摘要:

Proceedings of the Society for Analytical Chemistry CONTENTS Proc. SOC. Analyt. Chem. Vol. 3 No. 2 Pages 13-28 Radiochemical Methods Group I3 Particle Size Analysis Conference I 3 Reports of Meetings .. . . 13 “Thermometric Titrimetry” . . 16 “Effluent Analysis” . . .. 21 Obituary . . .. .. .. 24 Membership changes . . . . 25 Papers accepted for The Analyst 25 Publications Received . . . . 26 Notices .. .. .. . . 26 Forthcoming Meetings Back cover February 1966 Vol. 3 No. 2 February 1966 PROCEEDINGS THE SOCIETY FOR ANALYTICAL CHEMISTRY OF President of the Society A. A. Smales O.B.E. Hon. Secretary of the Society S. A. Price Hon. Treasurer of the Society D. T. Lewis C.B. Hon. Assistant Secretaries of the Society B. S. Cooper; D. W. Wilson Secretary Miss P. E. Hutchinson 14 BELGRAVE SQUARE LONDON S.W.1 Telephone BELgravia 3258 Editor 1. B. Attrill Proceedings is published by The Society for Analytical Chemistry and distributed t o members and all subscribers t o The Analyst without charge Single copies may be obtained direct from the Secretary The Society for Analytical Chemistry a t the above address (NOT through Trade Agents) price 2s. 6d. post free Remittances payable t o “Society for Analytical Chemistry” MUST accompany orders T H E S O C I E T Y FOR A N A L Y T I C A L C H E M I S T R Y DR. J. T. MARTIN (Assistant Director of the Long Ashton Research Station Bristol) will lecture on CHEMICAL CROP PROTECTION I N BRITAIN MARCH 9th 1966 at 7 p.m. in the MEETING ROOM OF THE CHEMICAL SOCIETY BURLINGTON HOUSE LONDON W.1. This lecture will be preceded at 6 p.m. by the Annual General Meeting of the Society

ISSN:0037-9697    

DOI:10.1039/SA96603FX005

出版商:RSC    

年代:1966

数据来源: RSC

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THE SOCIETY FOR ANALYTICAL CHEMISTRY Forthcoming Meetings-continued March Thursday 24th MIDLANDSECTION jointly with the Birmingham and Midlands Sections of the Royal Institute of Chemistry and the Society of Chemical Industry. “Automatic Analysis,” by H. W. Holy M.Sc. Ph.D. North Staffordshire College of Technology Stoke-on-Trent ; 7 p.m. SOCIETY organised by the Midlands Section jointly with Birmingham and Midlands Sections of the Royal Institute of Chemistry and the Society of Chemical Industry and the Midlands Section of the Chemical Society on “Nuclear Magnetic Resonance and Electron-Spin Resonance Spectroscopy.” Plenary Lecture “Magnetic Resonance An Introduction,’’ by Professor N. Sheppard. “Academic Application of Nuclear Magnetic Resonance” by J. A. Smith M.A. D.Phil. F.C.S. “Analytical Application of Nuclear Magnetic Resonance Spectroscopy par- ticularly as applied to Industry,” by J .K. Becconsall B.Sc. Ph.D. “Some Aspects of the Nuclear Magnetic Resonance Spectroscopy of Fluorine Compounds,” by L. F. Thomas B.Sc. Ph.D. Discussion on “Nuclear Magnetic Resonance Spectroscopy. ” “Introduction to Electron-Spin Resonance Spectroscopy and its Applications,” “Instrumentation and Experimental Techniques in Electron-Spin Resonance Discussion on “Electron-Spin Resonance Spectroscopy.” (For further details see January Proceedings.) 