of Mercury,” by R. F. Milton, B.Sc., Ph.D., F.R.I.C. (presented on his behalf by W. D. Duffield). MIDLANDS SECTION AND BIOLOGICAL METHODS GROUP A JOINT Meeting of the Midlands Section and the Biological Methods Group was held at 7 p.m. on Wednesday, April l l t h , 1956, at the University, Edmund Street, Birmingham, 3.The Chair was taken by the Chairman of the Midlands Section, Mr. J. R. Leech, J.P. The subject of the meeting was “The Fundamental Bases of Microbiological Assay” and the following papers were presented : “The Physiological and Biochemical Background of Microbiological Assay,” by R. H. Nimmo-Smith, M.A., D.Phil., M.B., Ch.B. (see summary below) ; “The Influence of Physical Factors on the Microbiological Assay of Antibiotics,” by J. W. Lightbown, M.Sc., Dip. Bact., F.P.S. (see summary below) ; “Practical Considera- tions of Microbiological Assay,” by K. A. Lees, F.P.S., D.B.A. (see summary below). THE PHYSIOLOGICAL AND BIOCHEMICAL BACKGROUND OF MICROBIOLOGICAL ASSAY DR. R. H. NIMMO-SMITH said that biosynthesis of new cell material involved the inter- mediation of a large number of essential metabolites-components of proteins, of nucleic acids, of coenzyme systems and so on.Micro-organisms varied in their ability to synthesise their own essential metabolites. A failure to synthesise any one was reflected by a failure to grow in a defined medium unless the metabolite was present in adequate concentration. Microbiological assay exploited this situation and was based upon a relationship between growth of the test-organism and concentration of added metabolites. For the proper conduct of assays some understanding of microbial growth-cycles and modification of their pattern by limiting concentrations of a single essential metabolite was necessary. THE INFLUENCE OF PHYSICAL FACTORS ON THE MICROBIOLOGICAL ASSAY OF ANTIBIOTICS MR.J. W. LIGHTBOWN said that, if the theory relating to the radial diffusion of a substance into nutrient agar was examined, deductions could be made that were helpful in designing and improving cup - plate assays of antibiotics and growth factors. A theoretical approach to this problem had been made by K. E. Cooper and D. Woodman (J. Path. Bact., 1946, 58, 75), but the formula obtained by these workers was based on linear diffusion and was not strictly applicable to radial diffusion. In fact, K. E. CooperMay, 19561 PROCEEDINGS 251 (Nature, 1955, 176, 510) found a better agreement between this theory and practice when using linear diffusion than was found with radial diffusion. A theoretical expression for radial diffusion was arrived at independently by J.Vesterdahl (Acta Path. Microbiol. Scund., 1947, 24, 273) and J. H. Humphrey and J. W. Lightbown ( J . Gen. Microbiol., 1952, 7, 129). This expressed the radius of the zone of inhibition, r, to be expected when a quantity, M , of antibiotic, with a diffusion constant D, was allowed to diffuse into agar of thickness h, which was seeded with a test organism whose sensitivity to the antibiotic was a. If the duration of the diffusion before the zone was fixed was t, then r2 = 9-21 Dt (log M - log 4~hDta). The validity of this expression had been shown experimentally by Humphrey and Lightbown, and certain deductions of importance in cup - plate assays could be made. The first of these was that the square of the diameter of the zone of inhibition was proportional to log concentration of antibiotic in the cup.This they had found to be so for the tetracyclines, viomycin and erythromycin, when assayed with Bacilhs pumilus, also for penioillin when assayed with either StaphyZococcus aurem or Sarcina Zuteu. However, when penicillin or streptomycin was assayed with Bacillus subtilis, a linear relationship with the zone diameter was observed. The difference between the two relationships would only be obvious if the dose intervals were large or if a very accurate assay was performed. I t followed from the theory that the sharpness of the zone edge would vary directly with the diameter of the inhibition zone and inversely with the duration of diffusion before the incubation of the assay plate. The slope of the dose - response curve was given by the expression- q - a , log p1 M2 = 9.21 Dt, M d, and d, being zone diameters given by concentrations and hf,, respectively. It was thus obvious that the slope was only affected by the diffusion constant of the antibiotic and the period allowed for diffusion and not by the thickness of the agar.It was independent of the sensitivity of the test organism but was affected by the rate of growth of this organism, which influenced t. In order to increase the sensitivity of an assay one could only reduce a or h, or increase t. Increase in t invariably produced hazy edges, and if F, was reduced too much, accuracy was lost owing to increased percentage variation in the thickness of the agar due to unevenness of the assay plates. The value for a could be decreased by choosing a more sensitive test organism and possibly by adding a sub-inhibitory concentration of the antibiotic being assayed to the assay agar.Finally, Mr. Lightbown demonstrated how the sensitivity of the test organism to an antibiotic might vary a t different depths in the agar. This happened with strepto- mycin, viomycin, erythromycin, neomycin and albomycin. The effect could be very marked under certain conditions and it was desirable, when assaying these antibiotics, to measure the zone diameter at the surface of the agar. PRACTICAL CONSIDERATIONS OF MICROBIOLOGICAL ASSAY MR. K. A. LEES said that the term microbiological assay implied an estimation of the comparative activity of a sample and defined reference standard against a chosen test organism.Only when absolutely pure substances, in the sense that impurities present were inactive, were being assayed in terms of one another was it justifiable to employ different methods in different laboratories. Mixed preparations implied the need for rigorous standardisation of test organism and other assay variables. Liquid - tube methods were more sensitive than plate methods, but were more subject to the influence of biological variation. Plate methods depended primarily on physical considerations and, because of the presence of both standard and unknown samples in the single biological-system unit, biological variation usually affected both standard and unknown equally. Plate methods were more amenable to statistical treatment and consequent day-to-day control. Each antibiotic raised individual problems, as for example with the antibiotic fumagillin.Fumagillin was not very active against bacteria or fungi, but was active against bacterial phage. Hence both phage and phage-sensitive252 ANNUAL REPORT OF THE COUNCIL, FEBRUARY, 1956 [Vol. 81 bacterium were inoculated into the assay agar and the fumagillin, by diffusion, inhibited the phage and, by permitting the bacterium to grow, revealed zones of growth against the clear background of phage-inhibited bacteria. ’ MICROCHEMISTRY GROUP THE fifth London Discussion Meeting of the Group was held on Wednesday, April l l t h , 1956, at 6.30 p.m., in “The Feathers,” Tudor Street, London, E.C.4. In the absence of the Chairman of the Group, the Chair was taken by the Honorary Secretary, Mr. D. W. Wilson, MSc., F.R.I.C. Mr. H. J. Cluley, MSc., F.R.I.C., and Mr. C. Whalley, BSc., F.R.I.C., introduced the subject of “Complexones in Microchemistry,” after which there was an informal discussion. PHYSICAL METHODS GROUP THE fifty-third Ordinary Meeting of the Group was held at 6.30 p.m., on Tuesday, April loth, 1956, in the large chemistry lecture threatre of the Imperial College of Science and Technology, South Kensington, London, S.W.7. The Chair was taken by the Chairman of the Group, Dr. J. E. Page, F.R.I.C. The subject of the meeting was “Plant Instrumentation” and the following papers were presented and discussed: “Progress in Plant Analytical Control Methods,” by B. W. Bradford, BSc., Ph.D., A.R.C.S., D.I.C., F.Inst.Pet. ; “The Sonic Gas Analyser,” by A. E. Martin, Ph.D., DSc.; “Automation in the Laboratory,” by D. A. Patient, BSc., A.1nst.P.

ISSN:0003-2654    

DOI:10.1039/AN9568100249

出版商:RSC    

年代:1956

数据来源: RSC

摘要:

