JUNE, 1958 THE ANALYST Vol, 83, No. 987 PROCEEDINGS OF THE SOCIETY FOR ANALYTICAL CHEMISTRY NEW MEMBERS ORDINARY MEMBERS Desmond Arthur Sidney Barnes, B.Sc. (Lond.) ; Thomas Malcolm Blackwood, B.Sc. (Edin.) ; Bernard Fitzgerald; John Kenneth Fleming, A.R.I.C. ; Neil Robert Francis, B.Sc. (Notting- ham) ; Harry William Houghton, B.Sc. (Nottingham) ; Archie Ronald Javes, B.Sc. (Lond.), F.R.I.C., F.Inst.Pet. ; Charles Edward Roland Jones; Derek Edward Icings, B.Sc. (Hull), A.R.I.C. ; Frederick Lishman, B.Sc. (Sheff.) ; Denis Naylor, B.Sc. (Sheff .) ; John Jonas Nicholls, B.Sc. (Lond.), F.R.I.C. ; Stanley Hope Philpot, A.R.I.C. ; William Crossley Purdy, B.A. (Amherst), Ph.D. (M.I.T.); Herbert Taylor, B.Sc. (Lond.), A.R.I.C.; Walter Westwood, BSc. (Liv.), A.I.M. JUNIOR MEMBERS Elizabeth Jane Hall, B.Sc.(Wales); David Henry Thow, B.Sc. (Edin.). DEATH Daniel Carswell Macpherson. WE record with regret the death of NORTH OF ENGLAND SECTION AND MICROCHEMISTRY GROUP A JOINT Meeting of the North of England Section and the Microchemistry Group with the North Lancashire Section of the Royal Institute of Chemistry was held at 7.30 p.m. on Friday, May 16th, 1958, at Redmans Park House Hotel, North Promenade, Blackpool. The Chair was taken by the Chairman of the North Lancashire Section, Mr. C. D. Lafferty, B.Sc., F.R.I.C. The following papers were presented and discussed: “The Micro Vacuum Fusion Deter- mination of Gases in Metals,” by &I. R. Everett; “The Chemical Determination of Nitrogen in Reactor Metals,” by J. A. Ryan, A.R.I.C.; “The Determination of Naturally Occurring Radioactive Impurities in a Uranium Purification Process,” by M.R. Hayes, A.R.I.C. ; “A Simple Manometric Method for the Determination of Carbon in Metals,” by M. R. Everett (see summaries below). The meeting was preceded at 2 p.m. by a visit to the Chemical Services Department Laboratories of the Springfields Works of the United Kingdom Atomic Energy Authority (Industrial Group). THE MICRO VACUUM FUSION DETERMINATION OF GASES I N METALS MR. M. R. EVERETT said that, in the vacuum fusion technique, a sample was added to a de-gassed graphite crucible or a de-gassed carbon-containing metal bath, maintained at a high temperature in vacuo. The hydrogen, oxygen and nitrogen contents of suitable metals could be calculated from analysis of the evolved gas, which consisted of a mixture of hydrogen, carbon monoxide and nitrogen. Sources of error in vacuum fusion were briefly considered.321322 PROCEEDINGS [Vol. 83 A micro-scale all-mercury-and-glass apparatus was described. This contained a 3.5-g molten-platinum bath at an operating temperature of 1900” C for the analysis of metals such as thorium, zirconium, uranium, niobium, vanadium, molybdenum and tungsten. Sample weights were of the order of 50 mg, and up to twelve samples could be analysed consecutively. A low-pressure circulating-type gas analytical system was used. Limits of detection were approximately 1 1j.p.m. for both hydrogen and nitrogen and 5 p.p.m. for oxygen. The author quoted results that demonstrated the agreement between vacuum fusion and chemical determinations of nitrogen for a large number of zirconium samples. In the analysis of metal of very low gas content, gaseous contamination on the surface of a prepared micro sample could cause an appreciable positive bias, particularly for oxygen, and results that showed the extent of this effect were also quoted.THE CHEMICAL DETERMINATION OF NITROGEN IN REACTOR hlETALS MR. J. A. RYAN said that the applicability of the Allen method for the determination of nitrogen in the reactor metals niobium, vanadium, zirconium, molybdenum and beryllium had been demonstrated by comparison of the performance of the method with the Dumas and caustic-fusion methods. Nitrides of the metals had been prepared and used for the comparison experiments.Although the Allen method could be used satisfactorily for all these elements, it could only be used for the determination of nitrogen in molybdenum on a restricted size of sample. The caustic-fusion method was applicable to fully nitrogenated vanadium, but not to samples of vanadium metal, for which it gave “nil” recoveries. No experiments had been carried out with the Dumas method on beryllium, owing to the hazardous toxic nature of the material, but the method could be applied satisfactorily to the other elements. THE DETERMINATION OF NATURALLY OCCURRING RADIOACTIVE IMPURITIES MR. M. R. HAYES said that pitchblende ore contained the radioactive-decay products of uranium in their equilibrium concentrations, and these radioactive impurities were separated from the uranium during the refining process and appeared in the various plant intermediates and residues.A knowledge of the concentrations of these radioactive impurities was required in order that measures to prevent ur due concentration of radioactivity could be taken and to control the disposal of radioactive wastes. Also, as some of the radioactive