9.45 a.m. STOKE-ON-TRENT Wednesday 30th BIRMINGHAM by D. H. Whiffen Ph.D. N.A.D. Spectroscopy,” by J. K. Brown B.A. Ph.D. Haworth Lecture Theatre The University Edgbaston Birmingham 15 ; MEETING OF THE GESELLSCHAFT DEUTSCHER CHEMIKER LINDAU 1966 THE meeting of the German Chemical Society Analytical Chemistry Technical Group with the Austrian Society for Microchemistry Analytical Chemistry VOCh and the Swiss Society for Analytical and Applied Chemistry will be held in Lindau (Bodersee) from April 13th to 15th 1966.The main topics to be discussed will be automatic analytical methods trace analysis and the limits of its application the combination of analytical procedures to structure elucidation. Enquiries concerning the meeting should be sent to Gesellschaft Deutscher Chemiker- Geschaftsstelle 6000 Frankfurt/Main Postfach 9075 Germany. THE SOCIETY FOR ANALYTICAL CHEMISTRY Forthcoming Meetings February Tuesday 22nd LONDON Wednesday 23rd LONDON Friday 25th PAISLEY March Wednesday 2nd LONDON Friday 4th NEWCASTLE Tuesday 8th NOTTINGHAM Wednesday 9th LONDON Wednesday 16th LONDON Friday 18th LEEDS Tuesday 22nd LONDON SPECIAL TECHNIQUES GROUP on “Special Techniques in Gas Analysis.” Speakers B.Riley C. G. Scott R. T. Parkinson and R. E. Wilson. Wellcome Building Euston Road London N.W. 1 ; 3 p.m. BIOLOGICAL METHODS GROUP. “Modern Techniques in the Bacteriological Examination of Food,” by Dr. Betty Hobbs. Meeting Room of the Chemical Society Burlington House Piccadilly London W.l.; 7 p.m. SCOTTISH SECTION. “The Balance Manufacturer Educator or Sycophant,” by M. V. Moorhouse. “Weighed in the Balance and Found Wanting,” by R. A. Chalmers B.Sc. College of Technology Paisley; 7.15 p.m. Ph.D. F.R.I.C. SOCIETY Informal Dinner. Park Lane Hotel Piccadilly London W.l; 7.15 p.m. for 7.45 p.m. NORTH OF ENGLAND SECTION jointly with the Newcastle upon Tyne Section of the Royal Institute of Chemistry on “The Analysis of Standard Metal- lurgical Samples.” Speakers P. D. Ridsdale B.Sc. A.I.M. and W. C. Coppins M.Sc. A.R.I.C. Lecture Theatre School of Chemistry The University Newcastle upon Tyne ; MIDLANDS SECTION jointly with the Forensic Society and the East Midlands 2.30 p.m. on “The Analysis of Drugs.” 5.30 p.m. 6.30 p.m. on “Drug Analysis with Special Reference to Forensic Analysis.” Boots Pure Drug Co. Ltd. Pennyfoot Street Nottingham. SOCIETY. 6 p.m. Annual General Meeting of the Society. 7 p.m. Ordinary Meeting. 6.30 p.m.* Section of the Royal Institute of Chemistry. Speakers J. Allen F.R.I.C. and S. G. E. Stevens B.Sc. F.R.I.C. Annual General Meeting of the Midlands Section. Speaker E. C. Clarke M.A. Ph.D. F.R.I.C. “Chemical Crop Protection in Britain,’’ by J. T. Martin Ph.D. D.Sc. F.R.I.C. Meeting Room of the Chemical Society Burlington House Piccadilly London w.l. MICROCHEMICAL METHODS GROUP Discussion Meeting on “The Determination of Molecular Weights.” “The Feathers,” Tudor Street London E.C.4; 6.30 p.m. NORTH OF ENGLAND SECTION jointly with Leeds University Union Chemical The University Leeds; 6.15 p.m. SPECIAL TECHNIQUES GROUP Discussion Meeting dealing with novel tech- Imperial College South Kensington London S.W.7; 6 p.m. * Please note that this is a change of time from that originally announced. Society. niques. [continued inside back cover PRINTED BY W. HEFFER k SONS LTD. CAMBRIDGE ENGLAND