252 ANNUAL REPORT OF THE COUNCIL, FEBRUARY, 1956 [Vol. 81 Annual Report of the Council : February, 1956 THE past year has seen the full operation of the Society in its widened activities following the important changes first initiated in 1953. All the scientific meetings of the Society have been well attended and valuable papers have been presented. The four Sections have each held several meetings and the three Groups many more meetings still, and as a result the activities of the Society have been country-wide. On November 29th, 1955, the Society organised a special meeting at the Beveridge Hall, University of London Senate House, at which Professor J. HeyrovskS;, D.Sc., Ph.D., Director of the Central Institute of Polarography, Prague, and an Honorary Member, gave a lecture entitled “The Development of Polarographic Analysis” to a large audience. A particularly successful meeting was held a t Ardeer, Ayrshire, on May 20th, 1955, when a Symposium on Gas Chromatography, arranged jointly by the Physical Methods and Microchemistry Groups with the Scottish Section, was held in the Ardeer Recreation Club.Both morning and evening meetings were well attended, and in the afternoon visitors enjoyed the generous hospitality of Imperial Chemical Industries and were conducted on a tour of the Stevenston Works and Research Laboratories, the I.C.I. providing transport and excellent meals for all. An event deserving of special mention was the first joint meeting of the Society with the Association of Public Analysts. This was held on December loth, 1955, in the Council Chamber of the City Hall, Cardiff, having been jointly organised by the Association and the Western Section of the Society.The meeting was honoured by a Civic Welcome given by the Deputy Lord Mayor and Deputy Lady Mayoress. The work of the newly reconstituted Analytical Methods Committee is now well under way. The appeal to Industry for funds, which was mentioned in the last Annual Report as having been launched, proved to be an outstanding success, the total contributions for 1955 amounting to ,c78794, with guarantees of further sums in the next two years and also a number of deeds of covenant for seven years, totalling altogether approximately L22,500. A Trust Fund has been formed and the Society is most fortunate in having Mr. Justice Lloyd- Jacob as an independent Trustee.The Analytical Methods Committee has met regularly during the year under the chairmanship of Dr. D. C. Garratt, acting in the capacity of a policy Committee for future work and as a steering Committee to the seven working Sub-Committees. In addition, the secretariat has assumed practically all of the secretarial and editing work of the Committee on Methods of Analysis of Trade Effluents, set up jointlyMay, 19561 ANNUAL REPORT OF THE COUNCIL, FEBRUARY, 1956 253 by the Society and the Association of British Chemical Manufacturers; three methods have already appeared in the January issue of The Analyst, three more are with the printers and some twenty to thirty methods are undergoing final editing to ensure a supply for publication for some months to come.Part of the Trust Fund has been set aside for a Research Student- ship, which has been awarded to Mr. T. T. A. Gorsuch, B.Sc., A.R.I.C., to undertake investi- gations on the determination of trace elements by radiochemical techniques. It is envisaged that Mr. Gorsuch will work at the Atomic Energy Research Establishment, Harwell, under the direction of Mr. A. A. Smales. A separate Report of the first years’ work of the Analytical Methods Committee is being distributed to all contributors to the Fund; a short summary is given later in this Report.* During the present year it is hoped that the Society’s headquarters and staff will be accommodated in a suite of offices on the top floor of 15-16 Belgrave Square, London, S.W.l.This is the outcome of an arrangement whereby the Society will be tenants of the Society of Chemical Industry on most advantageous terms. In addition, it is hoped that a large room will be available for holding Council and committee meetings. The roll of the Society now numbers 1842, an increase of 43 over the membership of a year ago. LONG MEMBERSHIP-The congratulations and good wishes of the Council are extended to E. H. Miller and G. W. Monier-Williams, who have completed 50 years of membership, and to N. T. Foley and C. H. Manley, who have completed 40 years. DEATHS-T~~ Council regrets to have to record the deaths of the following members- H. Ballantyne E. W. Deag J. McLaren F. H. Burstall T. F. Doyle A, More J. Clifford A. Green A. Tingle (Honorary Member) R.L. Collett 0. Jones T. S. Tweedie ORDINARY MEETINGs-six ordinary meetings of the Society were held during the year April, 1955, in London, organised by the Physical Methods Group, on End-point Detection By E. Bishop, B.Sc., By J. P. Dowdall, B.Sc., and the following papers were read and discussed- by Physical Methods : A.R.T.C., A.R.I.C. A.R.C.S., D.I.C., A.R.I.C., D. V. Sinkinson and H. Stretch, A.R.I.C. “The Location of the End-point in Titrimetric Procedures.” “End-point Determination by High-frequency Methods.” “Spectrophotometric Titrations.” “A Short Account of the Scope and Precision of Amperometric Titration.” By R. A. Chalmers, B.Sc., Ph.D. By J. Watt, B.Sc. May, 1955, in London: ‘ * The Detection and Determination of Traces of Polynuclear Hydrocarbons in Industrial Effluents and Sewage.The Examination of Some Gasworks Effluents.” By P. Wedgwood, M.Sc., M.Inst.Gas E., M.Inst.F., A.Inst.S.P., F.R.I.C., and R. L. Cooper, M.Sc., Ph.D., A.M.Inst .Gas E., A.R.I.C. “The Analysis of Mixtures of Phenols by Partition Chromatography and Ultra-violet Spectrophotometry.” ‘ The Determination of Traces of Benzene Hexachloride in Water and Sewage Effluents.’’ By W. Hancock, B.Sc., and E. Q. Laws, B.Sc., F.R.I.C. Part 111. By R. M. Pearson, A.R.I.C. October, 1955, in London: ‘ The Colorimetric Determination of Phosphorus in Steel and Copper-base Alloys.’’ By W. T. Elwell, F.R.I.C., and H. N. Wilson, F.R.I.C. “The Determination of Small Amounts of Carbon in Steel by Low-pressure Analysis.” By R. M. Cook, A.Met., B.Sc. (Eng.), and G.E. Speight, A.Met., B.Sc., F.R.I.C. ‘ The Determination of Small Amounts of Sulphate by Reduction to Hydrogen Sulphide, and Titration with Mercuric or Cadmium Salts with Dithizone as Indicator.” By E. E. Archer, B.Sc. * -\-ate by Editor-The full text of the Report of the Analytical Methods Committee is reproduced on p“. 261-275 of this issue.254 ANNUAL REPORT OF THE COUNCIL, FEBRUARY, 1956 [Vol. 81 November Znd, 1955, organised by the Biological Methods Group, on the Evaluation of By By By I(. C. Sellers, Anti-fungals : “Laboratory Evaluation of Drugs for Clinical Trial Against Dermatomycoses.” H. 0. J. Collier, B.A., Ph.D., M.I.Biol., and G. K. A. Smith, A.I.M.L.T. “Some Factors in the Planning of Fungitoxicity Experiments in the Laboratory.” R.J. W. Byrde, B.Sc., Ph.D., and G. M. Clarke, M.A., Dip.Stat. “Cattle Ringworm: Problems in the Evaluation of Treatment.” Ph.D., B.Sc., D.V.S.M., M.R.C.V.S. November 30th, 1955, organised by the Physical Methods Group: J a n u c q , 1956, organised by the Microchemistry Group : “Atomic Energy and the Analyst.” “Microchemical Methods in the Art Gallery and Museum.” By A. E. A. Werner, MA., “The Ring-oven Technique and its Application in Archaeology.” By H. Weisz, JOINT MEETING-AS mentioned above, the first Joint Meeting with the Association of Public Analysts was held in December, 1955, in Cardiff. Members of the Food Group of the Society of Chemical Industry were also invited to attend. The Chair was taken by the President of the Association of Public Analysts, Mr.T. McLachlan, D.C.M., A.C.G.F.C., F.R.I.C., and the following paper was presented and discussed: By H. J. Evans, BSc., F.R.I.C., W. Kwantes, M.A., M.B., B.Chir., Dip.Bact., D. C. Jenkins, B.Sc., M.Sc., F.R.I.C., and J. I. Phillips, F.R.I.C. Including the The following papers were By A. A. Smales, B.Sc., F.R.I.C. M.Sc., D.Phil., A.R.I.C. Dr. techn.Dip1.-Ing. “Sucrose Loss from Ice-cream on Storage.” NORTH OF ENGLAND sEcTIoN-The membership of the Section is 373. Summer Meeting at Blackpool, 6 meetings have been held. read and discussed- “The Importance of Analysis in Industry.” “Some Aspects of Forensic Chemistry.” “Margarine.” “Some Modern Tools of the Analytical Chemist.” F.R.I.C. “The Determination of Germanium by Analytical and Spectrographic Methods.” K. V.Aubrey, BSc., and G. R. Gregory. “Applications of Newer Techniques to the Analysis of Pharmaceutical Products.” D. C. Garratt, B.Sc., Ph.D., F.R.I.C. SCOTTISH SECTION-The membership of the Section remains unchanged at 103. Three ordinary meetings have been held, two in Edinburgh and one in Glasgow. In addition, Symposia were held on “Gas Chromatography” at Ardeer, in conjunction with the Physical Methods and Microchemistry Groups, and on “The Use of Radioactive Materials in Biological Assay” at Edinburgh, in conjunction with the Biological Methods and Physical Methods Groups and local sections of the Royal Institute of Chemistry, the Society of Chemical Industry and the Chemical Society. The 21st year of the Section’s activities culminated in the Annual General Meeting held at Glasgow on January 20th, 1956, attended by the President of the Society.The Section participated in the Ramsay Chemical Dinner organised by the Chemical Group of the Federation of Technical Societies in Glasgow. By J. Haslam, DSc., F.R.I.C. By G. B. Manning, B.Sc., M.B., Ch.B., F.R.I.C. By J. R. Nicholls, C.B.E., D.Sc., By By By W. L. Wren, B.Sc., F.R.I.C. The following papers were read and discussed- “The Determination of Small Amounts of Zinc in Various Materials.” By J. A. Hunter, B.Sc. “The Determination of Calcium and Magnesium in Plant Material Using Disodium Ethylenediaminetetra-acetate.” By Miss E. S. R. McCallum, B.Sc., and A. M. Smith, Ph.D. “The Chromatographic Separation and Determination of Alkaline-earth and Alkali Metals.” Edinburgh, April, 1955: By J.B. Headridge, B.Sc., and R. J. Magee, M.Sc., Ph.D.May, 19561 ANNUAL REPORT OF THE COUNCIL, FEBRUARY, 1956 255 Ardeer, May, 1955. Symposium on Gas Chromatography: “Gas - Liquid Chromatography.” “The Vapour-phase Chromatographic Analysis of Hydrocarbon Mixtures.” “Techniques Used in a Study of the Boron and Silicon Hydrides.” “Adsorption and Partition Methods.” By C. S. G. Phillips, M.A. “A Rapid Chromatographic Method for the Determination of Bromine-inert Impurities Discussion on Katharometers as Recorders in Gas Chromatography. Opened by Symposium on the Use of Radioactive Materials in Biological “The Determination of Radioactive Isotopes in Biological Samples.” By R. F. Glascock, “The Principles of Isotope-dilution Assays with Special Reference to Vitamin B12.” “Bio-assay of Radio-iodinated Plasma Proteins for Clinical Use.” By A.S. McFarlane, “Isotope-dilution Assay of Antibiotics in Fermentation Liquors with Particular Reference “The Assay of Aldosterone and Other Adrenal Steroids by the 24Na/42K Method.” By “Assay of T.S.H. Based on the Rate of Discharge of Radioactive Iodine from the “Labelled Metabolic Pools for Studying Quantitatively the Biochemistry of Toxic “The Use of 1311-labelled Serum Albumin in Determining the Inter-cellular Plasma By F. W. Jennings, B.Sc., M.Agr., I. M. Lauder, By A. J. P. Martin, Ph.D., F.R.S. By D. E. By A. B. Little- Chalkley, B.A., B.Sc. wood, B.A. in Ethylene.” Dr. Keulemans and A. F. Williams, B.Sc., F.R.I.C. By N. H. Ray, B.Sc., A.R.I.C. Edinburgh, July, 1955.Assay : B.Sc., Ph.D. By E. Lester Smith, DSc., F.R.I.C. M.A., B.Sc., M.B., Ch.B. to Benzylpenicillin and Griseofulvin.” R. N. Jones, B.A., Sylvia A. Simpson, B.Sc., and J. F. Tait, B.Sc., Ph.D. Thyroids of Chicks.” Action.’’ in Centrifuged Red Cells.” M. R. C .V. S., and W. Mulligan, M. Sc., Ph.D. By G. C. Ashton, B.Sc. By T. Kinnear, M.B.E., M.B., M.R.C.P., M.R.C.P.E. By F. P. W. Winteringham, F.R.I.C. “The Measurement of Health Hazards.” By J. F. Loutit, D.M., M.R.C.P. Glasgow, September, 1955, on the Determination of Traces of Lead: Introductory Talk. By N. L. Allport, F.R.I.C. “Lead in Biological Materials.” “The Determination of Lead by Square-wave Polarography.” By S. L. Tompsett, B.Sc., Ph.D., D.Sc., F.R.I.C. By D. J. Ferrett, M.A., D. Phil. Grangemouth, November, 1955 : “Some Industrial Applications of Ion-exchange Materials.” By T.R. E. Kressman, Ph.D., D.I.C., A.R.I.C. Edinburgh, December, 1955 : M.A., Ph.D., F.R.S.E. “Statistics for Chemists (Statistical Control in Chemical Analysis) .” ~’ESTERN SECTION-The membership of the Section is 88. Attendances at meetings have been satisfactory, having regard to the scattered area of the Section. As would be expected, the joint meetings with other Societies attract the largest attendances, and this enables some propaganda work to be done on the attractions of joining the Society. By B. Woolf, The following papers were presented and discussed- Bristol, January, 1955 : “Recent Advances in Bacteriological Examination of Water Supplies.” Taylor, M.A., M.D., D.P.H., M.R.C.S., L.R.C.P., Barrister-at-Law. By E. Windle Cardiff, February, 1955 : “Some Applications of Modern Techniques in Analytical Chemistry.” By J. R. Nicholls, C.B.E., D.Sc., F.R.I.C.256 ANNUAL REPORT OF THE COUNCIL, FEBRUARY, 1956 [Vol. 81 Gloucester, May, 1955 : “The Role of Iodine in Analytical Chemistry.” By Dr. K. Morgan. Bristol, October, 1955, held jointly with the Physical Methods Group, on X-ray Analysis: By Dorothy Crowfoot Hodgkin, By E. T. Hall, By E. R. Parkes, M.Sc., “The X-ray Analysis of the Structure of Vitamin BI2.” “X-ray Fluorescent Quantitative Analysis as a Tool in Archaeology.” “X-ray Diffraction Techniques in the Investigation of Crime.” B.Sc., M.A., Ph.D., F.R.S. M.A., D.Phi1. F.R.I.C. Bristol, January, 1956 : “Industrial Application of Sequestering Agents.” By R.L. Smith, B.Sc., Ph.D., A.R.I.C., and P. Womersley. MIDLANDS SECTION-The membership of the Section is 282. Meetings have been held in Birmingham and Nottingham. A special joint meeting with the Birmingham and Midlands Section of the Royal Institute of Chemistry was held on November 23rd, 1955, at which Professor J. HeyrovskS;, D.Sc., Ph.D., gave a lecture on “Modern Trends of Polarographic Analysis.’’ The following papers were read and discussed- “The Analytical Chemistry of Textiles.” “The Analytical Chemistry of Niobium and Tantalum, with Particular Reference to “4-Amino-4’-chlorodiphenyl as a Reagent for the Determination of Sulphate.” By “The Determination of Sulphur in Coals after Combustion in the Calorimetric Bomb.” “A Semi-micro Method for the Determination of Sulphur in Rubber.” By B.B. “The Determination of Sub-micro Quantities of Sulphate.” By A. S. Jones, B.Sc., “The Use of the Mass Spectrometer in Analysis.” By J. C. Robb, B.Sc., Ph.D., A.R.I.C. “Microwave Spectroscopy.” “The Analysts’ Dilemma: Colour or Stability.” By R. J. P. Williams, M.A., D.Phil., “Ring-oven Technique.” By H. Weisz, Dr.techn.Dip1.