im- purities were valuable by-products in the refining of uranium, analytical control was required to permit them to be recovered efficiently. Of the twenty-six radioactive isotopes occurring in the ore, the most important were shown to be thorium-230, polonium-210 and radium-226. The analytical methods used in the determination of these three isotopes were outlined. For thorium-230 and polonium-210, chemical separation followed by alpha counting was used. The methods for radium were purely physical: direct measurement of gamma-ray intensity at the higher levels and separation of radon gas followed by measurement of its activity at lower levels.The concentrations of these radioactive impurities, and mass balances obtained for them over a period of production, were discussed. IN A URANItJM PURIFICATION PROCESS A SIMPLE MANOMETRIC METHOD FOR THE DETERMINATION OF CARBON IN METALS MR. M. R. EVERETT described an apparatus that was simple, compact and portable. It could be used to isolate and determine carbon dioxide in oxygen or nitrogen carrier- gas streams having velocities of up t o 300 ml per minute. The sensitivity range was from 10 to 8000 pg of carbon. An efficient multi-loop cold trap isolated the carbon dioxide, which was afterwards expanded at room temperature in a small evacuated calibrated volume that included an atmospheric-column manometer.SCOTT1 SH SECTION A JOINT Meeting of the Section and the Methods of Analysis Panel (Glasgow) was held at 7.15 p.m. on Friday, April 25th, 1958, in the Royal College of Science and Technology,June, 19581 PROCEEDINGS 323 204 George Street, Glasgow, C.l. The Chair was taken by the Chairman of the Methods of Analysis Panel, Mr. J. H. Love. A lecture on “X-ray Fluorescence Techniques in Analytical Chemistry” was given by E. T. Hall, M.A., D.Phi1. (see summary below). X-RAY FLUORESCENCE TECHNIQUES IN ANALYTICAL CHEMISTRY DR. E. T. HALL said that the use of X-ray fluorescence both in the laboratory and in process control was an accomplished fact in the United States of America.However, in this country, in spite of the existence of the technique since 1914, the importance of the method was only just being realised. The speaker gave an outline of the technique together with some idea of how the physical, mechanical and electronic problems had been solved. Reference was made to commercial equipments available, and how automatic servo-controlled spectrometers could carry out automatic analyses of complex systems. Results could be taken either intermittently in digital form or continuously in analogue form. Some comparisons were made with optical spectrometers, and possible applications to trace analysis were indicated. Examples of suitable problems with their attendant advantages were described.Some mention was also made of the advantages of this technique in non-destructive archaeological analysis of valuable museum objects. SCOTTISH SECTION AND PHYSICAL METHODS GROUP A JOINT Meeting of the Scottish Section and the Physical Methods Group with the Aberdeen University Chemistry Society was held at 7.30 p.m. on Friday, May 16th, 1958, in the Main Lecture Theatre, Chemistry Department, King’s College, Old Aberdeen. The Chair was taken by the Chairman of the Physical Methods Group, Mr. R. A. C. Isbell, A.1nst.P. The following papers were presented and discussed: “The Analysis of Clays Using Ion-exchange Resins,” by Mrs. Jean McAuslin, BSc., A.R.I.C. ; “The Application of Gamma Radiation to the Non-destructive Examination of Coal,” by J.Craig Higgins (see summaries below). During the morning, the Chemistry Department of King’s College was open to visitors and there were demonstrations of a cathode-ray polarograph, a Unicam SP900 flame photo- meter and a high-sensitivity pH meter. In the afternoon, visits were paid to the Macaulay Institute for Soil Research and to the Ministry of Agriculture, Fisheries and Food Experi- mental Factory, THE ANALYSIS OF CLAYS USING ION-EXCHANGE RESINS MRS. JEAN MCAUSLIN described a method of clay analysis in which the sample was decomposed and the silica removed by treatment with hydrofluoric acid. The metallic constituents of the clay were then separated from one another and determined quantitatively. Iron and manganese were converted to anionic chloride complexes, and aluminium to an anionic phosphate complex. These complexes were then adsorbed on anion-exchange resin columns.A cation-exchange resin column was used to separate sodium and potassium from calcium and magnesium. Sodium and potassium were determined by flame-photometric methods, and titanium was determined colorimetrically. The remaining elements were determined by titration with ethylenediaminetetra-acetic acid. The behaviour of titanium had been investi- gated, and provision had been made to prevent its interference in the determination of the other metals. THE APPLICATION OF GAMMA RADIATION TO THE NON-DESTRUCTIVE EXAMINATION OF COAL MR. J. C. HIGGINS said that