ISSN:0037-9697    

DOI:10.1039/SA96603BX007

出版商:RSC    

年代:1966

数据来源: RSC

摘要:

February I966 Vol. 3 No. 2 Reports of Meetings ORDINARY MEETING AN Ordinary Meeting of the Society was held at 7 p.m. on Wednesday February 2nd 1966 in the Meeting Room of the Chemical Society Burlington House London W.l. The Chair was taken by the President Dr. A. A. Smales O.B.E. F.R.I.C. The subject of the meeting was “Determination of Purity in High-purity Organic Materials” and the following papers were presented and discussed “Methods of Determining Purity in Use in the Chemical Standards Division of N.P.L.,” by J. D. Cox Ph.D. D.I.C. A.R.C.S. ; “Some Methods for Determining the Purity of Pharmaceutical Products,” by J. H. Chapman Ph.D. D.I.C. F.R.I.C. WESTERN SECTION A JOINT Meeting of the Section with the Local Sections of the Chemical Society the Society of Chemical Industry and the Royal Institute of Chemistry was held at 5.30 p.m.on Monday December 13th 1965 in the School of Chemistry The University Bristol. The Chair was taken by Dr. R. Parsons B.Sc. A lecture on “The Partition of Mixtures of Homologues and Isomers by Chromato- 13 polarography” was given by Professor W. Kemula. 14 REPORTS OF MEETINGS [Proc. SOC. Analyt. Chem. A Joint Meeting of the Section with the Cardiff and District Section of the Royal Institute of Chemistry was held at 7 p.m. on Friday December 17th 1965 at University College Cardiff. The Chair was taken by the Chairman of the Western Section Mr. E. A. Hontoir B.Sc. A.I.M. The following paper was presented and discussed “Atomic-absorption Spectroscopy,” by H. Pugh MSc. F.R.I.C. MIDLANDS SECTION A JOINT Meeting of the Section with the Midlands Section of the Chemical Society was held at 6.30 p.m.on Friday December loth 1965 in the Haworth Lecture Theatre Chemistry Department The University Edgbaston Birmingham 15. The Chair was taken by the Chairman of the University of Birmingham Chemical Society Professor M. Stacey F.R.S. A lecture on “The Partition of Mixtures of Homologues and Isomers by Chromato- polarography,” was given by Professor W. Kemula. MICROCHEMICAL METHODS GROUP THE twenty-second Annual General Meeting of the Group was held at 6.45 p.m. on Friday December loth 1965 in the Meeting Room of the Chemical Society Burlington House London W.l. The Chair was taken by the Chairman of the Group Mr. R. Goulden F.R.I.C. The following Officers and Committee Members were elected for the forthcoming year Chairman-Mr.R. Goulden. Vice-Chairman-Mr. T. R. F. W. Fennell. Honorary Treasurer-Mr. F. H. Oliver. Honorary Secretary-Mrs. D. E. Butterworth Division of Molecular Science National Physical Laboratory Teddington Middlesex. Members of Committee-Mr. P. R. W. Baker Mr. M. P. Mendoza Mr. R. Rothwell Mr. R. Sawyer Dr. J. H. Thompson and Mr. D. W. Wilson. Mr. C. Whalley and Mr. H. Childs were appointed as Honorary Auditors. The Annual General Meeting was followed by an Ordinary Meeting of the Group at which the following paper was presented and discussed “Practical Experience in Statistics Applied to Chemistry,” by A. K. Soper M.Sc. F.R.I.C. BIOLOGICAL METHODS GROUP THE twenty-first Annual General Meeting of the Group was held at 6.30 p.m. on Thursday December 9th 1965 in “The Feathers,” Tudor Street London E.C.4.The Chair was taken by the Chairman of the Group Dr. M. W. Parkes. The following Officers and Committee Members were elected for the forthcoming year Chairman-Dr. M. W. Parkes. Vice-Chuirman-Mr. A. W. Macfarlane. Honorary Secretary and Treasurer-Mr. K. L. Smith Bio-assay Division Standards Department Boots Pure Drug Co. Ltd. Pennyfoot Street Nottingham. Members of Committee-Dr. Jillian M. Bond Miss A. M. Jones Mr. W. A. Broom Mr. K. L. Mansford Mr. W. H. C. Shaw and Dr. G. A. Stewart. Honorary Recorder-Dr. I. Fleming. Mr. D. M. Freeland and Dr. J. H. Hamence were re-appointed as Honorary Auditors. The Annual General Meeting was followed by a Discussion Meeting at which a discussion on “Problems and Dilemmas in Microbiological Assay” was opened by S.A. Price B.Sc. F.R. I .C. ATOMIC-ABSORPTION SPECTROSCOPY GROUP THE first