-Ing. Discussion on “Spectrophotometric Titrations” opened by R. A. Chalmers, BSc., Ph.D., “Some Physical Methods for the Analysis of Phosphorus Compounds.” By Dr. D. E. C. “Recent Advances in Inorganic Analysis.” B y R. Relcher, Ph.D., F.Inst.F., F.R.I.C. “Gas Chromatography.” By J. C. Tatlow, Ph.D., D.Sc., A.R.I.C. “Ionophoresis.” “Ultra-micro Methods for the Analysis of Organic Compounds.” By T.S. West, B.Sc., By A. G. Hamlin, B.Sc., F.R.I.C. Steel and Allied Materials.” A. J. Nutten, B.Sc., Ph.D., F.R.I.C. By H. C. Wilkinson, M.Sc., A.M.Inst.F., A.R.I.C. Bauminger, Ph.D., A.R.I.C. Ph.D., and D. S. Letham, MSc. By B. Bagshawe, A.Met. By . J. Sheridan, M.A., D.Phi1. A.R.I.C. and S. J. Clark, B.Sc., Ph.D., A.R.I.C. Corbridge. By A. B. Foster, B.Sc., Ph.D. Ph.D., A.R.I.C. MICROCHEMISTRY GRouP--Eighty-seven members have joined the Group during thc year Three meetings were held during the year, in Ardeer, London: The Annual General Meeting was held in London in January, 1956, and was Ardeer : Symposium on “Gas Chromatography” jointly with the Scottish Section and The papers presented at this meeting are detailed i n the Southampton: A joint meeting with the Mid-Southern Counties Section of the Royal and the membership is now 529.Southampton and London. followed by a meeting of the Society organised b y the Group, as reported above. the Physical Methods Group. report on the activities of the Scottish Section.May, 19561 ANNUAL REPORT OF THE COUNCIL, FEBRUARY, 1956 257 Institute of Chemistry on “Trace Elements in Archaeology and Agriculture.” The following papers were read and discussed- “Trace Elements in Archaeology.” By C. F. M. Fryd, B.Sc., A.R.C.S. “Methods for Determining the Trace-element Status of Plants.” By E. J. Hewitt, “The Estimation of Trace Elements in Plant Material and Soils by Means of Aspergilhs By D. J. D. Nicholas, B.Sc., Ph.D., A.K.C., F.R.I.C. In addition to the above, the activities of the Group have been augmented by the holding The following topics were introduced by B.Sc., Ph.D., A.K.C.niger.” of three informal discussion meetings in London. experts and discussed by the members present- “The Direct Determination of Oxygen in Organic Substances.” “The Micro-determination of Molecular Weight. ’’ “The Determination of Carbon and Hydrogen.” Arising from the first meeting, a collaborative investigation into the methods of oxygen determination was initiated. This is continuing under the control of the Analytical Methods Commit tee. PHYSICAL METHODS GROUP-The membership of the Group is now 572, an increase of 84 since last year. Two Group meetings were held in London and one at Ardeer jointly with the Scottish Section and the Microchemistry Group.Another meeting was held jointly with the Western Section in Bristol. The Group also participated in the Edinburgh meeting held jointly with the Scottish Section, the Biological Methods Group and the local sections of the Royal Institute of Chemistry, the Society of Chemical Industry and the Chemical Society. After the Annual General Meeting on November 30th, 1954, a discussion took place on “Possibilities in the Establishment of Standard Samples for the Determination of Some Trace Elements.” The following papers were read and discussed at other ordinary meetings of the Group- Solvent Extraction-London, January, 1955 : “Solvent Extraction. By H. M. N. H. Irving, M.A., D.Phil., F.R.I.C., L.R.A.M. “Laboratory Apparatus for Solvent Extraction.” By I.Wells, B.Sc., D.I.C., A. M . I. Chem . E. “Fractionation of Crude Fumagillin by Distribution Methods.” By R. R. Goodall, B.Sc., Ph.D., and J. K. Landquist, B.Sc., Ph.D. “Solvent Extraction in the Analysis of Precious Metals.” By W. A. E. McBryde, M.A., Ph.D. Gas Chromatography-Ardeer, May, 1955, and Radioactive Materials-Edinburgh, July, Details of the papers read at these meetings are given under the Scottish Section report. Details of the papers read at this meeting are given under the Western Section report. Mr. R. A. C. Isbell, for six years the Honorary Secretary of the Group, retired at the Annual General Meeting and is succeeded by Mr. L. Brealey. BIOLOGICAL METHODS GROUP-During the year the membership of the Group increased by 19 and now stands at 268.The Summer Meeting of the Group took the form of a joint meeting with the Scottish Section and the Physical Methods Group on “The Use of Radioactive Materials in Biological Assay.” The meeting was held in the University of Edinburgh on July 11th and 12th, 1955, and was supported by the local sections of the Royal Institute of Chemistry, the Society of Chemical Industry and the Chemical Society. The papers presented at this meeting are detailed in the report on the activities of the Scottish Section. On December loth, 1954, an ordinary meeting of the Group was held, immediately after the Annual General Meeting for the year 1953-54. The following papers were read- “The Evaluation of Vegetable Purgatives.” By J. W. Fairbairn, B.Sc. , Ph.D., F.P.S., Introductory Survey.” 1955 : X-ray Analysis-Bristol, October, 1955 : F.L.S., A.R.1 C.258 ANNUAL REPORT OF THE COUNCIL, FEBRUARY, 1956 [Vol.81 “The Disc - Plate Method of Assay with Neurospora Mutants for Thiamine, Pyridoxin, By E. C. Barton-Wright, D.Sc., “Observations on the Biological Estimation of Vitamin E.” By T. Moore, D.Sc., Ph.D. A symposium meeting on “Biological and Microbiological Met hods of Estimating Introductory Address. “The Microbiological Estimation of Vitamin B,, in Serum.” By R. H. Girdwood, “The Estimation of Vitamin B,, in Animal Feeding Stuffs with Lactobacillus leichmannii By D. H. Shrimpton, B.A., “The Estimation of Vitamin B,, in Milk.’’ By Margaret E. Gregory, Ph.D., A.R.I.C. “Biological Methods of Estimating Vitamin B,,.” By Marie E. Coates, Ph.D., F.P.S.“A Critical Analysis of the Method of Vitamin-B,, Assay with Euglena gracilis as Test ANALYTICAL METHODS COMMITTEE-AS has already been recorded, the past year has shown considerable activity in spite of difficulties experienced during the first few months owing to inadequate office accommodation. The amount of work increased rapidly, particularly in connection with the methods of analysis of Trade Effluents; the secretariat moved to a larger office at 20 Eastcheap, London, E.C.3, at the end of August and the staff was increased to three, including a part-time graduate assistant. The activities of the A.B.C.M. - S.A.C. Committee on Analysis of Trade Effluents has already been mentioned in some detail. The report of the Vitamin-B,, Panel of the original Vitamin Sub-committee (now dis- banded) has now been completed.The Vitamin-E Panel is preparing a report on the chromatographic assay of cc-tocopherol and the experimental work on the differential analysis of total tocopherols is proceeding. The Essential Oil Sub-committee report on the Determination of Linalol has been completed. The work of this Sub-committee is under review and a programme is being prepared. A report by the Pesticides Residues in Foodstuffs Sub-committee on the Determination of Small Amounts of Total Organic Chlorine in Solvent Extracts of Vegetable Material has been completed. The future work of the Sub-committee is at present under consideration with a view to broadening its scope The Metallic Impurities in Organic Matter Sub-committee, under the Chairmanship of Mr.T. McLachlan, suceeds the old Metallic Impurities in Foodstuffs Sub-committee, the scope of its work having been broadened. Collab-orative investigation is in progress on the molybdenum-blue method for arsenic. The tentative method for lead, published in 1954, is under review. The Meat Products Sub-committee, under the Chairmanship of Dr. H. G. Rees, succeeds the old Meat Extracts Sub-committee, the scope of its work having been broadened. An investigation into nitrogen factors for all types of meat is in progress and methods for the determination of starch are being considered. Following a proposal by the Microchemistry Group for collaborative work on the Unterzaucher micro method for the direct determination of oxygen, a Sub-committee has been formed under the Chairmanship of Mr.D. W. Wilson. The results of the first collabora- tive experiment are now being collated. The work of the old Standard Methods Sub-committee, which was responsible for the preparation of the Bibliography of Standard Methods, has now been assumed by the A.M.C.; the first objective is the publication in a single volume of the methods recommended by the A.M.C. in their Reports since 1927. The methods on soap analysis and assay of scheduled poisons have now been edited according to an agreed format and two more groups-metallic impurities in foodstuffs, and vitamins-are in preparation. A Joint Committee with the Pharmaceutical Society is to be set up under the Chairman- ship of Dr. K. R. Capper to collect and publish methods of analysis of those drugs that are no longer official but are still in demand in industry.Choline, Inositol and p-Aminobenzoic Acid.” F.R.I.C., and N. J. Butler. Vitamin BI2” was held on May 13th, 1955. Five papers were read to a large audience- By F. A. Robinson, M.A., LL.B., F.R.I.C. M.D., Ph.D., F.R.C.P.E., M.R.C.P. and Ochromonas Ynalhamensis as Test Organisms.’’ Ph.D. Organism.” By W. R. Pitney, M.D., M.R.A.C.P.May, 19561 ANNUAL REPORT OF THE COUNCIL, FEBRUARY, 1956 259 LIAISON COMMITTEE-During the year the following appointments have been made- Mr. D. W. Wilson, Laboratory Furniture and Fittings. Mr. M. A. Fill, Microchemical Apparatus and Laboratory Ovens. Mr. G. Middleton, Pyridine. Dr. J. G. A. Griffiths was again appointed the Society’s representative.Dr. J. Haslam represented the Society at the Ninth Chemists’ Conference of the Methods B.S.I. Committees: Joint Library Committee, Chemical Society : British Iron and Steel Research Association : of Analysis Committee (Metallurgy, General Division). Parliamentary and Scientific Committee : Mr. G. Taylor continued to represent the Society. The Council of the Society thanks all its representatives for the work they havecarried out in the various Committees and at the various meetings during the year on behalf of the Society. HONORARY TREASURER’S REPORT-once again finance has given the Council much food for thought during the past year. In the first instance the Council decided to change the financial year, which, since the inception of the Society, has ended on December 31st.With the Society’s Annual General Meeting being held very early in March, this has left little time for the accounts to be audited and a balance sheet printed in time for the Annual General Meeting. With this in mind the Council decided, on the advice of the Finance Committee, that in future the financial year should end on October 31st. This new arrangement came into operation last year, so that the balance sheet for this year shows the accounts for 10 months only, but in all subsequent years the balance sheet will cover a full 12 months. For some years now the Society has relied on a grant from the Chemical Council to balance its publications accounts. Early in the year the question of increasing the price of The AvzaZyst and Analytical Abstracts to outside subscribers and of increasing the subscription to the Society was considered at a Joint Meeting of the Policy and Finance Committees.This Joint Committee was against increasing the membership subscription, but it recommended that the price of The Analyst and Analytical Abstracts be increased in 1957 to 5 guineas. The whole question of finance had to be reconsidered once again, however, towards the end of the year, owing t o a subsequent considerable increase in the cost of printing and also of a threat of further increases in the future. It has now been decided by Council that from January lst, 1957, the price of The Analyst and Analytical Abstracts to outside subscribers shall be increased to 6 guineas, and the price of copies of Analytical Abstracts that are sold separately correspondingly increased.The Council has also decided that it will be necessary to increase the subscription of members of the Society. This step has been taken with some reluctance, but it is realised that only by this means can the continued existence of the Society be ensured. In this connection two main points must be borne in mind. Firstly, the membership subscription includes the two journals, The Analyst and Analytical Abstracts, and, moreover, the cost of producing these journals steadily increases year by year. Secondly, the activities of the Society increase year by year. All new activities of the Groups and Sections are available to all members without additional subscription, and the efficient organisation of these activities has required additions to our headquarters staff.Apart from these factors, we must look to the future and now that our journals are subsidised by grants our only means of building up reserves for future special activities is by subscriptions. I t is with these facts in mind that the Council have come to the decision that as from 1957 the subscription shall be raised to 3 guineas per annum. THE ANALYST-The 1955 volume contained 912 pages, compared with 792 in 1954. The numbers of papers and notes published in 1955 were 103 and 49, respectively, against 100 and 48 in 1954. Of the papers, three were lectures delivered at Special Meetings of the Society and two were Review Papers. After allowing for all matter other than papers and notes and for these five special papers, the average length of a paper or a note is 5-05 pages.This is an increase of half a page over the corresponding figure for 1954 and suggests that260 AKNUAL REPORT OF THE COUNCIL, FEBRUARY, 1956 [Vol. 81 the style of writing could well be made more concise. Summaries of fifteen papers presented at meetings but not being published in full in any journal were printed in the Proceedings of the Society. Ten issues of the Bulletin were distributed with The Analyst during the year; two of these were special issues devoted entirely to material issued by the International Union of Pure and Applied Chemistry. The increase of 700 in the number printed of each issue, made at the beginning of 1955, has been amply justified by the continued expansion of the circulation; for 1956 the number has been raised to 6000. ANALYTICAL ABSTRACTS-The second volume was completed in December, 1955, and contained 3556 abstracts occupying 468 pages as compared with 3190 abstracts and 392 pages in 1954. The number of journals abstracted has steadily increased, and it is now unlikely that any important papers escape abstracting. Arrangements have been made with Dr. Bussieff to supply us with abstracts from Moscow and with Dr. Saito to do the same from Japan. The arrangement with the S.C.I. for exchange of abstracts continues to work satis- factorily. The addresses of authors are being included for an experimental period beginning in Januar?, 1956. CHEMICAL couNcIL-During the year the Chemical Council has again made grants to the Society for the publication of original papers and abstracts. The Council acknowledges with thanks the sums of ,El400 for The Analyst and of El200 for Analytical Abstracts. A new appeal now being made t o Industry by the Chemical Council will include funds not only for original publications and the Chemical Society Library, but also for abstracts. CONFERENCE OF HONORARY SECRETARIES-A meeting of the Honorary Secretaries of the Sections and Groups of the Society was held in May, 1955, on the same lines as that of the previous year. Again the meeting was highly successful. STAFF-Mr. B. J. Walby, B.Sc., A.R.I.C., resigned the posts of -4ssistant Editor of The Analyst and of Analytical ,4bstracts at the end of April, 1955. Mr. N. C. Francis was appointed Assistant Editor of The Analyst and Mrs. H. I. Fisk, B.Sc., Assistant Editor of Analytical A bstracts. K. A. WILLIAMS, President. N. L. ALLPORT, Honorary Secretary.