planning the development of new coalfields required much preliminary proving and survey work.This was carried out to a large extent by exploratory boring. The samples obtained in “core” form from these boreholes provided a valuable cross-section of the coal seams present and their associated strata. The attenuation by coal of gamma radiation from a radioactive source had been utilised as the basis of an experimental non-destructive method of examining the physical structure of coal seams as provided by these core samples. The method had been used as an aid to the visual assessment of seam structure that was carried out before further physical and chemical tests were made.32-1 PROCEEDINGS [Vol. 83 The work done so far demonstrated the practicability of the method and showed it to be capable of differentiating between bands of coal that were closely similar in ash content and specific gravity.Sharp resolution of adjacent thin coal and dirt bands was possible and variations in mineral-matter content had been observed in places where they had not been demonstrated by standard preliminary examination. WESTERN A K I ~ MIDLAXDS SECTIOKS A JOIST Summer Meeting of the Western and Midlands Sections was held on Friday and Saturday, May 16th and 17th, 1958, in the Lecture Theatre, West Midlands Gas Board, Castle Foregate, Shrewsbury. The Chair was taken on Friday by the Chairman of the Mid- lands Section, Dr. R. Belcher, F.R.I.C., 1F.Inst F., and on Saturday by the Chairman of the Western Section, Mr. S. Dixon. MSc.. F. R.1 C. At 7 p.m. on Friday- the following papers were presented and discussed: “The Origins and Growth of Volumetric Analysis” and “The Origins of Quantitative Organic Analysis,” by TY.I. Stephen, B.Sc., Ph.D., A.R.I.C. At 9.30 a.m. on Saturday the following papers mere presented and discussed : “The Historical Development of the Public Analyst,” by G. V. James, IVI.B.E., M.Sc,, Ph.D., F.R.I.C., P.A.I.W.E.; “The Origins of Quantitative Chemical Analysis,” by R. E. Coulson, F.R.I.C. (see summaries below). THE ORIGINS ASD GROWTH OF VOLUNETRIC ANALYSIS DR. W. I. STEPHEN described the early history of titrimetry to show how this branch of chemical analysis had played an (equally as important part in the development of quantitative analysis as had gravimetry. The contributions of Mohr and Penny to the growth of the subject were also discussed.THE ORIGINS OF QVANTITATIVE ORGANIC ANALYSIS DR. W. I. STEPHEN described the contributions of Berzelius, Liebig, Gay-Lussac Subsequent developments in quantitative Some and Dumas to elemental organic analysis. organic analysis had depended entirely on the work of these famous chemists. mention was also made of the histoly of functional-group analysis. THE HISTORICAL DEVELOPMENT OF THE PUBLIC ANALYST DR. G. V. JAMES traced the place of food poisoning and the protection given by select individuals from early times, and described prohibitive legislation in historical times. He mentioned early analyticd tests for adulteration, and described the wide- spread sophistication of the early nineteenth century that led to the Lancet Commission and the first Food and Drugs Act of 1860.Some early books and instrumerts of this latter period were displayed. THE ORIGINS OF QUANTITATIVE CHEMICAL ANALYSIS 11~. R. E. COULSOX said that Klaproth had laid the foundations of quantitative analysis in his work on minerals. He had shown how even the most refractory materials might be brought into solution and the components separated. Berzelius had extended this work and applied current ideas of the structure of chemical compounds to check the analytical results obtained by himself and others, which had led to a clear under- standing of combining proportions. NIDLAKDS SECTIOK A s Ordinary Meeting of the Section was held a t 6.30 p.m. on Wednesday, April 16th, 1058, in the Mason Theatre, The University, Edmund Street, Birmingham, 3. The Chair was taken by the Chairman of the Section, Dr. R. Belcher, F.R.I.C., F.1nst.F. The following paper was presented and discussed: “The Analysis of Silicones and Related Organosilicon Compounds,” by J. C. B. Smith. ,4 JOIXT Neeting of the Section with the East Midlands Section of the Royal Institute of Chemistry was held a t 7.30 p.m. on Thursday, April 24th, 1958, in the College of -4rt and Technology, Leicester. The Chair was taken by the Chairman of the East Midlands Section, Dr. A. G. Catchpole, F.R.I.C.June, 19581 OBITUARY 325 The following paper was presented and discussed: “Developments in the Use of Redox Indicators,” by R. Belcher, Ph.D., D.Sc., F.R.I.C., F.1nst.F. BIOLOGICAL METHODS GROUP -4s Ordinary Meeting of the Group was held at 6.30 p.m. on Wednesday, April 16th, 1958, in the restaurant room of “The Feathers,” Tudor Street, London, E.C.4. The Chair was taken by the Chairman of the Group, Dr. S. K. Kon, F.R.I.C. -4 discussion on “The Mathematics of Sterility Testing” was opened by D. Xaxwell Bryce, BSc., B.Pharm., F.P.S., A.R.I.C.