Annual General Meeting of the Group was held at 6.30 p.m. on Tuesday November 30th 1965 in the Meeting Room of the Chemical Society Burlington House London W.l. The Chair was taken by the Chairman of the Group Mr. W. T. Elwell F.R.I.C. The following Officers and Committee Members were elected for the forthcoming year Chairman- Mr. W. T. Elwell. Honorary Secretary and Treasurer- Mr. D. Moore Hilger & Watts Ltd. 98 St. Pancras Way Camden Road London N.W.l. Members of Committee-Mrs. A. P. Gower Dr. R. M. Dagnall Dr. G. Nickless Mr. W. J. Vice-Chairman-Dr. J. B. Dawson. February 19601 ANALYTICAL METHODS COMMITTEE 16 Price Mr. E. G. Towndrow and Mr. R. A. White. Mr. C. J. Keattch and Dr. J. A. C.McClelland were appointed as Honorary Auditors. The Annual General Meeting was followed by an Ordinary Meeting of the Group at which a discussion on “Atomic Fluorescence Spectrometry” was opened by G. I. Goodfellow. THIN-LAYER CHROMATOGRAPHY GROUP THE first Annual General Meeting of the Group was held at 2.15 p.m. on Wednesday December lst 1965 at the Chelsea College of Science and Technology Manresa Road London S.W.3. The Chair was taken by the Chairman of the Group Dr. E. V. Truter A.R.C.S. The following Officers and Committee Members were elected for the forthcoming year Chairman-Dr. E. V. Truter. Honorary Treasurer (actiag Homravy Secretary)-Mr. F. W. S. Carver Explosives Research and Development Establishment Waltham Abbey Essex. Honorary Secretary-Dr. I. Smith. Members of Committee-Dr.T. L. Parkinson Dr. E. J. Shellard Mr. B. Warren Mr. J. S. Wragg and Mr. R. Butler. Dr. J. S. Purdy and Mr. E. J. Gallacher were appointed as Honorary Auditors. The Annual General Meeting was followed by an Ordinary Meeting of the Group at which the following papers were presented and discussed “A Study of the Oxidation of Nitroso-aromatics to Nitro-aromatics in Propellant Stabilisers Using Thin-Layer Chromato- graphy and Mass Spectrometry,’’ by J. W. Grindlay P. M. Wraighte and J. C. Wright; “The Determination of Anti-oxidants and Other Additives in Plastics by Thin-Layer Chromatography,” by G. B. Campbell; “Study of the Auto-oxidation of Lanosterol by Thin-Layer Chromatography,’’ by J. Scotney. Vice-Chairman-Dr. J. D. R. Thomas. THERMAL ANALYSIS GROUP THE first Annual General Meeting of the Group was held at 6.30 p.m.on Thursday December 2nd 1965 in the Meeting Room of the Chemical Society Burlington House London W.l. The Chair was taken by the Chairman of the Group Dr. R. C. Mackenzie F.R.I.C. F.G.S. F.R.S.E. The following Officers and Committee Members were elected for the forthcoming year Chairman-Dr. R. C. Mackenzie. Vice-Chairman-Dr. J. P. Redfern. Honorary Treasz+trev-Dr. A. A. Hodgson. Honorary Secretary-Mr. C. J. Keattch John Laing Research & Development Ltd. Manor Way Boreham Wood Herts. Members of Committee-Dr. D. Dollimore Mr. J. A. Forrester Dr. W. Manz Mr. E. P. J. Schilling Mr. D. A. Smith and Mr. F. W. Wilburn. Mr. W. Boardman and Dr. T. L. Parkinson were re-appointed as Honorary Auditors. The Annual General Meeting was followed by an Ordinary Meeting of the Group at which the following papers were presented and discussed “Coal Carbonisation Kinetics- Simple Thoughts on a Complex Matter,” by D.Fitzgerald M.A. B.Sc. Ph.D. M.1nst.F.; “The Analysis of Volatile Materials by Mass Detection Gas Chromatography,” by S. C. Bevan B.Sc. Ph.D. F.R.I.C. and S. Thorburn B.Sc. Dip.Ed. F.R.I.C. Analytical Methods Committee JOINT COMMITTEE ON METHODS FOR THE EVALUATION OF DRUGS THE Joint Committee of the Pharmaceutical Society and the Society for Analytical Chemistry has appointed a Panel to investigate the thin-layer chromatography of corticosteroids. The constitution of the Panel is Mr. C. A. Johnson (Chairman) Mr. R. A. Bastow Miss B. Gartside Mr. A. Hall Dr. W. McMeekin and Mr. J. S. Wragg with Mr. P. W. Shallis as Secretary. The terms of reference under which the Panel will work are- “To devise a thin-layer chromatographic procedure to limit foreign steroids in corticosteroids which it is hoped will prove suitable for use in Monographs of the B.P. and the B.P.C.”