ISSN:0003-2654    

DOI:10.1039/AN9568100252

出版商:RSC    

年代:1956

数据来源: RSC

摘要:

May, 19561 REPORT OF THE ANALYTICAL METHODS COMMITTEE, 1955 261 Report of the Analytical Methods Committee 1955 IT is now a year since the Analytical Methods Committee of the Society for Analytical Chemistry was reorganised on a new basis to permit its work to be expanded and expedited. The Report that follows gives a brief history of the Committee and reviews the progress that has been made during the past year; it is intended to isstre similar progress reports annually. It will be appreciated that any reconstruction must necessarily take time but, nevertheless, substantial progress has been made. The constitution of the Analytical Methods Committee is as follows- CHAIRMAN: D. C. Garratt, B.Sc., Ph.D., F.R.I.C. (Boots Pure Drug Co. Ltd.) N. L. Allport, F.R.I.C. Analytical Consalting Chemist and Bac- teriologist; Honorary Secretary of the Society A.J. Amos, B.Sc., Ph.D., F.R.I.C. Analytical and Consulting Chemist R. Belcher, D.Sc., F.Inst.F., F.R.I.C. University of Birmingham (Department of Chemistry) R. C. Chirnside, F.R.I.C. Reseaych Laboratories of The General Elec- tric Co. Ltd. J. H. Hamence, M.Sc., Ph.D., F.R.I.C. Public Analyst, Oflcial Agricultural Analyst and Consulting Chemist; Hon. Treasurer of the Society Imperial Chemical Industries Ltd. (Plastics Divisiort) Analytical and Consulting Chemist Public Analyst Department of the Government Chemist J. Haslam, D.Sc., F.K.I.C. D. W. Kent- Jones, B.Sc., Ph.D., F.R.I.C. T. McLachlan, D.C.M., A.C.G.F.C., J. R. Nicholls, C.B.E., DSc., F.R.I.C. A. A. Smales, B.Sc., F.R.I.C. Atomic Ertergy Research Establishment, K.A. Williams, BSc., Ph.D., A.Inst.P., Analytical a d Consulting Chemist; M.I.Biol., F.R.I.C. Harwell President of the Society M.Inst.Pet., F.R.I.C. SECRETARY: Miss C. H. Tinker, B.Sc., Ph.D., A.R.I.C. GENERAL REVIEW HISTORY OF THE COMMITTEE- The Society through its Analytical Methods Committee has always been recognised as being an admirably suitable body for the collaborative work required for preparing and promulgating standard and reference methods of analysis. The first Committee was appointed by the Council of the Society in April, 1924, as The Standing Committee on Uniformity of Analytical Methods and continued under this rather lengthy title until April, 1935, when it was changed to the less cumbersome one under which it now operates. The work of the Committee, its Sub-committees and panels has always been, and still is, carried out voluntarily by members who have full-time duties in their own spheres of work.The fact that the Sub-Committees.and panels have managed to continue, even during the Second World War, carrying out collaborative work on a diversity of problems and publishing 50 Reports in all since 1927 is some indication of the importance they attach to the work in hand, and the Society owes them a very large debt of gratitude for the unstinting help that they give. In the past, the secretarial duties were undertaken by a member of each committee, and because such work had, of necessity, to be fitted into their own limited free time, it was only natural that progress was sometimes slow. Therefore, when the Society became262 REPORT OF THE ANALYTICAL METHODS COMMITTEE, 1955 [Vol.81 a purely learned body for the promotion of analytical chemistry as a whole, the Committee came under review ard emphasis was laid on the need for expediting the preparation and publication of standard methods. Some reports from existing Sub-committees were nearing completion, new projects were awaiting implementation and, in particular, the “Bibliography of. Standard Methods,” published in 1949, required expansion into a complete collection of methods-a formidable task in itself. APPEAL TO INDUSTRY- It was clear that this large programme of work required a great deal more time than existing facilities allowed, however willing the helpers. So, at the end of 1954, Dr. D.W. Kent- Jones, then President of the Society, launched an Appeal to Industry for subscriptions to a 1 , u r d devoted to the work of the Committee. It was proposed in the first place to establish a full-time paid Secretariat, the Secretary being reponsible both for the servicing of the Committee and all its technical Sub-committees and for the collection, editing and publication of the volume of Standard Methods to supplement the Bibliography. I t was also proposed, should the Fund permit, to award one or more Studentships or Scholarships for research on important analytical problems. Such was the very gratifying and prompt response to the Appeal that it was evident that these proposals to help the needs of the Society in this important aspect of its work were welcomed by industry.Donations were received from 79 subscribers, including com- mercial and nationalised industries and trade associations. Of these, eight entered into seven-year Deeds of Covenant, three others guaranteed annual amounts for seven years and a further twenty-six promised sums for three years in the first instance. Many of the other subscribers have indicated that they will continue their support in order that the Committee should have a reasonable annual income to carry on its work. In 1955, -@SO0 was received, and the Committee has firm promises of k5700 for each of the years 1956 and 1957. TRUST FUND- A Trust Fund, called the Society for Analytical Chemistry Analytical Methods Trust Fund, has now been established with the moneys received.Mr. Justice Lloyd-Jacob, who has been a very good friend to the Society for some years, has very kindly consented to be an independent Trustee. The other four Trustees represent the Society, being Dr. K. A. Williams (President), Dr. D. W. Kent- Jones (Past President), Dr. J. H. Hamence (Honorary Treasurer) and Mr. N. L. Allport (Honorary Secretary). Thus for the first time, the Analytical Methods Committee becomes a financially independent unit within the Society. ’The text of the Deed of Trust is reproduced as Appendix I to this report. APPOINTMENT OF THE NEW ANALYTICAL METHODS COMMITTEE : ITS FUNCTION AND POLICY- With such initial support, the Committee was able to start its work of expansion without delay. The original Committee was reorganised, the personnel of the new Committee being limited to 12 (including the Officers of the Society) and being selected to represent a fair cross-section of the field of analytical chemistry.Dr. D. C. Garratt, who had been Honorary Secretary of the Committee since 1946, was invited to be Chairman of the new Committee and Dr. C. H. Tinker was appointed as its first paid Secretary in February, 1955. The first meeting of the Committee was held on February Znd, 1955, to discuss its future functions and policy, which would be wider in scope than in the past, since authority had been given by Council for the Committee to exercise greater powers than before and to be responsible for its own complete administration as well as acting as a steering committee for the technkal work of the Sub-committees and panels.In its capacity as a steering committee, it examines critically new projects, particularly to assess their value in the general field of analytical chemistry, and, on approving them, appoints Sub-Committees to investigate the best methods of analysis, since such methods are intended for reference purposes. It should be noted that the techniques recommended may involve the use of the most up-to-date equipment, which might not yet be available in every laboratory. All methods that are recommended will always be open to revision according to current requirements and research. It was agreed that Sub-committees should not be permanent but should be disbanded when the projects covered by their terms of reference have been completed.May, 19561 REPORT OF THE ANALYTICAL METHODS COMMITTEE, 1955 263 PROGRESS OF WORK- It will be evident from the detailed reports of individual committees that substantial progress has been achieved during the year.Secretariat-As was to be expected, the progress during the first few months was some- - what slow. Not only had the work of the existing Sub-committees to be reviewed with adjustments in their constitutions, where necessary, to permit the scope of their work to be broadened to bring it into line with the present needs, but also the Secretariat had to be organised ab initio to meet the requirements of the work. The Secretariat started modestly, consisting only of the Secretary; however, with the rapid increase in the volume of work during the year, more spacious accommodation was acquired and the personnel has now risen to three, a graduate having recently been engaged.Analytical Methods Committee and its Sub-Committees-In all, 30 meetings of the Com- mittee and its Sub-Committees and panels have been held during the year, of which 10 have been meetings of the Committee itself. At present there are seven active Sub-Committees under the aegis of the Committee. These deal with the following subjects- Meat Products Metallic Impurities in Organic Matter Essential Oils Pesticides Residues in Foodstuffs Trace Elements in Fertilisers and Feeding Stuffs Vitamins Direct Micro-determination of Oxygen in Organic Matter. Except for the last-named, which is a new Sub-committee, these committees are con- tinuing the work started under the old Committee, but for the first two the scope of work has been broadened with a corresponding change in constitution.Three reports have been prepared by their respective Sub-committees and have been approved for publication, as follows- Re$ort Prepared by Estimation of Vitamin El, Vitamin-B Panel Determination of Linalol Determination of Small Amounts of Organic Pesticides Residues in Foodstuffs Sub- Essential 61s Sub-committee Chlorine in Solvent Extracts of Vegetable Matter committee. The responsibility for the collection of the Standard Methods to supplement the Bibliography has now been assumed by the Committee itself and is no longer borne by a Sub-committee. A general form of presentation of the text of the methods has been agreed and so far two groups of the methods recommended in published Reports of the Analytical Methods Committee-namely, Analysis of Soaps (five methods) and Assay of Poisons (six methods)-have been collated and edited to conform to this. These are now under review to ensure that they are in line with current practice. Joint Committee on Analysis of Tyade Efluents-In addition to the Analytical Methods Committee and its Sub-Committees, there is an extremely active Committee on Methods of Analysis of Trade Effluents, which was set up jointly in February, 1954, by the Society and the Association of British Chemical Manufacturers under the Chairmanship of Mr.H. N. Wilson. This Joint Committee was appointed to continue the work originally started by an Analytical Sub-committee of the Association’s Trade Effluents Committee.The technical work of this Joint Committee is divided between four Panels and originally each Panel was responsible for its own secretarial administration, the Joint Committee acting as a steering and co-ordinating committee. Very soon after its establishment, the Secretariat of the Analytical Methods Committee assumed practically all the administrative and preliminary editing work of this Committee and its Panels and, as can be seen from the detailed progress report, this has become so voluminous that the greater part of the work of the Secretariat has been devoted to it during the last six or seven months. Although, strictly speaking, this work does not come directly under the aegis of the Analytical Methods Committee, the whole problem of the control of trade effluents is considered to be of such national importance and urgency that priority has been given to it in order to facilitate and expedite publication of the methods in The Analyst.264 REPORT OF THE ANALYTICAL METHODS COMMITTEE, 1955 [Vol.81 The preparation of methods has progressed rapidly and already the first three have been published (Analyst, 1956, 81, 59), three more have been prepared for publication in March, 1956, and there are some 20 to 30 others that have been completed and are now in various stages between approval by the Joint Committee and final editing, thus ensuring a constant supply for publication for some months to come. In all, 29 meetings of the Joint Committee and its Panels have been held since March, 1955.Research Studeuttshi+In the past, one of the difficulties of the Analytical Methods Committee has been to arrange for special investigations into certain fundamental problems that arise during the collaborative work of the Sub-committees and that require the services of a full-time worker. Such investigations can seldom be conveniently undertaken by members of the Sub-committee because they are already fully engaged in their own work. Because of the good financial start to the work of the Committee it was decided that part of the Trust Fund should be set aside at once t o meet this need by instituting a Studentship for research purposes, to be known as “The Society for Analytical Chemistry Studentship.” In view of the difficulties experienced in making accurate determinations of trace elements in organic matter, since these may be lost during the initial destruction of the organic material, the Committee has agreed that this problem should become the first subject for research.Since the behaviour of an element during ashing and subsequent chemical procedures can be followed by radiochemical techniques, the efficiency (or otherwise) of a particular method can be assessed, and it was decided that this new approach to the problem would be a fitting subject for the research work to be undertaken. Accordingly, arrangements have been made, by courtesy of the Director of the Atomic Energy Research Establishment, Harwell, for this work to be carried out under the direction of Mr. A. A. Smales at that Establishment, and the first Research Studentship, valued at jtT900 to Q O O O per annum for two years, has been awarded to Mr.T. T. A. Gorsuch, B.Sc., A.R.I.C., who takes up his appointment on April lst, 1956. EXPENDITURE- The audited statement of accounts (see Appendix 11) for the first nine months (February to October inclusive) shows an expenditure of Q715; the expenditure for November to January inclusive is about fT700, making a tota.1 for the year of approximately fT2400. The expenditure for 1956 will be considerably greater and is likely to be at least fT4000, the principal increases being due to‘increased salaries for the additions t o the staff and to expenses in connection with the Research Studentship. FUTURE WORK- As will be evident from the following detailed reports of the individual committees, there is still plenty of work in hand for some time to come.However, there is no lack of proposals and requests for problems to be tackled, and already the Committee is faced with the question of priorities. The collaboration with another organisation in the matter of analysis of trade effluents has proved so successful that exploratory talks have taken place with a view to collaboration with other organisations in other branches of the chemical industry. As a result, agreement has recently been reached with the Pharmaceutical Society for a Joint Committee to be set up to examine standard methods for the analysis of drugs and source materials that are either no longer official in the British Pharmacopoeia or in the British Pharmaceutical Codex, or are outside the scope of these two publications.REPORTS OF SUB-COMM1TTE;ES OF THE ANALYTICAL METHODS COMMITTEE MEAT PRODUCTS SUB-COMMITTEE CONSTITUTION- H. G. Rees, B.Sc., Ph.D., A.R.C.S., D.I.C., S. Back, B.Sc., F.R.I.C. Miss E. M. Chatt, B.Sc., F.R.I.C. 0x0 Lid. Crosse & Blackwell Ltd. British Food Manu facturing Indtxstries Research Association (Chairman) F.R.I.C.May, 19561 REPORT OF THE ANALYTICAL METHODS COMMITTEE, 1955 265 C. D. Essex, A.R.I.C. J. R. Fraser, B.Sc., A.C.G.F.C., F.R.I.C. S. M. Herschdoerfer, Ph.D., F.R.I.C. H. Amphlett Williams, Ph.D., A.C.G.F.C., 0 x 0 Ltd. Department of the Government Chemist T. Wall & Sons Ltd. Public Analyst F.R.I.C. APPOINTED-May 25th, 1955, to succeed the Meat Extract Sub-committee, the terms of reference having been broadened. FIRST MEETING-June 27th, 1955.NUMBER OF MEETINGS DURING THE YEAR-3. TERMS OF REFERENCE-"(^) The determination of the meat content of products containing meat; (b) the determination of the constituents of meat and meat products. NOTE-The term ‘meat products’ to include hydrolysed protein and, if found necessary, fish pastes.” PROGRAMME OF WORK- 1. The collection of data on nitrogen factors for all types of meat. 2. To investigate methods for the determination of starch. 3. To investigate the determination of yeast in order to ascertain the presence of yeast extract. At all times, the Sub-committee maintains liaison with the Food Standards Committee of the Association of Public Analysts. PROGRESS OF WORK- ,Nitrogen.factors-The collection of data on nitrogen factors is in progress; the literature is being searched, manufacturers are being approached and individual members of the Sub-committee are carrying out experimental work, 1. 2. 3. Determination of starch-Work not yet started. Determination of yeast-Work not yet :started. METALLIC IMPURITIES IN ORGANIC MATTER SUB-COMMITTEE CONSTITUTION- T. McLachlan, D.C.M., A.C.G.F.C., M.I.Biol., (Chairman) F.R.I.C. L. Brealey, B.Sc. C. L. Hinton, F.R.I.C. E. I. Johnson, MSc., A.R.I.C. I. MacIntyre, M.B., Ch.B. K. F. Milton, B.Sc., Ph.D., M.I.Biol., G. Taylor, O.B.E., F.R.I.C. G. E, Willis, B.Sc., Ph.D., A.R.I.C. F.R.I.C. Public A.italyst Boots Pure Drug CO. Ltd. British Food Manufacturing Industries Department of the Government Chemist Post-Graduate Medical School, University Analytical and Consultifig Biochemist Research Association of London Analytical and Consulting Chemist Imperial Chemical Industries Ltd.(Dye- stufls Division) APPOINTED-April 19th, 1955, to succeed the Metallic Impurities in Foodstuffs Sub-Com- mittee, the terms ,of reference having been broadened. FIRST MEETING-May loth, 1955. TERMS OF REFERENCE-“TO investigate the determination of small quantities of metals in organic matter.” NUMBER OF MEETINGS DURING THE YEAR-5. PROGRAMME O F WORK- 1. 2. To investigate the molybdenum-blue method for the determination of arsenic. To investigate methods for the destruction of organic matter to avoid loss or accretion of the metal being determined during the procedure.266 REPORT OF THE ANALYTICAL METHODS COMMITTEE, 1955 [Vol.81 3. To review, and revise if necessary, the method for lead published as a tentative recommended method by the earlier Sub-committee (Analyst, 1954, 79, 397). 4. To investigate methods for the determination of copper. At all times, the deliberations of the relevant Commission of the Analytical Section of the International Union of Pure and Applied Chemistry are noted. PROGRESS OF WORK- Molybdenum-blue method for arsenic-Collaborative experimental work is already in progress ; various reduction techniques are being investigated in relation to the subsequent spectrophotometric determination of the arsenomolybdate complex. Destruction of organic matter-The various accepted methods of wet and dry com- bustion, together with their many modifications, are being investigated to ascertain the conditions affecting the loss, retention or accretion of the metal being determined.As has already been recorded earlier in the General Review under “Research Student- ship,” this problem is considered of such importance to the analyst as to warrant special research being devoted to it. Method for lead-Evidence, both in this country and from abroad, has shown that, although it has been favourably received, the published tentative method has some limitations and work has now started on its revision. 4. Method for co@er-Work not yet started. 1, 2. 3. ESSENTIAL OILS SUB-COMMITTEE CONSTITUTION- W. H. Simmons, B.Sc., M.Inst.Pet., F.R.I.C. A. J. M. Bailey, B.Sc., M.P.S., F.R.I.C.J. F. Charpy C. ‘CV: Cornwell, M.Sc., F.R.I.C. G . W. Ferguson, B.Sc., Ph.D., F.R.I.C. D. C. Garratt, B.Sc., Ph.D., F.R.I.C. H. T. Islip, B.Sc., F.R.I.C. (Chairman) (Honorary Secretary) P. McGregor, B.Sc., A.H.-W.C., F.R.I.C. W. M. Seaber, B.Sc., F.R.I.C. J. H. Seager, M.Sc., F.R.I.C. G. E. Smith, B.Sc., F.R.I.C. Analytical and Consulting Chemist W. J . Bush G Co. Ltd. Formerly of J . & E. Atkinson Lid. A . Boake, Roberts & Co. Ltd. Analytical avtd Consulting Chemist Boots Pure Drug Co. Ltd. Colonial Products Laboratory, Colonial Department of the Government Chemist Analytical and Consulting Chemist Yardley G CO. Ltd. Staford Allen & Sons Ltd. Ofice APPOINTED-By the Committee on Uniformity of Analytical Methods (predecessor of the Analytical Methods Committee), August 21st, 1924.FIRST MEETING-October 16th, 1924. NUMBER OF MEETINGS DURING THE YEAR-1. PROGRESS OF WORKS-A Report on ‘‘ The Determination of Linalol in Essential Oils ” has been approved by the Committee and Council for publication. FUTURE PROGRAMME-On the completion of the specified programme of work the Sub- committee was formally dissolved. The following were recommended as subjects for future work- Peroxide value Ester determination Tertiary alcohols (including citronellol) Cineole - cresol tables (revision).May, 19561 REPORT OF THE ANALYTICAL METHODS COMMITTEE, 1955 267 PESTICIDES RESIDUES IN FOODSTUFFS SUB-COMMITTEE CONSTITUTION- G. Taylor, O.B.E., F.R.I.C. G. L. Baldit, BSc., A.R.I.C. E. D. Chilwell, B.Sc., F.R.I.C. Analytical and Consulting Chemist Plant Protection Ltd.Fisons Pest Cosltrol Ltd. (Chairman) (succeeded G. S. Hartley, D.Sc., on June 20th, 1955) €3. Egan, B.Sc., Ph.D., D.I.C., F.R.I.C. Department of the Government Chemist (representing the Food Group, Society of Chemical Industry) B. A. Ellis, M.A., F.R.I.C. Department of the Government Chemist J. C. Gage, B.Sc., Ph.D., A.R.I.C. Imperial Chemical Industries Ltd. (Indus- R. A. E. Galley, B.Sc., Ph.D., A.R.C.S., Colonial Products Laboratory, Cololzial D. C. Garratt, BSc., Ph.D., F.R.I.C. trial Hygiene Laboratories) D.I.C., F.R.I.C. Ofice Boots Pure Drug Co. Ltd. APPOINTED-February 4th, 1954, following a request by the Fungicide and Insecticide Research Co-ordination Service of the Agricultural Research Council. FIRST MEETING-March 26th, 1954.NUMBER OF MEETINGS DURING THE Y E A R 4 (including 2 Of the Working Party (q.v.) and 1 jointly with the Metallic Impurities in Organic Matter Sub-committee). TERMS OF REFERENCE-“TO examine the present position in respect of methods of analysis of foodstuffs for residual traces of pesticides, as the first action of the Sub-committee; and, further, if deemed desirable, to recommend for general acceptance methods of analysis now in use, or to develop or assist in the development of new methods of analysis or modifications of methods now in use.” PROGRAMME OF WORK- 1. To devise a method for the accurate and precise determination of small amounts of chlorine in solvent extracts of foodstuffs for the purpose of identifying the presence of chlorinated hydrocarbons.2. To investigate extraction procedures, and methods for removing organic impurities and colour from the resulting solutions. 