ISSN:0037-9697    

DOI:10.1039/SA966030013b

出版商:RSC    

年代:1966

数据来源: RSC

摘要:

16 THERMOMETRIC TITRIMETRY [Proc. SOC. Analyt. Chem. Thermometric Titrimetry The following are summaries of papers presented at the Joint Meeting of the Midlands Section of the Society and the Birmingham and Midlands Section of the Royal Institute of Chemistry held on September 15th 1965 and reported in the October issue of Proceedings (p. 147). Introduction to Thermometric Titrimetry BY L. S. BARK (Royal College of Advanced Technology Salford Lancashive) MR. BARK stated that as a thermometric titration utilised the enthalpy change of a reaction to locate the end-point of the reaction it could be defined as a titration in an adiabatic system in which the temperature was plotted against the volume of the titrant used. As most reactions showed detectable heat changes thermometric methods could be used for various types of reactions.Factors such as adverse colour changes and turbidity (arising from the original sample or caused by precipitation of materials from solution) which affected photometric titrations and which might have an adverse effect on electrode systems in electrometric methods had no significant effect on thermometric methods. The apparatus used for thermometric titrations was essentially a burette in conjunction with a sensitive device for measuring the temperature change of the titrand system. The earliest type of apparatus used had comprised a thermostatted burette that delivered the titrant into a titrand contained in a Dewar flask. The temperature change had been measured with a Beckmann thermometer or one of similar sensitivity. Although the time required for a simple titration with this type of system had been approximately 45 to 60 minutes deter- minations such as those of calcium with oxalate the calcium-to-magnesium ratio in dolomite and investigation of basic-salt formation of beryllium cobalt and nickel compounds had been made.The first major advance had been made in 1953 by replacing the thermometer with a thermistor bridge capable of recording temperature change and replacing the simple burette with a constant-flow burette. The introduction of an automatic-piston burette in 1957 had completed the system which was now considered to be the basic apparatus for thermometric titrations. Fast delivery had been advocated by some workers who used the rapid change in temperature and consequent large change in bridge current to enable first and second derivative curves to be drawn thus indicating more clearly the points at which relatively large heats of reaction occurred.The heat losses or gains (due to ambient temperature changes) of titra- tions that could be made in 10 to 20 seconds were not large enough to interfere with end-point detection and had therefore obviated the need for a thermostating of the titrand in a Dewar flask. It had also been possible to automate the burette so that the titration became a “dead-stop” titration and the titre was presented digitally or on paper. This method was claimed to achieve a greater accuracy than that obtained by using the normal type of recorder and chart paper and hence calculating the volume of the titrant used by measuring the length of trace on the paper.Other workers who had used a slow delivery of titrant claimed to be able to determine multiple equivalence-point titrations with greater accuracy. Among the various determinations that had been made were acid - base redox pre- cipitation complexometric and simple non-aqueous titrations. Titrations in organic solvents were readily accomplished by this method the low specific heat of the materials used allowed small energy changes to give relatively large temperature changes. It was suggested that further advances would be made by improving the metering of the flow and the delivery of the titrant and in electronic amplification of the signal that was received from the thermistor. Further development had depended on the particular rate of delivery of titrant. February 19661 THERMOMETRIC TITRIMETRY 17 Thermodynamic Background and Possible Application to Analytical Probleins BY H.J. V. TYRRELL (Chelsea College of Science and Technology Manresa Road London S . W.3) PROFESSOR TYRRELL said that most reactions involved an evolution or absorption of heat the amount of heat evolved being a function of the molar enthalpy change in the reaction and of the extent to which the reaction had taken place. When the reaction was complete further addition of reagent normally gave rise to a much smaller heat change that arose from the dilution of the reagent. Therefore if the heat evolved per unit addition of reagent was measured there would in general be a detectable change in this amount when the reaction was complete i.e. at the end-point. An enthalfiimetric titration then became a possibility.As heat evolution could not be measured directly but only temperature changes the name thermometric titration was to be preferred. The ease of detection of the end-point depended upon the size of the enthalpy change in the reaction in contrast with normal titrimetric procedures where the sharpness of the end-point depended upon the magnitude of one or more equilibrium constants i.e. upon standard free-energy changes. A large enthalpy change might be associated with an unfavourable free-energy change and for this reason reactions unsuitable for normal titrimetric procedures might give sharp end-points in a thermometric titration. A striking example was the ease with which weak acids such as boric acid and the ammonium ion might be determined with a thermometric end-point by titration with alkali.The enthalpy change could be either positive or negative as long as it was sufficiently large. Recent advances in instrumentation had made it possible to carry out such titrations easily and quickly. The method had been widely applied to aqueous and non-aqueous solutions and even to certain fused-salt systems. The chief disadvantage might be lack of selectivity associated with the fact that almost all reactions showed a sizeable value of AH but sometimes kinetic factors could intervene in a favourable manner. For example calcium could be determined in the presence of magnesium with oxalate; this was because the precipitation of magnesium oxalate was too slow to occur in the short time required for the experiment to be completed. Thermometric titrations could also be used in principle to measure enthalpy and free-energy changes in reactions; the principal problem was the improvement of the experimental tech- niques so as to achieve the highest possible accuracy in measurement of the temperature changes.An Apparatus for Recording Thermometric Titration Curves BY W. S. SEBBORN (Research Laboratory Kodak Ltd. Wealdstone Harrow) MR. SEBBORN described the apparatus constructed and used in the Kodak Research Labora- tory which was based on work described by Jordan and Alleman and by Zenchelsky and Sagatto and which now contained some important modifications that enabled it to be con- siderably simplified. By using a specially designed high-speed mixer it was possible to add the titrant at a rate of up to 10 ml per minute so allowing a titration to be completed in 20 seconds or less.This not only allowed the derivative of the temperature-time curve to be used so giving sharper end-point discrimination but also rendered less significant those heat losses or gains due to small changes in ambient temperature and eliminated the need to carry out titrations in Dewar vessels. Titrations were carried out in polythene beakers of about 50 ml capacity. The stirrer used was a circular paddle made from Perspex lying in a horizontal plane and drilled with oblique holes in a random fashion. This paddle was supported by a central vertical spindle formed from an F23 (Standard Telephones & Cables Ltd.) thermistor and was attached by this to a vibration generator operating at mains frequency. By this arrange- ment the paddle could be vibrated in a vertical plane with an amplitude of about inch.The diameter of the paddle was chosen so that there was minimal clearance between it andthe wall of the polythene beaker used as the titration vessel. 18 THERMOMETRIC TITRIMETRY [Proc. SOC. Analyt. Chew. The thermistor used type F23 was in the form of a small glass-covered bead at the end of a thin rod. It was possible to use this to support the vibrating disc and consequently the relative position of the thermistor bead and the stirrer remained constant thus eliminating a possible source of variation. At the time when work was carried out a suitable burette was not commercially available and a syringe burette was constructed with a standard 5-ml Chance glass syringe giving a delivery rate of 7 ml per minute.Temperature changes and times were followed on a recording millivoltmeter similar to the practice of earlier workers but it was found more convenient to replace the normal bridge circuit with one giving constant sensi- tivity over a temperature range of 15" to 30" C. Because titration times were from 10 to 20 seconds duration it became necessary to use greater chart speeds than those employed by earlier workers in order to obtain the necessary precision of measurement of time and hence volume of titrant used. Speeds used were about 30 inches per minute. This gave 10 inches of record per titration allowing k0.5 per cent. accuracy in measurement of titre. For routine titrations involving a single end-point the recording titrator was more conveniently replaced by a digital read-out burette.The recording titrator was however eminently suited for investigative work and for titrations involving multiple end-points. These included titrations with 0.1 N hydrochloric acid showing (a) multiple end-points obtained in titration of photo- graphic developer containing alkali carbonate and sulphite and (b) results of titration of silver nitrate by hydrochloric acid oxidation - reduction reactions with sulphate - cerate iodine and permanganate; and multiple cation titrations with EDTA. The use of interposition of an endothermally reactive cation to sharpen the end-point of an exothermal reaction or to improve separation of successive exothermal end-points was illustrated. The advantages and wide applicability of thermometric titration were mentioned; most determinations normally performed gravimetrically could be carried out volumetrically by thermometric means.One thermistor took the place of various indicators or electrode systems used in other techniques and maintenance was simple. At this stage of instrumenta- tion however it was not possible to work with such low concentrations as were possible with potent iome t ric techniques. Sensitivity of measurement was of the order of 0-001°C. Some typical reactions that had been studied were illustrated. Development of an Automatic Titrator with Digital Readaut BY P. T. PRIESTLEY AND M. SMITH (Research Laboratory Kodak Ltd. Wealdstone Harrow) MR. PRIESTLEY said that the recorded curve obtained in a thermometric titration showed a temperature ordinate and a titre abscissa in millilitres that was equivalent to the distance measured along the length of the chart.The straight-line portions of the curve were normally extrapolated to give the initial and end-points of the titration and the titre was given by the value of the distance between the points of intersection. This method of evaluating the titre was not satisfactory for routine operation as it was tedious and introduced sources of error. If the intial and end-points could be detected automatically then the burette delivery could be controlled so allowing measurement of the volume of titrant used in the titration. Alterna- tively with constant rate of delivery the time interval between the points could be auto- matically measured to give an evaluation of the titre. Zenchelsky and Segatto working in New Jersey during 1956 showed in a subsequent paper how the first and second derivatives of the temperature - time plot could be used to obtain sharper discrimination of the initial and end-points of the thermometric titration.They proposed an upper limit in titrant-addition rate of 2 ml minute-l with 50 ml of titrand and in practice obtained rates of temperature change around 0.2" C minute-1 giving rise to an output of 1 mV minute-1 from their thermistor-bridge circuit. This small signal was amplified by using a servo-potentiometer system with a gain of lo5 and the amplified voltage was differentiated by two resistance - capacitance networks each having a time constant of 0.5 second. The titre was evaluated by measuring the distance between the two resulting peaks corresponding to the initial and end-points of the titration.February 19661 THERMOMETRIC TITRIMETRY 19 Mr. Priestley said that Zenchelsky and Segatto's apparatus together with his own method of vibration stirring had led him to believe that higher rates of titrant addition were possible thereby giving higher rates of change of temperature with time and allowing relatively simple electronic circuits to be used in the construction of an automatic titrator. A prototype was constructed which used a syringe burette with a constant rate of 7 ml minute-1 and which gave a typical output of about 50 mV minute-l substantially larger than that obtained by Zenchelsky. The signal from the thermistor was filtered and differentiated by a resistance - capacitance network with a time constant of 50 milliseconds. The resulting square wave was amplified by a transistorised amplifier to give a useful signal whose time period was the required time or titre of the titration.The end-point detector comprised a transistorised relay circuit that could detect sudden changes in its input voltage. The relay therefore changed state as soon as the thermistor in the titrand detected a change of temperature due to the start of the titration and it reverted to its original state when the temperature stopped changing at the end-point. The burette which incorporated an