3. To investigate methods for the determination of organo-phosphorus compounds, 1. Determination of small amounts of chlorine-For the purpose of this work a small Working Party was appointed, consisting of: G. Taylor, O.B.E., F.R.I.C. (Chairman) ; A. J. Feuell, B.Sc., Ph.D., A.R.I.C. (Colonial Products Laboratory); D. C. Garratt, B.Sc., Ph.D., F.R.I.C. ; G. A. Sergeant, M.Sc., A.R.I.C. (Department of the Government Chemist). This work has been completed and a Report on “The Determination of Small Amounts of Organic Chlorine in Solvent Extracts of Vegetable Material” has been approved for publicat ion. 2. Extraction procedure-Collaborative experimental work is now being carried out by the same Working Party.3. Organo-Phosphorw com+ounds-Work not yet started. PROGRESS OF WORK- TRACE ELEMENTS IN FERTILISERS AND FEEDING-STUFFS SUB-COMMITTEE CONSTITUTION- J. H. Hamence, M.Sc., Ph.D., F.R.1 .C. D. C. Garratt, B.Sc., Ph.D., F.R.I.C. E. I. Johnson, M.Sc., A.R.I.C. R. F. Milton, B.Sc., Ph.D., M.I.Biol., Public Autalyst, Oflcial Agricultural (Chairmart) Analyst ami! Cons.uZti.lg Chemist Boots Pure Drug CO. Ltd. Department of the Government Chemist Analvtical and Consulting Biochemist F.R.I.C.268 REPORT OF THE ANALYTIiCAL METHODS COMMITTEE, 1955 [Vol. 81 R. L. Mitchell, B.Sc., Ph.D., F.R.I.C. A. A. Smales, BSc., E.R.I.C. Atomic Energy Research Establishment, C. Whalley, B.Sc., F.R.I.C. APPOINTED-February 4th, 1954.FIRST MEETING-March 30th, 1954. TERMS OF REFERENCE---(‘TO devise appropriate methods of analysis (to be recommended for inclusion in the Regulations under the Fertilisers and Feeding Stuffs Act, 1926) for the determination of the trace elements manganese, copper, zinc, cobalt, molybdenum, iodine, selenium and fluorine, and also for boron, magnesium and iron, which can be expected to be present in fertilisers in small quantities as distinct from traces.” PROGRAMME AND PROGRESS OF WORK-The terms of reference indicate the scope of the work and it is intended that methods should also be devised for feeding stuffs in appropriate cases. It is also intended to collaborate in a general revision of the methods of analysis at present prescribed in the Regulations under the Fertilisers and Feeding Stuffs Act, 1926. Samples of typical materials, with added known amounts of trace elements, have been circulated to selected members of the Sub-Committee for preliminary exploratory work, in which both physical and chemical techniques are being used. V ITAMI NS When the new Committee reviewed the work of the various Sub-Committees, it was decided not to recall the Vitamins Sub-committee but merely to allow the work of the two existing Panels-on vitamin B,, and vitamin E-to be completed. For this reason, only the details of these two Panels are given below. V i tamin-B,, Panel COSSTITUTION- Macauley Institute for Soil Research (Department of Spectrochemistry) Harwell Paint Research Station.NUMBER OF MEETINGS DURING THE YEAR---;?rTOne.A. J. Amos, B.Sc., Ph.D., F.R.I.C. F. Wokes, B.Sc., Ph.D., F.P.S., F.R.I.C. W. F. J. Cuthbertson, BSc., Ph.D., F.R.I.C. J. E. Ford, B.Sc., Ph.D. F. W. Norris, D.Sc., A.R.C.S., D.I.C., F.R.I.C. S. A. Price, B.Sc. G. E. Shaw, BSc. R. E. Stuckey,B.Sc., Ph.D., F.P.S., F.13.I.C. G. Sykes, M.Sc., F.R.I.C. (Chairmafi) (Honorary Secretary) Analytical and Consulting Chemist Ovaltine Research Laboratories Glaxo Laboratories Ltd. National Institute for Research in Dairying University of Birmingham (Department of Applied Biochemistry) Vitamins Ltd. Evans Biological Institute British Drug Houses Ltd. Boots Pure Drug Co. Ltd. APPOINTED-February 24th, 1953. As a result of its recommendations, the Panel was appointed as above. FIRST MEETING-December 7th, 1953. PROGRESS OF WORK-The Panel has completed its work and a Report on “ The Estimation of Vitamin B12” is being published in March, 1956.Vitainin-E Pan.el CONSTITUTION- An ad hoc Advisory Panel met on April 23rd, 1953. NUMBER OF MEETINGS DURING THE YEAR-2. The Panel has now been disbanded. A. L. Bacharach, M.A., F.R.I.C. J. Green, B.Sc., Ph.D., A.R.I.C. A. R. Moss, B.Sc., Ph.D. H. N. Ridyard, B.Sc., A.K.C., F.R.I.C. Research Association of British Flour Glaxo Laboratories Ltd. Vitamins Ltd. Roche Products Ltd. (Chairman) (Honorary Technical Secretary) MillersMay, 19561 REPORT OF THE ANALYTICAL METHODS COMMITTEE, 1955 269 P. W. Russell Eggitt, B.Sc., A.R.I.C. C. A. Shacklady, B.Sc., A.R.I.C. P. Stross, B.Sc. G. Walley, BSc., F.R.I.C. R. J. Ward, B.Sc., A.R.I.C.E. C. Wood, B.Sc., Ph.D., A.R.C.S., F.R.I.C. F. Brown, MSc., Ph.D.* P. Harris, Ph.D.* Spillers Ltd. J . Bibby & Sons Ltd. British Drug Houses Ltd. Unilever Ltd. The Dunn Nutritional Laboratory, Vedical Analytical a d Consultiflg Chemist Christie Hospital and Holt Radiam Insti- Distillation Products Industries, Rochester, Research Council tute, Manchester New York, U.S.A. * Corresponding member. APPOINTED-March, 1953. the need for standardising methods of vitamin-E estimation. tions, the Panel was appointed as above. FIRST MEETING-December 9th, 1953. An ad hoc Advisory Panel met on May 8th, 1953, to consider As a result of its recommenda- NUMBER OF MEETINGS DURING THE YEAR-5. TERMS OF REFERENCE (OF ADVISORY PANEL)--(-(To survey the methods already proposed for the estimation of vitamin E and to recommend to the [Vitamins] Sub-committee a standard method or methods.” PROGRAMME OF woRK-It was decided to consider only chemical methods for estimating tocopherols, collectively and individually, in food and feeding stuffs.A study of the method of Emmerie and Engel, with recent modifications involving chromatographic separation, was therefore undertaken. PROGRESS OF WORK-AS a result of collaborative experimental work, the Panel believes that a method for the determination of a-tocopherol can be recommended and a draft method is now under consideration. A draft of a general introduction to the whole report is also in hand. Work continues on elaborating this method for the differential determination of any or all of the seven known tocopherols. DIRECT MICRO-DETERMINATION OF OXYGEN IN ORGANIC MATTER SUB-COMMITTEE This Sub-committee was set up as a result of a proposal by the Microchemistry Group of the Society to carry out collaborative experimental work on the Unterzaucher method for the determination of oxygen.CONSTITUTION D. W. Wilson, M.Sc., F.R.I.C. G. C. Ackroyd, B.Sc., A.R.I.C. P. R. W. Baker, B.Sc., A.R.I.C. Miss B. B. Bauminger, Ph.D., A.R.I.C. W. T. Chambers, B.Sc., Ph.D ., A.R.I.C. (Chaimnarc) A. F. Colson, B.Sc., Ph.D., F.R.I.C. Miss M. Corner, B.Sc., F.R.I.C. R. R. Gordon, Ph.D. G. Ingram, A.R.I.C. F. J. McMurray F. H. Oliver C . Whalley, B.Sc., F.R.I.C. H. J. Warlow Sir John Cuss College (Department of D.S.I.R., Fuel Research Station Wellcome Research Laboratories Dunlop Research Centre British Rubber Prodwers’ Research Asso- Imperial Chemical Irtdustries Ltd.(Alkali D.S.I.R., Chemical Research Laboratory National Coal Board, Central Research Courtaulds Ltd. Wellcome Chemical Works Courtaulds Ltd. D.S.I.R., Fael Research Station Paint Research Station Chemistry) ciation Division) Establishment270 REPORT OF THE ANALYTICAL METHODS COMMITTEE, 1955 [Vol. 81 APPOINTED-June 28th, 1955. MEETINGS-NO meetings have yet been held, the preliminary work being conducted by post. PROGRAMME OF WORK-TO investigate the Unterzaucher method, and its modifications, for the micro-determination of oxygen. PROGRESS OF WORK-Four samples of organic substances have been circulated to the Sub- Committee for collaborative experimental tests, each member employing his or her own version of the method.Detailed report forms have also been circulated and a number of these have now been returned to the Secretary for collation, before discussion at the first meeting. REPORT OF THE A.B.C.M.-S.A.C. JOINT COMMITTEE ON THE ANALYSIS OF TRADE EFFLUENTS CONSTITUTION- Representing The Association of British Chemical Manu facturers- H. N. Wilson, F.R.I.C.* J. G. Maltby, B.Sc., F.R.I.C.* F. G. Broughall, B.Sc., F.R.I.C. D. C. Garratt, B.Sc., Ph.D., F.R.1.C:. I. S. Wilson, M.Sc., Ph.D., A.R.I.C. Representing The Society for Analytical Chemistry- J. H. Hamence, M.Sc., Ph.D., F.R.f.C.* Public Analyst, Oficial Agriczdtural L. Klein, M.Sc., Ph.D., M.Inst.S.P., F.'R.I.C. C. J. Regan, B.Sc., F.R.I.C. J. G. Sherratt, BSc., F.R.I.C.K. A. Williams, B.Sc., Ph.D., A.Inst.P., N. T. Wilkinson, F.R.I.C. Imperial Chemical Industries Ltd. (Billing- (Chairman) ham Division) Distillers Co. Ltd. (Secretary) Midland Tar Distillers Ltd. Boots Pure Drug Co. Ltd. Monsanto Chemicals Ltd. Analyst and Consulting Chemist Mersey River Board Formerly Chemist-in-Chie f, London County Public Analyst and Consulting Analytical Analytical and Consulting Chemist Imperial Chemical Industries Ltd. (Alkali Council Chemist M.Inst.Pet., F.R.I.C. Division) J. S. Evans Miss C. H. Tinker, BSc., Ph.D., A.R.I.C." Federation of British Industries Secretary to the Analytical Methods Com- mittee * Members of the Publication Sub-Committee, t o which J. B. Attrill, M.A., F.R.I.C., Editor of The ,4nalyst, has been co-opted. APPOINTED-AS a Joint Committee by the Society and by the Association of British Chemical Manufacturers, February 17th, 1954.FIRST MEETING-March 19th, 1954. NUMBER OF MEETINGS DURING THE YEAR--^ 1 (including 5 of the Publication Sub-Committee). TERMS OF REFERENCE-"TO devise and recommend methods of analysis as applied to trade effluents, specifying in each case their applicability and limitations, but not the interpretation of the results of such tests as would be used to decide on the quality of an effluent. Such methods would be published by the Society as Recommended Methods." CONSTITUTION- PANEL 1 : ORGANIC MATTER-GENERAL C . J. Regan, B.Sc., F.R.I.C. Formerly Chemist-in-Chie f, Loadon County G. S. Clements, A.R.C.S., F.R.I.C. Public Health Department, London County W.M. Cameron, M.Inst.S.P., F.R.I.C. Main Drainage Department, Middlesex (Chairman) Council (Secretary) Council County CouncilMay, 19561 REPORT OF THE ANALYTICAL METHODS COMMITTEE, 1955 271 W. T. Lockett, M.Sc. M a i n Drainage Department, Middlesex T. B. Moore, B.Sc. A . E. J. Pettet, B.A. I. S. Wilson, M.Sc., Ph.D., A.R.I.C. Miss C. H. Tinker, B.Sc., Ph.D., A.R.I.C. County Council North Thames Gas Board D.S.I.R., Water Pollution Research Lab- Monsanto Chemicals Ltd. Secretary to the Analytical Methods Com- oratory mittee FIRST MEETING-March 31st, 1954. hrUMBER OF MEETINGS DURING THE YEAR (AS FROM MARCH IST, 1955)-5. PROGRAMME OF WORK- Methods f o r determining oxygen demand-(a) general considerations ; ( b ) permanganate value (oxygen absorbed from permanganate) ; (c) biochemical oxygen demand ; (d) dichromate value (oxygen absorbed from boiling dichromate) .Methods f o r determining combined nitrogen-(a) free and saline ammonia ; (b) albuminoid nitrogen; (c) organic nitrogen; ( d ) total unoxidised nitrogen; (e) nitrogen as nitrite; (f) nitrogen as nitrate. Methods for determining total organic carbon. Methods f o r determining phosphorus. ,Vethods for determining chloride ion (chlorion) . To list inhibitory substances, present in some trade effluents, which may interfere in any of the recommended methods. PROGRESS OF WORK- Work completed-Methods for determining the following have been passed to the Main Committee for approval : permanganate value; dichromate value ; chloride ion (chlorion) ; organic carbon.Work in hand-Draft methods for determining the following are nearing completion : ( a ) the various forms of combined nitrogen; (b) biochemical oxygen demand; (c) phosphorus. PANEL 2 : METALLIC CONTAMINANTS CONSTITUTION- N. T. Wilkinson, F.R.I.C. Imperial Chemical Industries Ltd. (Alkali D. C. Garratt, B.Sc., Ph.D., F.R.I.C. Boots Pure Drug Co. Ltd. J. H. Hamence, M.Sc., Ph.D., F.R.I.C. Pzablic Analyst, Oficial Agricultural Analyst and Consulting Chemist J. G. Sherratt, B.Sc., F.R.I.C. Public Analyst and Consulting Analytical Chemist Miss C. H. Tinker, B.Sc., Ph.D., A.R.I.C. Secretary to the Analytical Methods Com- (Chairman) Division) (Secretary) mittee FIRST MEETING-September loth, 1954. NUMBER OF MEETINGS DURING THE YEAR (AS FROM MARCH 1ST, 1955)-6. PROGRAMME OF WORK- Preliminary treatment of sample.Methods for determining aluminium, antimony, arsenic, barium, cadmium, chromium, copper, iron, lead, manganese, mercury, molybdenum, nickel, potassium, selenium, silicon, silver, sodium, sulphate, titanium and zinc. PROGRESS OF WORK- Work completed-The following methods were published during the year (Analyst, 1956, 81, 59) : Preliminary treatment of sample (destruction of organic matter) ; determination of arsenic ; determination of copper. Methods for determining the following have been prepared for publication in March, 1956: iron, mercury and nickel. Methods for determining the following have been passed to the Main Committee for approval : chromium, lead and selenium.272 REPORT OF THE ANALYTICAL METHODS COMMITTEE, 1955 [Vol.81 Work is proceeding on methods for zinc and silver, and methods for other metals and sulphate are being considered, Work irt hand-The final draft method for manganese is being prepared. PANEL 3 : NON-METALLIC CONTAMINANTS CONSTITUTION- It. G. Broughall, B.Sc., F.R.I.C. W. G. Carey, F.R.I.C. G. U. Houghton, M.Sc., Ph.D., F.R.I.C. E. A. W. Whitlock, B.Sc., A.R.I.C. Midland Tar Distillers Ltd. Public Analyst and O$icial Agricultural Analyst; Consultant South Essex Waterworks Co. Wallace & Tieynan Ltd. (Chairman) MEETINGS-The Panel has not met; so far its work has been conducted by post. PROGRAMME OF worn-Methods for deterrnining free chlorine, cyanide, fluorine, formaldehyde, phenols, sulphide, sulphite, thiocyanate and thiosulphate. PROGRESS OF WORK-Methods for determining phenols and sulphide are in draft.PANEL 4.: PHYSICAL TESTS CONSTITUTION- J. G. Sherratt, B.Sc., F.R.I.C. L. Klein, M.Sc., Ph.D., M.Inst.S.P., F.R.I.C. G. A. Vaughan, A.R.I.C. K. A. Williams, B.Sc., Ph.D., A.Inst.P., M.Inst.Pet., F.R.I.C. Miss C. H. Tinker, BSc., Ph.D., A.R.I.C. (Secretary) mittee Public Analyst and Consulting Analytical Mersey River B o d Coal Tar Research Associatiort Analytical and Consulting Chemist Secretary to the Analytical Methods Com- (Chairman) Chemist FIRST MEETING-May 11 th, 1954. NUMBER OF MEETINGS DURING THE YEAR (A4S FROM MARCH IST, 1955)-8. PROGRAMME OF WORK- Method of sampling. Measurement of colour, transparericy, temperature and pH. Determination of suspended solids, settleable solids, dissolved solids, immiscible liquids such as oil or tar, hardness (total hardness, calcium hardness and magnesium hardness), acidity and alkalinity.PROGRESS OF WORK- Work completed-The following methods have been passed to the Main Committee for approval : method of sampling ; general description ; measurement of colour, temperature, transparency and pH ; determination of suspended solids, settleable solids, residue on dissolved solids and matter extractable by light petroleum. Work in hand-Work is proceeding on methods for the determination of acidity, hardness and immiscible volatile liquids. February 14th, 1956 APPENDIX I TEXT OF THE DEED OF TRUST THIS DEED OF TRUST is made the first day of February One thousand nine hundred and fifty six BETWEEN THE SOCIETY FOR ANALYTICAL CHEMISTRY whose registered office is situate at 7/8 Idol Lane E.C.3 in the City of London (hereinafter called “the Society”) of the one part and THE HONOURABLE SIR GEORGE HAROLD LLOYD-JACOB of Fredley Manor Nickleham in the County of Surrey and DOUGLAS WILLIAM KENT-JONES of 18 Welsby Court Eaton Rise W.5.in the County of London and KENNETH ALAN WILLIAMS of 11 St. Dunstan’s Avenue W.3, in the County of Middlesex and JACK HUBERT HAMENCE of 43 Westland Drive Hayes in the County of Kent and NOEL LIONEL ALLPORT of 325 KenningtonMay, 19561 REPORT OF THE ANALYTICAL METHODS COMMITTEE, 1955 273 Road S.E.ll in the County of London (hereinafter together called “the Trustees’’ which expression shall where appropriate include the Trustees or Trustee for the time being hereof) of the other part (1) The Society is an association not for profit and was in the year One thousand nine hundred and seven registered under the Companies Acts 1862 to 1900 as a company limited by guarantee and not having a share capital The principal objects of the Society are to encourage assist and extend the knowledge and study of analytical chemistry and of all questions relating to the analysis nature and composition of natural and manufactured materials generally and to promote or assist to promote the efficiency and the proper administration of the laws relating to the control and composition of such materials generally and to take any steps which may be considered advisable for advancing or protecting the interests of analytical chemistry (2) The Society being desirous of establishing such a charitable trust as herein appears has caused to be transferred into the joint names of the Trustees the investments and cash (herein together called “the Initial Fund”) particulars whereof are set out in the Schedule hereto to the intent that the same shall be held upon the trusts and with and subject to the powers and provisions herein declared and contained concerning the same (3) I t is apprehended that further moneys investments and property may hereafter be transferred to the Trustees as an accretion to the Initial Fund (4) The Society has from among its members formed a Committee called and hereinafter referred to as “the Analytical Methods Committee” for the purpose of advising the Trustees on all matters concerning the allocation and application of the Trust Fund NOW THIS DEED WITNESSETH and it is hereby agreed as follows:- 1.THE Trustees shall hold the Initial Fund and all such further moneys investments and property as may from time to time be transferred or paid to the Trustees as an accretion thereto (as and when the same shall be received) and the investments and property from time to time representing the same upon the trusts and with and subject to the powers and provisions hereinafter contained 2. THE Initial Funds and such moneys investments and property as aforesaid and the WHEREAS - - 1 investments and property from time to time representing the same (hereinafter collectively called “the Trust Fund”) shall constitute a fund to be known as “the Society for Analytical Chemistry Analytical Methods Trust Fund” 3.THE Trustees shall hold the Trust Fund upon trust subject to the provisions of the next succeeding Clause hereof to apply the capital and income thereof in such manner as the Trustees shall think fit in promoting and encouraging the acquisition and dissemination of knowledge in regard to methods of chemical analysis the study and improvement of methods of chemical analysis and the education of persons as analytical chemists 4. THE Trustees shall out of the Trust Fund pay all costs and expenses of or incidental to the preparation and execution of these presents and the transfer to the Trustees of the investments comprised in the Initial Fund and the costs charges and expenses of the Trustees in or about the management of the Trust Fund and the execution of the trusts and powers upon and subject to which the same is held 6.WITHOUT prejudice to the generality of the powers conferred upon them by Clause 3 hereof it is hereby declared that the Trustees may for the purposes of exercising such powers :- (a) establish and maintain a Secretariat and staff to work under the direction of the Analytical Methods Committee and Sub-committees and panels thereof and may under the like direction organise such research and other activities as may be expedient to discover and publish particulars of standard or approved methods of analysis (b) provide or assist in providing all necessary means including books instruments plant equipment and chemical and other materials for the pursuit of research and274 REPORT OF THE ANALYTICAL METHODS COMMITTEE, 1955 [Vol.81 investigation into all matters relating to the development and establishment of methods of analysis (c) establish and maintain bursaries scholarships studentships and grants-in-aid for the benefit of students of and workers in any college university or other laboratories in which the study of analytical chemistry is pursued (d) establish and maintain studentships to be called “the Society for Analytical Chemistry Studentships” of such annual value as the Trustees may from time to time determine to be awarded in manner hereinafter mentioned to students of and workers in any college or university or other laboratories in which the study of analytical chemistry is pursued and to be held and enjoyed as hereinafter provided (e) establish and maintain a scholarship or scholarships to be called “the Society for Analytical Chemistry Scholarships” of such value as the Trustees may from time to time determine and such scholarships shall be awarded to such persons and be held and enjoyed as hereinafter provided (f) establish or maintain or assist in establishing or maintaining a chair or professorship for the advancement of analytical cheinistry at any university teaching hospital or place of learning in the United Kingdom (g) develop organise enter into and carry out or co-operate in any scheme or schemes which is or are calculated to further the objects of the Trust Fund 6.ANY such studentships or scholarships as aforesaid shall be awarded at such intervals to such persons and in such manner and shall be held and enjoyed for such period and upon and subject to such terms and conditions as shall from time to time be determined by regulations to be made by the Trustees in consultation with the Analytical Methods Committee and the Trustees may at any time revoke or alter any regulations made under the provisions of this clause and make new regulations in the place thereof- 7.THE Trustees may invest so much of the Trust Fund as shall not be immediately required in any investments permitted by law for the investment of trust money or any investments which at the time of investment are officially quoted on the Stock Exchange London Provided that no investment shall be made in the shares or securities of any company the paid up capital of which at the time of investment is less than five hundred thousand pounds or its equivalent in the currency of the place of registration of such company with power for the Trustees to vary such investments for others of any nature hereby authorised 8.THE statutory power of appointing a new Trustee or new Trustees hereof shall apply IN WITNESS whereof the Society has caused its common seal to be affixed and the Trustees have set their respective hands and seals the day and year first above written SCHEDULE El00 Ceylon Government 3ay0 Stock 1959 El00 39% Conversion Stock El00 33% War Stock k6000 Cash The Deed of Trust was signed and sealed on behalf of the Society by the President, Dr. K. A. Williams, the Honorary Secretary, Mr. N.L. Allport, and Messrs. J. R. Leech, L. Hinton and H. W. Hodgson, and signed and sealed by the Trustees, The Honourable Sir George Lloyd-Jacob, Dr. D. W. Kent-Jones, Dr. K. A. Williams, Dr. J. H. Hamence and Mr. N. L. Allport.\ May, 19561 REPORT OF THE ANALYTICAL METHODS COMMITTEE, 1955 275 APPENDIX I1 INCOME AND EXPENDITURE ACCOUNT OF THE ANALYTICAL METHODS COMMITTEE FROM FEBRUARY lST, 1955, TO OCTOBER 3 1 ~ ~ , 1955 L L Rent, Light, Heat and Telephone . . 40 Donations received January 1st to Salaries . . .. * . .. 1198 October 31st from lndustry as Other Expenses, including Printing Balance Carried to Balance Sheet . . Office Equipment . . .. .. 232 result of Appeal . . . . . . 8794 and Stationery . . .. .. 236 7079 - -- i8794 A8794 __ - - APPENDIX I11 SUBSCRIBERS TO THE TRUST FUND Albright & Wilson Ltd. Allied Bakeries Research Laboratories Ltd. James Anderson & Co. (Colours) Ltd. The Associated Ethyl Company Ltd. Bakelite Ltd. Raker Perkins Ltd. Baker Platinum Ltd. J. Bibby & Sons Ltd. A. Boake, Roberts & Co. Ltd. Boots Pure Drug Co. Ltd. Borax Consolidated Ltd. Bovril Ltd. The British Aluminium Co. Ltd. The British Arkady Co. Ltd. British Celanese Ltd. The British Drug Houses Ltd. British Electricity Authority British Glues & Chemicals Ltd. The British Oxygen Co. Ltd. Brotherton & Co. Ltd. W. J. Bush & Co. Ltd. Cadbury Brothers Ltd. W. Canning & Co. Ltd. Chivers & Sons Ltd. Cooper, McDougall & Robertson Ltd. The Crookes Laboratories Ltd. The Distillers Company Ltd. Dunlop Research Centre The English Electric Co. Ltd. Esso Development Co. Ltd. Ferranti Ltd. Fisons Ltd. A. Gallenkamp & Co. Ltd. Glaxo Laboratories Ltd. Arthur Guinness, Son & Co. (Park Royal) Ltd. Thomas Hedley & Co. Ltd. H. J. Heinz Company Ltd. Hopkin & Williams Ltd. Horlicks Ltd. Huntley & Palmers Ltd. Ilford Ltd. Imperial Chemical Industries Ltd. Johnson, Matthey & Co. Ltd. Laporte Chemicals Ltd. Levy & West J. Lyons & Co. Ltd. Macfarlane, Lang & Co. Ltd. John Mackintosh & Sons Ltd. The Man-Made Fibres Producers’ Committee Marks & Spencer Ltd. The Marmite Food Extract Co. Ltd. May & Baker Ltd. The Metal Box Company Ltd. The Millers’ Mutual Association Monsanto Chemicals Ltd. National Coal Board L. Oertling Ltd. 0x0 Ltd. Peek, Frean & Co. Ltd. Pilkington Brothers Ltd. Procea Products Ltd. Quaker Oats Ltd. Reckitt & Colman Ltd. Research Laboratories of The General Elec- Roche Products Ltd. Rowntree & Co. Ltd. Scribbans-Kemp Ltd. “Shell” Research Ltd. Spratt’s Patent Ltd. Stafford Allen & Sons Ltd. Stanton Instruments Ltd. John & E. Sturge Ltd. Tate & Lyle Ltd. Thorium Ltd. Unilever Ltd. Virol Ltd. Vitamins Ltd. Wallace & Tiernan Ltd. The Wellcome Foundation Ltd. tric Co. Ltd.

ISSN:0003-2654    

DOI:10.1039/AN9568100261

出版商:RSC    

年代:1956

数据来源: RSC

摘要:

276 SLATER: TH:E EVOLUTION OF [Vol. 81 The Fourth Bernard Dyer Memorial Lecture The Evolution of ,Agricultural Research BY SIR WILLIAM SLATER, K.B.E. (Delivered after the Annual General Meeting of the Society, February 29th, 1956) WHEN we meet to honour a great man, we can do so best by considering one of the qualities which marked him as outstanding amongst his fellows. Bernard Dyer had many admirable qualities, any one of which might form the subject of a lecture in his honour. In picking a subject, however, the lecturer must have in mind not only the quality he selects but also, if honour is truly to be paid, the need to show how those following in Dyer’s footsteps may draw strength and inspiration from the study of this aspect of his life and work. Before I decided on the subject of this lecture, I read again the admirable word picture of Dyer the man and of the work he did, painted by Sir John Russell in the first memorial lecture, knowing I should find there the inspiration I sought in picking a facet of Dyer’s work which might enable rle to say something not entirely unworthy of the occasion.As I read, I became more and more impressed by Dyer’s ability to grasp the essentials of a practical agricultural problem, to state it with great clarity and simplicity, and to apply his knowledge of chemistry to its solution. He did not speak in high-flown phrases of science for science’s sake, nor did he enunciate his findings in terms intelligible only to his fellow scientists. Almost every investigation he undertook arose from the need to solve a problem of importance to agriculture, either one which he had set for himself or, more often, one which had been put to him by a group of farmers who were his clients.The results he obtained were stated with a simple clarity understandable to the intelligent layman, such as is achieved only by a small select band of gifted scientists. Yet in the work he was doing he was laying a large part of the foundation of modern soil chemistry. I hope to show how these qualities, whereby Dyer was able to serve faithfully the practical needs of agriculture, whilst at the same time so orientating his work that he achieved results of great basic importance, are called for in the planning and organisation of agricultural research as we know it to-day. Perhaps the best way to begin is to iask the very simple and fundamental question: “What is agricultural research?” Whenever this question is asked, the answers tend to be varied and to be confused by the concept of agriculture as a science in its own right. Agriculture is not a science; it is an industry concerned with the growing of crops and the raising and care of stock.It is perhaps true that it is indeed, as is sometimes said, a “way of life,” because to some men there is no other acceptable occupation, but essentially it is an industry, producing goods for sale and providing a livelihood for those working in it. Once this is accepted, the nature of agricultural research becomes simply the study by scientific method of the problems of agriculture. There is no scientific discipline which holds a special place in this work; it is a meeting ground of all the sciences, and each problem must be attacked by the men best equipped for its solution. As in every other industry, the more the individual scientist knows of the industry he is serving the better able he will be to provide a solution to its problems.It is not, however, essential or even desirable that every worker should have a wide knowledge of agriculture; it is important that the problems he is called upon to solve should be stated to him clearly in terms which he can understand and which will enable him to appreciate their importance to the practical farmer. To do this, men are wanted with an intimate knowledge of agriculture and with a wide scientific training, to act as the interpreters between the laboratory and the production process.These men must be able to recognise and assess the problems that are facing the producer and to analyse these problems into their scientific components before they are put to the laboratory worker. They must be able to discuss the nature of the problem in scientific terms and be capable of understanding the method which the scientist proposes to use for its solution. At the same time, they should be sufficiently familiar with the broad outline of scientific progress to be able to suggest where the results of scientific work offer possibility of application in practice. Finally, it should be their duty to study the best way in which new knowledge can be incorporated into commercial farming.May, 19561 AGRICULTURAL RESEARCH 277 The task of these intermediaries clearly demands qualities rarely found in one man, and would be impossible were it not that many laboratory workers, by their knowledge of at least the aspect of agriculture related to their own work, can meet him more than half-way and that more and more farmers are receiving training which enables them to help in stating their problems in scientific language and in applying new knowledge on their farms.It is entirely fallacious to believe that the work done by the intermediary between the laboratory and the field requires a lower order of intelligence than that needed in a laboratory worker. The idea that, provided a man has mud on his boots and can talk in a bluff, hearty way to farmers about their troubles and worries, he can fill this difficult role is nonsense.Contact between research workers and farmers as a whole has to pass first through the more intelligent and highly trained section of the farming population, and hence it is with this section the intermediary must be qualified to deal; to win their respect his scientific knowledge must be manifestly greater than their own. It is true he must know his farming well and he must have the gift of getting on with farmers and farm workers, but he must equally be a man with a high degree of intelligence and a scientifically trained mind and be endowed with more than an ordinary share of imagination. The training and recruitment of men for this type of work is one of the major problems of agricultural research, and I shall return to it later. When Bernard Dyer began his work in agricultural chemistry, farming, under the influence of Lawes and Gilbert and of Augustus Voelcker, was turning more and more to the chemist for advice and help.The science of chemistry was at the same time itself advancing rapidly, so that the small band of pioneer workers, engaged in applying chemistry to the solution of agricultural problems, had a wide range of knowledge and techniques available to them for use in their investigations. Before the First World War, fundamental knowledge in the major scientific disciplines continued to grow faster than it could be used by the workers then engaged in agricultural research. It seemed unlikely that the rate of application of the scientific facts and methods at their disposal would ever be fast enough to exhaust the store on which they drew.From 1920 onwards, however, there was a great and rapid expansion in the number of workers engaged in agricultural research and in the facilities available to them. Much of this growth was stimulated by the farmers and horticulturists themselves; it was the logical sequence to the employment of the private consultant. In the next decade, many of our leading research institutes were founded and those already in being greatly expanded. The major problems of agriculture were vigorously attacked by the exponents of many different scientific disciplines. Those for which a solution could be sought by the straight- forward application of the knowledge and techniques already available were dealt with first and many notable and valuable results were achieved.There were, however, other problems of great practical importance which could not be solved by the direct application of the facts and methods already available to the workers. On some it was impossible even to make a start, whilst in others a promising beginning was made only for the workers to find themselves a t a dead end; they could progress no farther until the immediate obstacle could be surmounted or an entirely new path of attack opened. The character of agricultural research has, as a result, greatly changed in the last twenty years. Although scientific knowledge was advancing during this period more rapidly than ever before, it was obvious that the worker in agricultural research could not wait for someone else to provide the basic information he needed or to evolve the new tech- nique without which he could not progress; he found that he himself must carry out investi- gations in fundamental science to forge the tools he wanted for his work.In the period between the two World Wars, the recruits to agricultural research were mostly men trained in one of the basic sciences, who were drawn by an interest in agriculture to apply their knowledge and skill to the solution of its problems. They may at first have known little about farming methods, but they learned very quickly, as they brought a trained mind to work with enthusiasm and sympathy on the task to which they had been drawn. With the increasing need for fundamental work, another type of recuit has come into the agricultural research service in increasing numbers, a man who is more attracted by a desire to seek scientific knowledge for its own sake than to solve the applied problems. He sees in a research institute the extensive facilities needed for much modern research and the opportunity to devote his time solely to the work in which he is interested, without278 SLATER: THE: EVOLUTION OF [Vol.81 the distractions of teaching he would have in a university appointment. These men, joining the staff of an existing institute to work, say, in the field of biochemistry, may never get the understanding and sympathy for agriculture which is characteristic of the older workers who entered agricultural research to apply their knowledge to the solution of practical problems.There is an advantage in having a number of workers concentrating on fundamental studies and not concerning themselves with the industry. Often the temperament and intellectual approach of a man capable of doing original work of this type are unsuited to applied research. This difference may be sometimes overstressed and the scientist working in a pure field may become a little “precious.” It is, however, impossible to dispute that the difficulty of keeping in touch with the literature and developments in any single modern science makes it essential to have a number of men who concentrate on a science rather than on the broad problems of an industry. There are, nevertheless, two aspects of the recruitment of these pure scientists which must be carefully watched.The first is the maintenance of the right balance between the different types of workers and the second the need to ensure that the workers and the work in the pure science subjects are of a kind and quality to justify the expenditure involved. In many university departments there has been a growing tendency to encourage science graduates to look to pure rather than to applied research as a career. It has become almost a sign of failure if a graduate does not get a post-graduate award and stay at his university to work for a Ph.D. degree. The goal at which men are encouraged to aim is a career in pure research, with a long list of scientific publications and the Fellowship of the Royal Society as a final objective.No one would quarrel with the desirability of this goal, but few among the science graduates of our universities have the imagination, the determination and the intelligence to achieve it. Yet once a man has set out towards it, he finds a change of direction most difficult. Schooled to think of applied research as an inferior type of work, he must regard a change from pure research, in which he follows his own fancy in selecting a problem, to applied, in which his problems are provided for him, as a retrograde step. He often continues to struggle along the way he has chosen, vigorously and sometimes bitterly resenting any suggestion that he should change it, long after he has lost all inspiration and when his work has become dull and routine; pure only in that it has no foreseeable application.As a result of this early indoctrination in the universities, many young men, joining the staff of one of the agricultural research institutes, consider it almost a right that they should continue to select their own problems, seeking knowledge for its own sake, but keeping a close eye on the personal reputation to be gained from a steady flow of published papers. Nor can they be blamed for this attitude to their work; the scales are heavily weighted in favour of a worker who makes even a moderate showing in this type of research. When I graduated, just before the First World War, I consulted my professor about the career I should follow in chemistry, expressing a desire to undertake research with the hope of later finding a place on the staff O F a university.I was fortunate in holding one of the very few post-graduate awards available and hence I felt in a position to contemplate this course. My professor agreed that I should try my hand at this very difficult game, but then went on to issue a warning. Only a few, he said, of those who started on a university career could ever hope to gain a university chair and the rest could look forward to a poor financial reward. I should, he explained, be gambling on having the necessary ability and luck to obtain one of the plums of the profession. If, on the other hand, I were prepared, after a year’s training in research or in one of the branches of analytical chemistry, to go into industry or into a consulting practice, I might well, if I reached the top, earn more than a professor and, if I proved to have no more than average ability, a much better income than mediocrity received in a university.He mentioned no other openings than a university where a career in pure research could be followed for the good reason that there was virtually none. Although to-day the biggest financial rewards are still to be obtained in the higher posts in industry, the average research worker is at least as well paid in a government research institute as he is in industry, and probably better. The system whereby a man receives regular increments and promotion, provided. he works steadily and is competent, gives him certainty of earning a reasonable salary; whilst if he shows himself above average he can win more rapid promotion and a final salary roughly comparable with that of a correspondingMay, 19561 AGRICULTURAL RESEARCH 279 post in a university.In producing evidence of a man’s contribution to scientific knowledge when he is to be considered for early promotion, it is much easier to make a case on the basis of published papers arising from fundamental studies than it is on work directed to the solution of applied problems, which may often be unsuitable for publication in a scientific journal. As a result, the man working on fundamental problems of his own selection has a somewhat better chance of early promotion. Thus, both personal interest and financial advantage now weigh in favour of the choice of fundamental research, with the result that increasing numbers of workers in agricultural research wish to concentrate on this type of investigation.Of the men doing so, many are not able to maintain the flow of new ideas and self-engendered enthusiasm needed for success and, after a time, their work loses its value. They may still be very capable scientists, but they require a stimulus from without to keep them going at full pitch. There has, therefore, perhaps been a tendency to get the work on agricultural research out of balance by favouring fundamental studies too much and by continuing to give encouragement to men on this class of work when they might be more usefully and happily employed on applied problems. We must, therefore, in the next few years, give careful con- sideration to this question of maintaining a correct balance between fundamental and applied work and find a means whereby those with real ability to evolve new principles and techniques and to seek the basic knowledge we need are permitted to do so and fully rewarded, whilst at the same time we encourage equally by suitable financial advancement the larger number of workers to concentrate on the solution of applied problems, to which they are more fitted.We may draw confidence for such a course from a study of Bernard Dyer’s work. He would, I am sure, never have claimed that he was doing more than solve problems for his clients, yet from his work has come most of our methods of soil analysis; to-day much of the work of this type is classed as fundamental research to be carried out only as a matter of personal inspiration.Surely we have given to much honest professional chemistry an air of mystic inspiration that is entirely unjustified. It would be just as reasonable to assume that the same qualities of mental exaltation were required to write a Times leader and, say, an ode of Keats. So far I have discussed only the problem of men, because it is much the most important, but even the most brilliant man must have a building in which to work and equipment to use. Since the war, there has been an alarming rise in the needs of all types of workers for apparatus and equipment. It is not the same apparatus that is costing more; it is an entirely new range of instruments that is called for. A new technique such as chromato- graphy has its special demands; the centrifuge must now work faster and be refrigerated; there must be ultra-violet and infra-red spectrophotometers ; and the humble hand calculating machine has given way to a complicated electrically operated machine, which in turn will soon be followed by an electronic computor.Whilst we may all be convinced of the need to give full financial support to research as the soundest investment the nation can make, the very high cost of equipment must make us think carefully to see that when it is provided it is fully and properly used and that we do not purchase some expensive gadget for no other reason than that a rival laboratory already has one and some day we may have a use for it. We may, for example, ask ourselves whether some pieces of equipment can be provided in more than one or two laboratories and hence whether work requiring their use should be concentrated there.The traditional approach to this problem has been to provide equipment whenever the work of an institute seemed fully t o justify it. There must, however, be a limit to this, depending on the relative costs of the instrument and its servicing as compared with the salaries of the workers. Before the war, it rarely happened that a single instrument cost more than a fraction of the annual salaries then paid to those who were to use it, and called for little in the way of annual servicing. Now is is not unusual to find a small group of scientists with total salaries of, say, k3500 per annum, who want an instrument or instruments for the further development of their work, costing ,ElO,OOO or more and requiring in the wages of technicians and other charges E2000 to ;63000 per annum for its servicing.The same equipment may already be available in another laboratory financed from the same source. If it is, we must ask ourselves whether it is already fully used and, if not, whether the group now asking for duplicate equipment cannot also use it. The one is produced, the other happens. The efficient use of expensive equipment raises a number of difficult issues.280 SLATER: THE EVOLUTION OF [Vol. 81 It may well be that the apparatus is so far used only for relatively short periods by the one group and could easily meet the needs of the other, but it is rarely possible to arrange for such co-operation. The second group is inevitably at the other end of the country, and even if they could be directed to move to the laboratory where the required apparatus is available, there are always a dozen reasons why this move cannot be made.The laboratory invariably has no space for their other wo’rk, which has to be carried on apart from the need for special apparatus. They will certainly require other expensive equipment which is only provided in the laboratory where they now are, and if the scientists can be moved the laboratory technicians certainly cannot.. The last argument is unanswerable, because nowadays no scientist appears to be able to work without at least one technician with specialised training. In agriculture, we have a difficult pro‘blem in providing large-scale facilities for work on farm animals, particularly where this involves the isolation of sick animals.The farming organisation to grow the food and manage the stock for large numbers of stall-fed animals is complex, and, unless it is highly efficient, the costs become prohibitive. Institutes for this type of work must of necessity be limited to one or two and be situated in the country, away from large urban populations; much of our veterinary research is carried out in universities and research institutes where the facilities for keeping animals under controlled conditions are limited and have to be shared between numbers of workers with many different interests. Investigations which it is not anticipated will call for many animals have a habit of developing, for their successful conclusion, the need for much larger numbers.The statement that “to obtain a statistically significant result two groups with not less than twenty (or may be thirty) animals in each will be required” is all too well known. But here again we have the problem of Mahomet and the Mountain, the worker responsible for the experiment cannot go to the animals and we cannot move the animals to the worker. Ideally, each worker should have the animals he requires provided near his laboratory, but, quite apart from the prohibitive cost of such a plan, it would be grossly wasteful, and often would be impracticable because the necessary land and staff were unobtainable. So far no solution has been found to this problem, but it seems probable that in the end the worker, finding that the experimental farm and its animals are immovable, will decide that he must himself go to this particular mountain.All that can be done at present is to make this journey as easy as possible. The need to make it will continue to grow without our intervention if the cost of providing these facilities goes on rising more rapidly than the funds available. A comparison of the programmes of research being undertaken before the war and now shows the great increase in the complexity of the work and the marked degree in which it is fragmenting into more and more separate and highly specialised branches. As an example of this development, the control of weeds in growing crops will serve well. For more than fifty years attempts have been made to use chemical sprays to kill weeds, whilst damaging the affected crops as little as possible; but up to the outbreak of the Second World War they had not progressed very far.Some success had been achieved, depending largely on differences in physical character between the crop and the weeds; thus onion crops were sprayed with sulphuric acid, which ran down the narrow, smooth vertical leaves but remained on the broad flat leaves of many of the invading weeds. During the war chemists and plant physiologists in the laboratories of Imperial Chemical Industries at Jeallott’s Hill, at the Rothamsted Experimental Station, and later at Oxford, studying the chemistry and mode of action of plant hormones, evolved the idea of using related substances as selective herbicides, and from this work has arisen the whole range of substituted phenoxyacetic acid compounds now widely used on our farms.These discoveries at the same time opened up a wide series of new problems for investigation. The chemist was concerned in the synthesis of different series of organic compounds related in structure to the substances known to affect plant growth in different ways. The biochemist and the plant physiologist were interested in the mode of action of these substances and in such questions as their translocation in the plant. A range of biological tests had to be developed for the study of the activity of growth-regulating substances, and of chemical tests to deter- mine how long they took to disappear from the plant or the soil. The bacteriologist was involved in investigating the ways in which micro-organisms break down these compounds.New field techniques have had to be worked out by the botanist and statistician to measure the efficiency of the different herbicides in destroying weeds and their effect on the yieldMay, 19561 AGRICULTURAL RESEARCH 281 and quality of the different crops in which the weeds were growing. The same team of workers had also to study the effects of treating crops and weeds at different stages of growth and the impact of such factors as the type of soil, the nutritional status of the crop, the crop variety and the local climatic conditions on the efficiency of the herbicide. With the help of a chemist, they had to study the formulation of the solutions used for spraying and how the different solvents and diluents affected the efficiency of the active compound.The possibility of applying radioactive-tracer techniques to these problems meant that before long the chemists and physicists skilled in this work arrived with their specialised needs in laboratories and equipment. In the latest developments coming from the Agri- cultural Research Council Unit at Wye College, a study of the enzymic breakdown of non-toxic substituted phenoxybutyric and other phenoxyaliphatic acids to the toxic phenoxyacetic compounds has shown that it is possible to prepare compounds of specific molecular structure effective only against plants containing the enzyme system capable of reacting with them. The further exploitation of this concept must take us much further into the biochemistry of plant enzymes and all the related problems of plant growth.This illustration from a small but important section of agricultural research serves. to show how each part of the work is calling for an increasing number of specialists. It cannot be expected that all these men will be interested in practical farming and able to relate the small field in which they work to the broad general problems of agriculture. Many of the scientists required come from an urban background and until they join an Agricultural Research Institute they may have little or no knowledge of farming, let alone have given thought to its technical problems. It has been suggested that the institutes should recruit only men with a farming, or at least a country, background, but that is impossible.When a biochemist is needed with a good knowledge of, say, protein chemistry and capable of undertaking individual research, the field of selection is small enough, without imposing on it the further qualification of a rural upbringing. We should make very slow progress if we confined our efforts in this way. As in the future our laboratories employ greater numbers of these specialised research workers, the need for men who can bridge the gap between them and the farmer becomes increasingly important. I have already mentioned the work these men must do and the qualities required for this work and I want now to return to the consideration of the type of training they need; or, put another way, where we should look for possible recruits.The most obvious place is in the agricultural schools of the universities. An examination, however, of the courses of study followed for the agricultural degrees does not suggest that, in general, they will produce the type of man we need. The curriculum in agriculture attempts to cover an extremely wide range of subjects, so that the student’s time is filled with attendance at lectures and practical classes. He must study chemistry, physics, botany and zoology, and the applied aspects of these sciences; he is required t o learn something of economics, accounting, land agency and building construction; in addition, he must acquire knowledge of crop and animal husbandry, which includes such diverse subjects as the management of farm machinery and the care of sick animals.The curriculum is not the same in each university, but in most schools of agriculture all the above subjects are covered and in many there are others in addition, arising from the special interests of the staff. If the students entering the course were outstanding men, it would still be impossible to use such a wide range of subjects as the proper basis for training in scientific method. Agriculture is in most universities one of the few remaining pass-degree courses and unless a man is determined to follow it he will, if he has shown the necessary ability, tend to be diverted to an honours school. Although in doing so his tutors may be directing him wisely, the result is to drain away many of the best university entrants from agriculture. Whilst there are outstanding exceptions of men who have achieved distinction in research work after graduating in agriculture, it is true that most agricultural graduates have not the basic training in science to enable them to take up a research career.They cannot in the time at their disposal have mastered any one scientific discipline and they certainly cannot have spent the hours in the laboratory which alone can lead to a mastery of its techniques. Whilst the agricultural graduate may be well able to talk to the farmer about his problems and to draw the scientist’s attention t o them, he is unlikely to be able to appreciate the laboratory problems involved, or exactly how the specialist scientist is, or should be, attacking the problem. He is equally unlikely to keep closely enough in touch with academic work to be able to recognise the importance282 SLATER: THE EVOLUTION OF [Vol.81 to the farmer of a discovery made in the laboratory, when the specialised originator of the idea has not done so. There are many openings for which the agricultural graduate is well qualified, but apart from the exceptional man, he is not suited to uphold the interests of agriculture in an institute increasingly staffed by specialists. What is required is the type of man entering agricultural research before the Second World War who, as I have said earlier, did so because of a strong desire to apply his knowledge and skill in one of the basic sciences to the practical problems of agriculture. Some such men do come from farming stock; the small farms of Wales and Scotland have already provided us with many of our best men of this type.Such men need little training in agriculture. Others have been fired with a desire to help in food production, by reading or hearing of the vital importance to the world of a larger agricultural output, or by coming by chance on some interesting application of their science to an agricultural problem. This group of recruits must, if they are not to become narrow specialists, be given the opportunity to get a general knowledge of farming. One way is to send them to take a post-graduate course in agriculture, such as that given in Cambridge; the other is to ensure that when they first join a research institute they are given problems which will take them on to farms, where they will acquire a general knowledge of agriculture.It is surprising how quickly, for example, a chemist, if he is the right man, will pick up a good general knowledge of farming. We need go no farther than the man we honour to-day and to your first Memorial Lecturer to find outstanding examples of chemists whose names will live long in the history of agriculture. The National Agricultural Advisory Service provides a wider illustration of the value of this type of training and of how well it fits a scientist to act as intermediary between the laboratory specialist and the farmer. The specialist advisory officers in such subjects as soil and nutrition chemistry, entomology and plant pathology are recruited from men who have taken chemistry, botany or zoology as their first-degree subject.Some have followed this by taking the diploma in agriculture or that in agricultural science at Cambridge, but others, after a preliminary period of research training in a university, have been taken directly into the service. There they get every opportunity to visit farms in company with the district and county officers, who have been selected for their knowledge and experience in agriculture and horticulture. Within a remarkably short time the specialist officer picks up a general knowledge of the industry. He can never know so much about the practical details of farming as his colleagues who have taken an agricultural degree, but he can apply his scientific knowledge and training to answer the unusual questions which arise on the farm.He may not be able to set a plough or milk a cow, but he can put the farmer right on the fertilisers to use or the rations to feed to stock, where traditional practice has broken down. There is no doubt that this group of scientists is highly respected and valued by the farmers. At the same time their training enables them to talk freely and easily with the specialist worker in a research institute and to carry out themselves investigations generally of an applied character. These men are clearly of the type required to form the bridge we are seeking to build, but they are too few in number and have -too many other duties to complete it. What is needed is another span, formed of similar men based on the research institutes. There are still in our institutes many men with this training, and between them and the specialist advisory officers there is close co-operation.The proportion of research workers with a general knowledge of agriculture is, however, falling and, unless we make a conscious effort to increase it and make liaison with the Advisory Service a definite part of their duties, our span of the bridge may collapse. All branches of agriculture are not equally well covered in the National Agricultural Advisory Service with scientifically trained specialists and in those where this scientific training is lacking lies the greatest danger of the laboratory and the farm parting company. The advisory officer not having a sound scientific training avoids contact with the scientist he does not understand and who does not understand him. The research worker, for his part, finding no response to proposals for the application of his specialised knowledge, tends to withdraw into his laboratory and concentrate more and more on fundamental research. I t is in these branches that the research institutes will have to make the greatest efforts t o find men with sound scientific training and a general knowledge of agriculture.May, 19561 AGRICULTURAL RESEARCH 283 Looking into the future we see, therefore, two groups of men working together in the agricultural research institutes, both having their roots in the basic sciences, but applying their knowledge in different ways; the one group going ever deeper into specialised investi- gations in the laboratory and the other devoting itself to the immediate solution of the applied problems of the industry and maintaining contact with the Advisory Service and the farmers. The qualities of Bernard Dyer of which I spoke at the beginning-his ability to grasp the essentials of a practical problem, to state it clearly and simply and to apply his knowledge of chemistry to its solution-are qualitites that will be called for more and more in the future development of agricultural research, and your Society is doing a service to the advancement of agriculture, which Dyer loved so much, by making us pause and think of what he did and what he stood for, when this Memorial Lecture is delivered.