electro-magnetic counter was driven by a syn- chronous motor and micrometer-screw mechanism that imparted linear motion to the piston of a glass syringe. The latter was fitted with a pair of non-return valves arranged so that fresh titrant was introduced into the syringe from a reservoir when the piston was withdrawn whilst in the other direction titrant was dispensed through a delivery arm into the vessel containing 25 ml of titrand.During a titration the timer was set to count automatically when the rate of temperature change exceeded 0.5" C minute-l. At the end-point the timing counter stopped no further titrant was dispensed and the burette automatically refilled. The 50 cycles second-1 mains frequency was used as a timing standard and titres were shown to a precision of 0.02 second in a useful titre range of say 5 to 20 seconds (0.5 to 2-0ml of titrant). The titrator has been used with titrations involving neutralisation chelation precipita- tion and redox reactions. In general the 2-sigma (2 standard deviations) reproducibility was about 1 per cent.Thermometric Titrations of Some Precipitation Reactions BY R. J. N. HARRIES (Neath Technical College Neath Glamorgan) MR. HARRIES described an apparatus that was suitable for carrying out thermometric titra- tions comprising a 600-ml silvered Dewar flask as reaction vessel and a thermopile for tempera- ture measurement. The thermopile was made of 30-s.w.~. copper wire and cotton-covered 24-s.w.~. Eureka resistance wire each junction being soldered and contained in a thin-glass tube. Some mercury was placed at the bottom of each glass tube in order to immerse the junction and facilitate heat transfer. Twelve cold junctions and twelve hot junctions were constructed. Each wire of the thermopile was about 50 cm long and it was found to produce 0.0006 volt "C-l.A glass stirrer operating at about 300 r.p.m. was used to stir the reaction mixture. The stirrer motor was not synchronous. The burette was constructed from a uniform graduated glass capillary tube and delivered 0.10 ml of titrant in 15 seconds. A thin capillary tube was used to introduce the titrant into the solution in the reaction vessel. It was made to dip just below the surface of the reacting liquid. The relative positions of thermopile stirrer and burette tip did not appear to be critical . The voltage from the thermopile was balanced on a Tinsley 3387B potentiometer with a 2-volt accumulator fitted with a voltage dropper as a storage cell. A Pye Scalamp galvano- meter was used as the null-point detector its graduated scale was removed and it was adapted for use with a wall scale 70 cm away.Mr. Harries outlined the procedure in which a measured volume of the solution to be analysed was placed in the Dewar vessel and if necessary diluted so that a reasonable galvano- meter deflection was obtained on introducing 0.1 ml of titrant. The minimum volume that could be used was 25 ml or the thermopile would not be in contact with the solution. The 20 THERMOMETRIC TITRIMETRY [Proc. SOC. Analyt. Chem. stirrer was switched on and when thermal equilibrium was reached the burette tip was intro- duced. The titrant temperature and laboratory temperature were not controlled. After 0.1 ml of titrant had been delivered into the reaction vessel the potentiometer reading was taken for at least five readings after the end-point. A graph of potentiometer reading against volume of titrant was drawn from which the end-point could be deduced.Silver nitrate titrations.-Satisfactory results were obtained with chloride bromide iodide ferric yanide t hiocyanat e oxalat e nitroprusside and chromate . With potassium dichromate the formation of silver chromate was indicated; this was verified by analysis of the precipitate (Ephraim Inorganic Chemistry 5th English Edition Gurney and Jackson). Potassium cyanide showed two arrest points corresponding to AgCN and Ag(CN),-. With potassium ferrocyanide the formation of the heterometallic supercomplex K(Fe(CN),Ag3) was shown by an intermediate arrest point the final compound being Attempts to analyse orthophosphate pyrophosphate acetate and cobaltinitrite failed because of their small heats of reaction.An attempt was made to analyse mixtures of chloride bromide and iodide but this was only partially successful becaus e co-precipitatio n occurred. Co-precipitation was found to be least with iodide - bromide mixtures and most with bromide - chloride mixtures. It was also found that co-precipitation was least when the halides were present in equimolecular proportions. Iodide - bromide analysis was accurate to 1 per cent. when the ratio of I- to Br- was 1 to 1 but could fall to as much as 10 per cent. if the ratio of I- to Br- was 4 to 1 or 1 to 4. Chloride - bromide analysis was more strongly affected by co-precipitation the ratio of chloride found to chloride added being as high as 1.385 when the ratio of Br- to C1- was 4 to 1.’ (Kolthoff and Stenger Volumetric Analysis Volume I 2nd revised Edition Interscience Publishers Inc.and Clarke J. Chem. SOC. 1926 768). It was found that the addition of neutral electrolyte to decrease co-precipitation was unsuccessful. In all mixed- halide titrations the total halide was found with an accuracy of less than 1 per cent. Mercwous nitrate titrations.-Chloride bromide oxalate cobalticyanide and nitro- prusside gave satisfactory results. Thiocyanate and iodide titrations failed because of dis- proportionation of the mercurous compounds initially formed. With potassium ferrocyanide an intermediate arrest point indicated the formation of a heterometallic supercomplex I(,(Fe(CN),Hg,) that could not be isolated because of its de- composition into products varying in colour from pale green to dark blue. The final com- pound was Hg,(Fe(CN),Hg2) which was stable and was isolated and analysed.Ag(Fe(CN)6Ag3)* With potassium permanganate no stoicheiometry was found. Acetone as Solvent in the Enthalpimetric Titration of Acidic Substances BY G. A. VAUGHAN (Coal Tav Reseavch Association Gomevsal Leeds) MR. VAUGHAN said that the enthalpimetric titration of acidity with a non-aqueous alkali often showed only a light change in slope at the end-point but it had been found that if acetone was used as the solvent for the acid it acted as an “indicator.” A rapid rise in temperature occurred at the neutralisation point due to the formation of diacetone alcohol from the reaction of the acetone with the excess alkali. In order to make use of this “indicator” action it was necessary that the acetone was dry and as free from carbon dioxide as possible the non-aqueous titrant was concentrated and added continuously with stirring and if the sample had been dissolved in another solvent at least three times its volume of acetone had to be used. The method was applicable to a wide range of acidic substances including 2,6-disubstituted phenols keto-enols and imides and could also be used to determine traces of acidity. The complete paper has been published in The Analyst 1965 90 594.