ISSN:0003-2654    

DOI:10.1039/AN9568100276

出版商:RSC    

年代:1956

数据来源: RSC

摘要:

May, 19561 AGRICULTURAL RESEARCH 283 Investigations into Methods of Determination of Lithium in Its Ores BY P. W. SYKES Certain methods for the analysis of lithium ores have been examined It is concluded that the most accurate and the errors in them determined. method is the Berzelius attack followed by flame photometry. THE Lawrence Smith methodl for the decomposition of silicate minerals and the isolation of the alkali metals as chlorides has, for many years, been used in the determination of lithium in its ores. It has been critically investigated by Kallmann2 and other workers, but on the whole it has stood the test of time. The other classical method of decomposition of silicate ores is that of Berzeli~s,~ but his has found little favour since the introduction of the Lawrence Smith method, because of difficulties in the chemical separations involved in the isolation of the alkali metals.It was, however, used by Bacon and Sparks4 for the analysis of spodumenes, the lithium being determined by the periodate method, and by Ellestad and Horstman5 in the determination of small quantities of lithium in silicate rocks, use being made of flame photometry. Numerous methods of separating lithium from the other alkali metals have been proposed, but those based on the isoamyl alcohol method of Gooch6 or the ether - ethanol methods of Rammelsberg7 and of Palkin* appear to have been most widely used. The methods have been summarised by F o r ~ t e r . ~ The flame photometer has permitted the determination of lithium in solution to be carried out with ease and accuracy and without the necessity for separating it from the other alkali metals.I t has been used by Brumbaugh and Fanuslo for the determination of lithium in spodumene, after attack on the ore by the Berzelius method. The flame photometer has proved most useful for the determination of small quantities of lithium in residues that are normally discarded. With its aid both the Lawrence Smith and the Berzelius methods have been investigated as means for getting the lithium contents of ores into solution. In addition, the effectiveness of a conventional ether - ethanol method for the separation of lithium from the other alkali metals has been investigated. ORES The most important ores containing lithium, most of which have been examined in this investigation, are as follows- Amblygonite .. . . Li A1 (F, OH) PO, Triphylite . . . . Li (Fe, Mn) PO, Lepidolite . . . . K Li Al, (Al,Si,Olo) (F, OH), Zinnwaldite . . . . K Li Fe A1 (A1Si,Ol0) (OH), Spodumene . . . . Li A1 (SiO,), Petalite . . .. . . (Li, Na, H) A1 (Si,OJ,284 SYKES: INVESTIGATIONS INTO METHODS OF [Vol. 81 The ore is heated with a mixture of six parts of calcium carbonate and one part of ammonium chloride, and the sinter is cooled, digested with water and filtered. The water extract is acidified, boiled to remove carbon dioxide, and calcium is precipitated with ammonium hydroxide and ammonium carbonate. The solution is evaporated to dryness and the ammonium salts are removed by heating. The solid is dissolved in water acidified with hydrochloric acid, and traces of sulphate are precipi- tated by barium chloride.The solution is made alkaline again with ammonium hydroxide, excess of barium is removed with ammonium carbonate and any remaining calcium with ammonium oxalate. The filtrate is again evaporated to dryness and ignited to remove ammonium salts. The solid is dissolved in dilute hydrochloric acid, and the solution is filtered and again evaporated to dryness. The lithium chloride is then separated from the other alkali-metal chlorides, as described by Schoeller and Powel1,ll by extraction with a mixture of one part of absolute ethanol and 3 parts of diethyl ether. The filtrate is evaporated, sulphuric acid is added, and the residue is finally dried, ignited and weighed as lithium sulphate.The E.E.L. flame photometer (Evans Electroselenium Ltd.) has been used throughout this investigation. The method used is as follows. Standardise the flame photometer (using a standard solution containing 15 parts of Li,O per million) at a reading of 60 on the linear scale. Then spray into the flame the prepared unknown solution and take the reading. Repeat this procedure five times and average the readings. From a calibration graph obtained by spraying solutions of known concentration in to the flame, the concentration of the unknown may be determined. The standard deviation in the determinaiion of the lithium content of a solution contain- ing about 15 parts of Li,O per million was determined experimentally to be about 5 parts in 1000, provided that the standard solution was sprayed into the flame before and after each determination of the unknown.It has been found that the highest accuracy is obtained by using the centre portion of the instrument scale, and in most cases the concentrations of the unknown solutions were adjusted to give readings in this region. CRITICAL EXAMINATION OF THE COMBINED LAWRENCE SMITH AND THE LAWRENCE SMITH METHOD The method used is briefly as follows. FLAME PIHOTOMETRY The instrument has been described by Collins and Polkinhorne.12 ETHER - ETHANOL METHOD Various reports have from time to time appeared that the lithium is not completely liberated and rendered soluble in water by the Lawrence Smith attack, but it has always been considered that , if the extracted residue (consisting of calcium carbonate and the water- insoluble components of the decomposed ore) is completely soluble in concentrated hydro- chloric acid, the attack is complete.It was however found that, after 0.5 g of a finely ground sample of petalite had been heated with 3.5 g of Lawrence Smith mixture, in accordance with what had been the usual practice, a considerable quantity of lithium was not leached out of the sinter by water, although the leached residue fulfilled the condition of complete solubility in concentrated hydrochloric acid. Increasing the quantity of mixture to 7 g for 0.5 g of ore markedly increased the amount of lithium extracted. The increase in the amount from samples of other ores was small, as shown in Table I. TABLE I DETERMINATION OF Li,O IN ORES BY COMBINED LAWRENCE SMITH AND ETHER - ETHANOL METHOD, DIFFERENT AMOUNTS OF LAWRENCE SMITH MIXTURE BEING USED Li,O found when 3-5 g of mixture used, Li,O found when 7 g of mixture used, Ore % % Amblygonite A . ... 7.40, 7.35 7-45 Lepidolite H .. .. 3.73, 3-71 3.77 Lepidolite J . . .. .. 3.75 3.75, 3.75 Amblygonite B . . .. 8.48, 8-43 8.48 Petalite . . .. .. 3.42, 3.46 4*06,4*08May, 19561 DETERMINATION OF LITHIUM IN ITS ORES 285 But even with use of the increased amount of mixture, it has been shown that extraction of lithium is not complete. Eight water-insoluble residues from Lawrence Smith attacks (each with 7 g of mixture) on several samples of lepidolite were tested for residual lithium content. With every residue, a small but appreciable amount of lithium was extracted either by reheating the dried residue from the Lawrence Smith attack with ammonium chloride and re-extracting with water, or by dissolving the residue in hydrochloric acid and evaporating to dryness to precipitate silica.In each case the calcium was precipitated by ammonium carbonate, redissolved and reprecipitated before the lithium was determined in the solution. The smallest amount of lithium extracted corresponded to about 0-03 per cent. and the largest to 0.08 per cent. of Li,O in the ore. Similarly, six residues from attacks on ambly- gonite have been examined and lithium has been found to be present in every analysis in amounts corresponding to 0-05 to 0.085 per cent. of Li20 in the ore. The fineness of grinding of the ore sample can also affect the amount of lithium rendered water-soluble by the Lawrence Smith attack.A sample of triphylite that had been ground through a 100-mesh sieve was analysed for lithium by the Lawrence Smith attack, followed by flame photometry. Values of 4.25 and 4-58 per cent. of Li20 were obtained. The same sample after further grinding gave a value of 6.34 per cent. of Li20, and by the Berzelius attack followed by flame photometry, 6-43 per cent. of Li20. PURIFICATION STEPS- Two residues, which should be free from lithium, are rejected at the purification stage. The first consists of calcium carbonate, which has been redissolved and reprecipitated to ensure that it carries away no lithium. In fact, whenever such a residue was examined, the lithium content, although detectable, was quite insignificant.The second residue consists of barium sulphate, barium carbonate, calcium carbonate and calcium oxalate, and is quite small. Several such residues have been examined, and by redissolving (as f a r as possible) in acid and reprecipitating, lithium corresponding to between about 0.005 to 0.015 per cent. of Li,O in the ore was extracted. During this stage of the analysis, ammonium salts are twice removed by evaporation to dryness and ignition. The temperature of the material must barely reach a very dull red heat, or lithium chloride may be lost by volatilisation. In the second ignition the lithium may be partly present as lithium oxalate, and an incomplete extraction in the next stage will occur if this oxalate is not completely decomposed by heat.A temperature considerably above that required to volatilise the ammonium salts is necessary, but something less than a dull red heat is sufficient. EXTRACTION OF LITHIUM- Six residues from lepidolite analyses have been examined; lithium was detected in all, The amount was small (corres- ponding to between about 0.01 and 0.016 per cent. of Li,O in the ore) except in one residue, with which the temperature of ignition in the purification stage was insufficient to decompose lithium oxalate, when the amount found was equivalent to 0-63 per cent. of Li20 in the ore. With amblygonites, in which the ratio of lithium to other alkalis is very much higher, the lithium content of these residues was negligible. A number of samples of the lithium sulphate directly derived from such solutions has been examined.The lithium, sodium and potassium present in each were determined by means of the flame photometer; the results of a fair selection of these are given in Table 11. In all cases small amounts of sodium and potassium are weighed and appear as Li20 in the result of the analysis. Calcium also has been detected in the final lithium sulphate in small quantities by spectrographic examination, but the actual amount present has not been determined. The extracted residue-This should be free from lithium. The ether - ethanol extract-This should be free from all metals except lithium. THE LAWRENCE SMITH ATTACK FOLLOWED BY FLAME PHOTOMETRY INITIAL TREATMENT OF THE ORE- Losses incurred by the failure of the Lawrence Smith procedure to extract the whole of the lithium from the ore have been described above.The following method was used for the determination by flame photometry of the lithium in the solution resulting from the286 SYKES: INVESTIGATIONS INTO METHODS OF [Vol. 81 Lawrence Smith attack. Acidify the aqueous extract from the Lawrence Smith sinter with hydrochloric acid until just red to methyl orange, and make up to 500ml. Heat 25ml almost to boiling and add a 25 per cent. solution of ammonium carbonate dropwise until :rABLE 11 DETERMINATION OF LITHIUM IN THE ETHER - ETHANOL EXTRACT Equivalent Li,O in ore Accepted values from flame-photometric determination of from weight I A \ Ore of Li,SO,, lithium, sodium, potassium, % % % % Lepidolite G . . . . 3-97 3.88 0.042 0.02 1 Lepidolite H .. .. 3.93 3.88 0.042 0.017 Lepidolite J . . .. 3.75 3.73 0.024 0.0 15 Lepidolite K . . . . 3.32 3.35 0-038 0.023 Amblygonite C .. 9.07 8.98 0.035 trace Total of flame- photometric figures , 3.94 3.94 3.77 3.41 9.01 % no more calcium carbonate is precipitated. Set aside for a few minutes, and then filter off the precipitate and wash it. Cool the solution and make it up to either 100 or 200m1, depending on the expected Li,O content of the ore. Use this solution for analysis by the flame photometer as described. No clear evidence has been obtained that a significant loss of lithium occurs by the use of this procedure in place of the double precipitation of calcium carbonate normally used in the Lawrence Smith procedure. INTERFERENCE OF OTHER ELEMENTS ON THE DETERMINATION OF LITHIUM BY THE FLAME A feature of the Lawrence Smith attack is the virtual absence from the leach solution of constituents of the ore other than the chlorides of the alkali metals and calcium.Since the last named is removed by precipitation before carrying out the determination, only the alkali metals have to be considered. Sodium chloride does not interfere at any concentration investigated-the highest was about 100 times that normally obtained in a Lawrence Smith leach solution, and was over 30 times the Li,O concentration. The effect of potassium chloride is shown in Table 111, and of rubidium chloride in Table IV. PHOTOMETER- TABLE I11 EFFECT OF POTASSIUM CHLORIDE ON DETERMINATION OF LITHIUM BY FLAME PHOTOMETRY Equivalent Potassium Equivalent Li,O present, chloride added, Li,O found, Error, p.p.m.p.p.m. p.p.m. % 15 20 15.12 + 0.8 15 40 15.16 + 1.1 15 100 15.27 + 1.8 15 200 15.32 + 2.1 15 500 15-51 + 3.4 0 40 5 40 5-28 + 5.6 10 40 10.30 + 3.0 15 40 15.18 + 1.2 20 40 20.10 + 0.5 - 0.1 - TABLE IV EFFECT OF RUBIDIUM CHLORIDE ON DETERMINATION OF LITHIUM BY FLAME PHOTOMETRY Equivalent Rubidium Equivalent Li,O taken, chloride added, Li,O found, Error, 15 20 15-05 + 0.3 15 40 16.1 1 + 0.7 15 100 15.18 + 1.2 p.p.m. p.p.m. p.p.m. %May, 19561 DETERMINATION OF LITHIUM I N ITS ORES 287 The potassium contents of a number of solutions from lepidolite analysis have been determined by means of the flame photometer; owing to the emission by rubidium of a red light fairly close in wavelength to that of potassium, the resulting figure includes a proportion of the rubidium.However, the composite figure was nearly constant for a number of different samples of lepidolite and is consistent with an ore content of about 9 per cent. of K,O and 3 per cent. of Rb,O, giving a solution for analysis containing about 10 p.p.m. of Li,O, 35 p.p.m. of KC1 and 10 p.p.m. of RbCl. From Tables I1 and I11 it will be seen that, as a result of the presence of the potassium and rubidium salts, the lithium content as determined by the flame photometer will be about 3 per cent. high. This error can be eliminated by including the appropriate concentration of potassium and rubidium chlorides in the standard with which the unknown solution is compared. Provided they are not too large, variations in the potassium and rubidium contents will not produce any serious error in the lithium determinations.With amblygonite, which normally contains only very small quantities of alkalis other than lithium, no correction is necessary, provided that the calcium has been removed. BERZELIUS ATTACK FOLLOWED BY FLAME PHOTOMETRY The details of the Berzelius attack are based on a method worked out by Messrs. Alfred H. Knight and are described later. Briefly, the ore is heated with hydrofluoric and nitric acids until it has dissolved. Ideally the whole of the constituents of the ore (with the exception of silicon, which escapes as silicon tetrafluoride) are obtained in solution, and are then converted to sulphates by reaction with an excess of sulphuric acid. In practice, with lepidolite a small residue that stubbornly resists the attack is always found, and is presumably of different composition from the bulk of the ore.No trace of lithium has been detected in the solution resulting from the repeated extraction of this residue with hydrofluoric and sulphuric acids. The solution containing the lithium as lithium sulphate is then analysed by flame photometry. Since practically the whole of the ore is obtained in solution, the possibility of the loss of lithium in the residue is excluded, and for this reason the method has much to recommend it, but the presence of the other constituents of the ore increases the possibility of error due to interference with the flame-photometric determinations. TABLE V Equivalent Li,O present, p.p.m.10 10 10 10 10 10 Equivalent Li,O present, p.p.m. 10 10 10 10 10 10 0 5 10 15 20 25 INTERFERENCE OF ALUMINIUM Aluminium oxide added, p.p.m. 0 20 40 60 80 100 Concentration of sulphuric acid, N 0.32 0-32 0.32 0-32 0-32 0.32 Equivalent Li,O found, Error, 9.65 - 3.5 9.65 - 3.5 9-65 - 3-5 9.7 - 3 9-65 - 3.5 9.7 - 3 p.p.m. % INTERFERENCE OF SULPHURIC ACID Aluminium oxide added, p.p.m. 60 60 60 60 60 60 60 60 60 60 60 60 Concentration of sulphuric acid, N 0.0 0.16 0.32 0.40 0.48 0.64 0.32 0-32 0-32 0.32 0-32 0.32 Equivalent Li,O found, p.p.m. 10.05 9.8 9.75 9.65 9-6 9.5 0 4.9 9-8 14-55 19.45 24.4 Error, + 0.5 - 2 - 2.5 - 3.5 - 4 - 5 - 2 - 2 - 3 - 2.5 - 2.5 % -288 SYKES: IIWESTIGATIONS INTO METHODS OF [Vol. 81 That due to the other possible interfering substances is given in Tables V, VI and VII.All results are average of 5 readings. The interference due to the other alkali metals is mentioned above. TABLE VII INTERFERENCE OF PHOSPHORIC ACID I Equivalent Equivalent Equivalent >i,O present, P,O, added, Li,O found, Error, p.p.m. p.p.m. p.p.m. % 15 79 . 14.95 - 0.5 15 226 14.8 - 1 15 565 14-75 - 1.5 15 1130 14.35 - 4.5 I t will be seen that aluminium has no interfering effect at the relevant levels, and that sulphuric acid has a definite depressing effect on the lithium emission. (It is the sulphuric acid that causes the error in Table V.) In practice these effects are allowed for as shown in Table VIII by the addition of potassium, rubidium, sulphuric acid and phosphoric acid to the lithium standards in amounts depending on the ore being analysed and the method of attack used.Phosphoric acid has a small depressing effect. TABLE VIII ADDITIONS REQUIRED TO LITHIUM STANDARDS Lawrence Smith attack- KC1 RbCl g p.p.:rn. of Li,O p.p.m, p.p.m. Ore Sample weight, Lithium standard, required, required, nil nil nil nil nil nil Amblygonite . . 0.5 Lepidolite Berzelius attack- 0.5 52.5 15 35 10 17-5 5 All standards contain 25 ml of 50 per cent. w/w sulphuric acid per litre p20, g p.p.m. of Li,O p.p.m. Ore Sample weight, Lithium standard, required, 79 53 { :! 26 nil nil nil Amblygonite . . 0.15 Lepidolite . . 0.3 K2SO4 Rb,SO, required, required, p.p.m. p.p.m. nil nil nil nil nil nil 63 16-0 42 10-7 21 5.3 These figures in- this Table are based on- (a) ( b ) amblygonite, 9 per cent. of Li,O; 47 5 per cent.of P,O,; lepidolite, 4 per cent. of Li,O; 9 per cent. of K,O; 3 per cent. of Rb,O. The interfering substances (with the exception of sulphuric acid) are assumed to vary in proportion to the lithium content. A comparison of results obtained on the same ore by all three methods investigated is given in Table IX. Many determinations were conducted on amblygonite C because of the discrepancies between the results of the earlier analyses. The reason for these discrepancies has not been discovered; all that can be said is that the differences confirm the view that the Lawrence Smith ether - ethanol method is not the most reliable for lithium determinations. The Lawrence Smith method followed by flame photometry also suffers from the disadvantage that the attack does not get all the lithium into solution.It is therefore concluded that the Berzelius attack followed by flame photometry is the most accurate (and incidentally the most rapid) method for the determination of the lithium content of ores. A detailed description of this method follows.May, 19561 289 DETERMINATION OF LITHIUM I N ITS ORES TABLE IX COMPARISON OF RESULTS All figures are expressed as percentage of Li,O in the ore Column A. Accepted values from weight of lithium sulphate. Column B. Values from lithium content, determinkd by flame photometer. of lithium sulphate. Column C. Total known loss in residues; ether - ethanoi method: Column D. Value by flame photometer after Lawrence Smith attack. Column E. Known loss in residues, flame-photometer method. Column F.Value by flame photometer after Berzelius attack. Lawrence Smith attack A r \ Ether - ethanol A r 3 Ore A Lepidolite G Lepidolite H 3.99 8.61 8.54 8.61 9.05 9.00 9.33 9-07 9.23 8-32 8.29 Amblygonite D . . { Petalite . . Spodumene .. 5.65 B 3.87 3.76 3-88 3-29 3-85 8.50 8.69 8.57 8.55 8-94 9.19 8-98 9.1 1 - - - 8.15 7.67 7.56 - - - C 0.10 0.06 0.65 0-08 0.08 0.06 0-09 - - - 0.06 0.06 0.06 - - - - - I - - - Sum'of B and C 3.86 3.94 3.94 3.93 8.58 8.75 8.66 - - - 9.00 9.04 9.17 I - - - - - I - - Flame photometry D 3.88 3.77 3.77 8-90 9.10 9.05 9.05 9-21 9-17 9.23 9.13 8.67 8.62 8-11 8.13 4-25 4-24 6.98 - - - - Sum'of E D a n d E - - 0.03 3.91 0.07 3.84 - - - - - - 0.06 9.23 0.06 9.29 0.05 9.18 - - Berzelius attack F 4.03 3-98 3.89 3-9 2 9.25 9.32 - - - - - - - - - 8.70 8.25 4-20 4.16 6.04 - - METHOD The method is intended for use with the E.E.L.flame photometer, and is not necessarily suitable for instruments of other makes. REAGENTS- Sulphuric acid, 50 per cent. w/w, sp.gr. 1.400. Phosphoric acid, dilute-Dilute 2 ml of phosphoric acid, sp.gr. 1.75, to 1 litre with distilled water. Potassium sul$hate - rubidium sulphate solution-Dissolve 0.1 67 g of AnalaR potassium sulphate and 0.043 g of rubidium sulphate and make up to 200 ml with distilled water. Lithium sul@hate containing 4000 $.p.m. of Li20 (A)-Weigh out 4.946 g of pure lithium carbonate (dried for Q hour at 110" C) and wash it into a 300-ml conical flask with a funnel in the neck. Add slowly through the funnel 27.4 ml of 5 N sulphuric acid, and gently boil the solution until all the carbonate has dissolved and the carbon dioxide has been driven off.Cool, transfer to a 500-ml cali- brated flask, add 25 ml of mercuric chloride solution (10 p.p.m.) and make up to the mark with distilled water. Lithium sulj5hate containing 200 p.j5.m. of Li,O (B)-By pipette put 25 ml of lithium sulphate solution A into a 500-ml calibrated flask, add 25 ml of mercuric chloride solution (10 p.p.m.) and make up to the mark with distilled water. Working standard containing 15 $.P.m. of Li20-(a) For lepidolite analysis: take 15 ml of lithium sulphate solution B, 15 ml of potassium sulphate - rubidium sulphate solution and 5ml of 50 per cent. w/w sulphuric acid and make up to 200ml with distilled water. Add distilled water to a total volume of 100 to 150 ml.290 SYKES : INVESTIGATIONS INTO METHODS OF [Vol.81 (b) For amblygonite analysis: take 15 ml of lithium sulphate solution B, 7 ml of dilute phosphoric acid solution and 5 ml of 50 per cent. w/w sulphuric acid and make up to 200 ml with distilled water. Working standard containing 10 9.p.m. of Li,O-(a) For lepidolite analysis: take 10 ml of lithium sulphate solution B, 10 ml of potassium sulphate - rubidium sulphate solution and 5 ml of 50 per cent. sulphuric acid and make up to 200 ml with distilled water. (b) For amblygonite analysis: take 10 ml of lithium sulphate solution B, 4.7 ml of dilute phosphoric acid solution and 5 ml of 50 per cent. w/w sulphuric acid and make up to 200 ml with distilled water. Certain of the standard solutions are made up to contain about 0.5 p.p.m.of mercuric chloride in order to prevent the growth of moulds, which interfere with the smooth performance of the atomiser. PROCEDURE FOR SOLUTION OF THE ORE- The approximate weight of ore required is 0-15 g if the Li20 content is 8 to 9 per cent. and 0.3 g if the Li,O content is about 4 per cent, Grind rather more than the required xmount of ore in an agate mortar until no gritty pieces are perceptible. Weigh out the required quantity of this ground sample in a platinum dish. Add about 10 ml of 40 per cent. AnialaR hydrofluoric acid and 5 ml of concentrated nitric acid and evaporate t o dryness on a water bath in a fume-chamber. Add about 5 ml of distilled water and evaporate to dryness. Repeat the treatment with hydrofluoric and nitric acids and again evaporate to dryness.Add about 5 ml of distilled water and 10 ml of 50 per cent. sulphuric acid, and evaporate as far as possible on the water bath. Transfer the dish to a hot-plate, or heat over a small flame to drive off the sulphuric acid to dryness. The heating should not be sufficient to cause loss by spitting or by creeping of the contents over the edge of the dish. Add about 10 ml of water and 25 ml of 50 per cent. w/w sulphuric acid, and heat on the water bath (with addition of distilled water if necessary) until the solid is detached from the platinum dish. Wash out completely into a 600-ml beaker, add water to bring the volume to about 400ml and bring to the boil. Cover the beaker with a clock-glass and allow to digest on the hot-plate until solution is complete. A small insoluble residue sometimes remains when a sample of lepidolite is examined.Cool, filter into a 1-litre calibrated flask, make up to the mark with distilled water and use this solution for analysis by flame photometry. PROCEDURE FOR FLAME PHOTOMETRY- Sp:ay the appropriate 15 p.p.m. working standard solution into the flame and adjust the sensitivity control to give a reading of about 60 on the linear scale. Spray distilled water into the flame for at least 1 minute and adjust the zero. Without re-adjusting the sensitivity, take readings in succession of the 15 p.p.m. standard, the unknown solution and the 10 p.p.m. standard. Continue to take readings of the three solutions in the same order, without adjusting the sensitivity, until six sets of values have been obtained, which should be free from any pronounced drift from one series to the next.Light the flame and adjust the instrument according to the makers' instructions. If A is the reading of the 15 p,p.m. standard, B is the reading of the 10 p.p.m. standard, C is the reading of the unknown solution, and Y is the p.p.m. of Li20 in the unknown solution- C - B y == ___ x 5 + 10. A - B The average (P) of the six values for 'Y is then taken. The lithium content of the ore is given by- P 1.0 x weight of ore taken' Li,O, per cent. = -May, 19561 DETERMINATION OF LITHIUM I N ITS ORES 29 1 PROCEDURE FOR ORES OTHER THAN LEPIDOLITE AND AMBLYGONITE- For the analysis of spodumene or petalite, standards containing 10 and 15 p.p.m. of Li,O with 5 ml of 50 per cent. w/w sulphuric acid per 200 ml of solution are suitable. For the most accurate results, these ores may require special standards. I thank Messrs. Alfred H. Knight for a description of their method of attack on lithium ores, Mr. J. Hogan and Mr. R. F. Trew, who have carried out some of the analyses referred to, and Mr. L. M. Miall for his assistance in the preparation of this paper for publication. The work was carried out in the laboratories of Kemball, Bishop & Co. Ltd., to whose directors I am grateful for permission to publish these results. REFERENCES 1. 2. 3. 4. 5. 6. 7. 8. 9. Forster, C. F., Analyst, 1954, 79, 629. 10. 11. 12. Smith, J. Lawrence, Amer. J . Sci., 1871, 50, 269. Kallmann, S., Ind. Eng. Chem., Anal. Ed., 1944, 16, 712. Berzelius, J. J., Pogg. Ann., 1824, 1, 169. Bacon, F. R., and Sparks, J. T., Ind. Eng. Chem., Anal. Ed., 1945, 17, 230. Ellestad, R. B., and Horstman, E. L., Anal. Chem., 1955, 27, 1229. Gooch, F. A,, Amer. Chem. J., 1887, 9, 33. Rammelsberg, C., Pogg. Ann., 1845, 66, 79. Palkin, S., J . Amer. Chem. SOC., 1916, 38, 2326. Brumbaugh, R. J., and Fanus, W. E., Anal. Chew., 1954, 26, 463. Schoeller, W. R., and Powell, A. R., “Analysis of Minerals and Ores of the Rarer Elements,” Collins, S. C., and Polkinhorne, H., Analyst, 1952, 77, 430. Third Edition, Griffin & Co. Ltd., London, 1955, p. 44. KEMBALL, BISHOP & Co. LTD. THREE MILL LANE BROMLEY-BY-BOW LONDON, E.3 Octobev 5th, 1955

ISSN:0003-2654    

DOI:10.1039/AN9568100283

出版商:RSC    

年代:1956

数据来源: RSC

摘要:

May, 19561 The DETERMINATION OF LITHIUM I N ITS ORES Determination with the Aid of of Aluminium in Iron Chromatographic and 29 1 Steel Separation BY J. R. BISHOP The separation of aluminium from steel on a cellulose column is described, and it is shown that large amounts of iron can be removed from a cellulose column while aluminium is quantitatively retained. The aluminium is then removed by eluting with dilute acid and is subsequently determined polaro- graphically. The method is rapid, is capable of routine operation and requires only simple apparatus. The results obtained on a variety of steels are given. THE determination of aluminium in steel is difficult, the main problem being to separate small amounts of aluminium from large amounts of iron. Separations described in the literature, including precipitation of aluminium as hydroxide under controlled conditions, mercury-cathode electrolysis, cupferron precipitation and extraction of iron by organic solvents, are usually tedious and incomplete. A method of mercury-cathode electroly- sis recently published,l in which a new type of cell is used, achieves separation in a single stage and is not too time-consuming, but the cleaning and storage of relatively large amounts of mercury, when many determinations are carried out, can be a problem.In recent years metal separations by chromatography of inorganic ions have become available, and are often quicker and easier than the classical procedures. Work carried out in these laboratories2 has shown that small quantities of aluminium can be separated easily when in solution together with nickel, manganese, lead, cobalt, bismuth, copper, zinc and iron; this method was used for the determination of aluminium in tin - lead solders, after the bulk of the main metals had been removed by a preliminary treatment.Subse- quent experience showed that it was possible to remove large quantities of iron from a cellulose column while aluminium was retained ; no preliminary separation was needed. A similar292 BISHOP: THE DETERMINATION OF ALUMINIUM I N IRON AND separation, cobalt and nickel being isolated from steel, had been indicated already by Burstall, Davies and Wells,3 but this procedure seems to have been little used in steel analysis. A concen- trated solution of the steel to be analysed is applied to the top of a short cellulose column.The iron and the bulk of most of the alloying metals are removed by elution with acidified ethyl methyl ketone, and aluminium and nickel are left in the top portion of the column. The metals are then recoverable by elution with dilute acid, and the aluminium can be determined in the resulting solution after suitable concentration. The method of Willard and Dean,4 which gives a polarographic wave by the reduction of the complex formed between aluminium and an azo dye, has been found very convenient. For mild steels it could be applied directly to the eluate after evaporation and simple treatment. Large amounts of nickel interfere, however, and must be removed. METHOD FOR PLAIN STEELS [Vol. 81 The procedure arrived at after preliminary experiments is essentially simple.PREPARATION OF SAMPLE FOR CHROMATOGRAPHY- Weigh 0.1 to 1.0 g of steel, choosing the weight so that the amount of aluminium will be about 50 pg. Place the sample in a 250-ml tall beaker, and dissolve it with gentle heating in 10 ml of concentrated hydrochloric acidl. Add 10 ml of water and oxidise by dropwise addition of 1 ml of 100-volume hydrogen peroxide. Simmer until excess of peroxide is removed and then evaporate to about 51-111. Allow to cool and add quickly, i.e., not by gradual addition, a suitable amount of freshly distilled ethyl methyl ketone, followed if necessary by drops of concentrated hydrochloric acid, in order to form a homogeneous solution. The details of this step vary according to the type of steel being analysed: certain alloy steels tend to give solutions having two phases, and this must be avoided; for a simple mild steel, however, no difficulty is found if the amount of ketone is 25 to 50 ml.Transfer this solution to a prepared cellulose column. PREPARATION OF CELLULOSE COLUMN- Prepare the column with aqueous acid to remove any contaminating aluminium. Add 5 g of cellulose powder (Whatman, Standard grade) to 90 ml of diluted hydrochloric acid (1 + 5) and pour this slurry into a silicone-treated chromatographic tube. Allow the column to settle and then to drain; wash it successively with 200 ml of diluted hydrochloric acid (1 + 5 ) , 200 ml of water, 100ml of freshly distilled ethyl methyl ketone and 100ml of an eluent prepared by mixing 80 ml of constant-boiling hydrochloric acid with 1920 ml of freshly distilled ethyl methyl ketone.SEPARATION OF ALUMINIUM- Transfer the sample solution to the column with small washings of the ketone eluent, allowing the column to drain between washings. Wash the column with about 2-ml portions of the ketone eluent, rinsing the walls above the cellulose with each addition, until all iron is washed away from the column. Reject the eluate. Recover the aluminium, which remains at the top of the cellulose column together with any nickel, by passing 200 ml of diluted hydrochloric acid (11-5) through the column. DETERMINATION OF ALUMINIUM- Evaporate the solution obtained as described above to dryness, add 0-5 ml of 60 per cent. perchloric acid, cover the beaker and heat to fuming, uncover and evaporate to dryness. Dissolve the residue in a few drops-of diluted perchloric acid ( l + l ) , add 2 drops of methyl red solution and carefully make the solution just alkaline with 10 per cent.sodium hydroxide. Re-acidify by dropwise addition of N perchloric acid and then add 0-2 ml of 5 N perchloric acid. Add 1 rnl of 2 N sodium acetate solution and 5 ml of a 0.1 per cent. solution of Solo- chrome violet RS, transfer to a 10-ml calibrated flask and dilute to the mark. Immerse the flask for 5 minutes in a water bath at 55" to 70" C, allow it to cool, de-aerate the solution, and record a polarogram between 0 and -- 0.8 volt against a standard calomel electrode, using a dropping-mercury cathode. NOTE ON METHOD- With steels containing small amounts of aluminium it is necessary to observe all the precautions used in trace-metal analysis.The materials used in large quantities, hydrochloric Add 50 ml more of eluent and allow to drain.May, 19561 STEEL WITH THE AID OF CHROMATOGRAPHIC SEPARATION 293 acid and ethyl methyl ketone, are best purified by redistillation. With reasonable care the blank readings can be kept below or near to the limits of detection. For routine analysis of steels containing moderate amounts of aluminium the columns can be prepared from cellulose and ketone eluent without the acid wash, provided adequate blank columns are used. MODIFICATION FOR STEELS CONTAINING NICKEL IN ALLOYING AMOUNTS In the chromatographic separation, nickel remains on the column, together with alu- minium, after elution; it likewise accompanies the aluminium in the acid solution washed off the column.The amount of nickel in plain steels is insufficient to interfere with the polarographic aluminium determination, but alloying amounts give concentrations that interfere significantly. Nickel can be removed from such steels to an extent sufficient to render the polarographic determination of aluminium possible, by a short small-scale mercury-cathode electrolysis, in a simple cell, carried out on the solution obtained from the column. The need for such a separation would of course not exist if the aluminium were to be determined by a method with which nickel would not interfere. RESULTS To test the method for plain steels, known amounts of aluminium were added to known weights of aluminium-free steel, which were then taken through the described procedure.The recoveries are shown in Table I. TABLE I RECOVERY OF ADDED ALUMINIUM FROM 0-5-g PORTIONS OF AN ALUMINIUM-FREE PLAIN STEEL Aluminium added, Aluminium recovered, Recovery, Pg PLg % 600 576 96 400 376 94 300 288 96 200 200 100 30.0 29.0 97 22-5 24.5 109 20.0 21.0 105 15-0 14-5 97 10.0 8-5 85 5.0 5.5 110 5-0 4.5 90 TABLE I1 TYPICAL RESULTS FOR VARIOUS STEELS Aluminium content Aluminium found Steel reported by other workers, by present method, % % 0.025 0.020 /::::: 0-020 MGS/182* .. .. 0.004 to 0.005 MGS/183* .. . . 0.016 to 0.019 [0-019 L.K. Nitriding steel . . 1.25 { ;;;; [ 0.049 * . N 0.05 { ::z B.C.S. 255 . . [ 0-044 * Analysed by Methods of Analysis Committee of the Metallurgy Division of the British Iron and Steel Research Association.6294 BARRETT : MICRO-DETERMINATION OF [Vol.81 A large number of aluminium determinations on un-alloyed steels have been carried out successfully by this method over the last few years in these laboratories. Determinations were carried out on sleveral steels already analysed and reported by other workers. Most of these analyses included the mercury-cathode electrolysis for nickel removal. The results are shown in Table 11. CONCLUSIONS The figures given in Tables I and I1 confirm that large quantities of iron can be removed on a cellulose column while aluminium is retained quantitatively. The main advantages of the method are rapidity, simplicity of apparatus and the clear-cut separation obtained. Even when the additional step of a small-scale mercury-cathode electrolysis is necessary in order to remove nickel, the method is still rapid and capable of routine operation; the small amount of mercury used in the separation is only slightly contaminated with nickel and is easily removed. Thanks are due to Dr. H. Liebmann for 'constant encouragement during the investigation, to Mr. B. T. G. Layzell, who carried out some of the comparative work, and to Mr. J. 0. Lay of the British Iron and Steel Research Association, who supplied the anaiysed steels. REFERENCES 1. 2. 3. 4. 5 . THE METAL Box COMPANY LIMITED Methods of Analysis Committee of B.I.S.R.A., J . Iron G. Steel Inst., 1954, 176, 29. Bishop, J. R., and Liebmann, H., Analyst, 1953, 78, 117. Burstall, F. H., Davies, G. R., and Wells, R. A., Disc. Faraday Soc., 1949, 7 , 179. Willard, H. H., and Dean, J. A., Anal. Ckem., 1950, 22, 1264. Methods of Analysis Committee of B.I.S.R.A., J . Iron & Steel Inst., 1954, 176, 263. RESEARCH DIVISION November llth, 1955 ACTON, W.3

ISSN:0003-2654    

DOI:10.1039/AN9568100291

出版商:RSC    

年代:1956

数据来源: RSC