ISSN:0037-9697    

DOI:10.1039/SA9660300016

出版商:RSC    

年代:1966

数据来源: RSC

摘要:

February 19661 EFFLUENT ANALYSIS 21 Effluent Analysis The following are summaries of papers presented at the Joint Meeting of the Midlands Section with the Guild of Associates of the College of Advanced Technology Gosta Green held on December 7th 1965 and reported in the January issue of Proceedings (p. 2). Examples of the Use of Empirical Methods in the Analysis of Complicated Effluents BY F. G. BROUGHALL (The Midland Tar Distillers Ltd. Oldbury Birmingham) MR. BROUGHALL referred to previous papers dealing with particular aspects of effluent analysis during the design of methods and plant for the pre-treatment of chemical-works effluent and to standard works on analysis of sewage and trade waste.* He stressed the value of empirical methods with certain types of effluent. The particular effluents investigated were produced during operations connected with the distillation and refining of coal tar in which water was contaminated by contact with tar and tar oils.The main oxygen-absorbing bodies present were monohydric phenols polyhydric phenols and thiocyanate. In previous published work on effluents of the gas - liquor type that were of similar composition to those produced during tar distillation the substantial difference between the permanganate value found and the permanganate value calculated from the results of the analysis was obvious. It had long been suspected that the difference found when attempting to balance the oxygen absorbed by such an effluent with the oxygen equivalents of the compounds identified by chemical analysis was due to the presence of polyhydric phenols and their oxidation products.The available methods for determining polyhydric phenols as such and as “total phenols” were not entirely satisfactory but no method was available for determining the oxidation products. Some of the aspects of the behaviour of polyhydric phenols in effluents could be explained on the assumption that atmospheric oxidation proceeded in stages which probably involved condensation between molecules resulting first in highly coloured water- soluble products and then resinous insoluble materials. Arising from experiments designed to recover the residual oxygen-absorbing material after biological oxidation of such effluents a method of “evaporation analysis” had been developed in which the total polyhydric phenols oxidised and unoxidised were precipitated by evaporating the effluents to dryness.The volatile products were collected by a preliminary distillation through a condenser and in order to meet the requirements of the investigation in hand the contaminating materials were assessed in terms of permanganate value. The difference between the original permanganate value and the sum of the permanganate values of the volatile material in the distillate and the water-soluble material after evaporation and filtration gave a value for the precipitated material that had been shown to be related to the total polyhydric phenols. This method had been used to explain the behaviour on biological oxidation of certain effluents containing polyhydric phenols that changed on storage. A laboratory activated sludge unit had been fed with samples of fresh effluent from a pre- treatment plant discharging to a sewer system.Portions of the feed had been put into stock with limited access to air during the filling up of the stock bottle. After several weeks a stock of liquor which was known to respond to biological treatment when fresh was available in a partly oxidised state. When fed to the laboratory treater an inferior effluent was produced and the differences between it and the original were shown in the “evaporation analysis,” the precipitated material being nearly five times greater. A pre-treatment process for effluent liquors containing polyhydric phenols was under investigation and involved atmospheric oxidation in the presence of lime. The evaporation analysis was not precise but gave results that were sufficiently complete to explain several aspects of the behaviour of this liquor.If the precipitation was complete the water-soluble * Ministry of Housing and Local Government “Methods of Chemical Analysis as applied to Sewage and Sewage Effluents,” H.M. Stationery Office 1956 ; Association of British Chemical Manufacturers and the Society for Analytical Chemistry “Recommended Methods for the Analysis of Trade Effluents,” W. Heffer & Sons Ltd. 1958; American Public Health Association “Standard Methods for the Examination of Water etc.,” Various Editions; Isaac P. C. G. Editor “Waste Treatment (Proceedings of the Newcastle Symposium),” Pergamon Press 1959 p. 240; J . PYOG. Inst. Sew. Purif. 1960 3 248. 22 EFFLUENT ANALYSIS [Proc. SOC. Analyt. Chew. material after filtration should consist entirely of inorganic salts but organic material was still present most of which could be absorbed by carbon.This extension to the original method involving the use of active carbon had been used to show the changes that took place in pre-treated effluent on storage and to show that similar material could be produced during biological oxidation i.e. the material that was not readily absorbed by carbon appeared to constitute most of the residual oxygen-absorbing material remaining after biological oxidat ion. Determination of Some Inorganic Constituents of Trade Effluents BY N. T. WILKINSON (Imperial Chemical Industries Mond Division Research Depavtrutent P.O. Box 7 Northwich Cheshive) MR. WILKINSON stated that in the Association of British Chemical Manufacturers and the Society for Analytical Chemistry’s Joint Publication “Recommended Methods for the Analysis of Trade Effluents,” all the methods of analysis described were chemical and that the only reference made to physical methods of analysis was an appendix outlining the use of flame photometry.He considered that because of the developments made in other physical methods such as polarography X-ray fluorescence and atomic absorption recommendations should be made regarding the use of these methods and guidance given on their value compared with chemical methods so that the analyst would be able to decide on the most efficient and economical method of carrying out a particular analysis. He considered however that there was still a great demand for the use of chemical methods of analysis and it was important to know in using a particular chemical or physical method the effect that various substances had on the analytical method Mr.Wilkinson described recent work he had carried out on the colorimetric determination of mercury present as a mercury salt in effluents containing sodium carbonate. On acidifica- tion some of the mercury had been lost by evolution with the carbon dioxide liberated. He also described the interference that occurred when the solution was acidified with sulphuric acid. Modifications to the existing recommended method were stated and results shown were of a high order of accuracy. The lecturer continued by describing his recent work on the titrimetric determination of calcium and magnesium with standard EDTA solution in the ranges 1 to 70 p.p.m.of calcium and 0.5 to 20 p.p.m. of magnesium. The titration of calcium in a solution with a pH above 12 had been first carried out and followed by the titration of magnesium after the pH of the solution had been adjusted to 10. The effect of a number of anions and cations was demonstrated. The titrimetric determination of calcium in the range 0.02 to 0.4 p.p.m. and of magnesium in the range 0.01 to 0.1 p.p.m. with Solochrome Black as indicator and with a spectrophotometer to determine the end-points was described. It was shown that in solutions containing high concentrations of calcium magnesium and phosphate the calcium and magnesium could be determined accurately and quickly by the spectrophoto- metric technique after suitable dilution of the sample. A few years ago the determinations could only be made gravimetrically after a basic acetate separation of the phosphate Other methods briefly dealt with were the colorimetric determination of fluoride (reference being made to the recently published method developed in the Government Laboratory) the volumetric determination of sulphate by the thoron and sodium rhodisonate methods and the determination of iron by the 1 ,lo-phenanthroline 2,2’-bipyridyl and the 4,7-diphenyl-l,lO-phenanthroline (bathophenanthroline) methods.The effect of a number of anions and cations on these methods was mentioned. Determination of Organic Matter in Sewage and Trade Wastes and some Observations of the Determination of Cyanide BY S. H. JENKINS (Birmingham Tame and Rea Distvict Draivlage Board Tame Valley House Newhall Street Birmingharut 3) DR.JENKINS said that by means of laborious analytical procedures it was possible to identify specific compounds in mixtures of sewage and trade wastes but that it was only by looking February 19661 EFFLUENT ANALYSIS 23 for groups of compounds such as fatty acids glycerides or carbohydrates that most of the organic matter in such mixtures could be accounted for. Even then the result would be applicable only to a particular sample and comparisons between the results obtained on such a sample and the results of analysis of other samples would be difficult to make. This was because of the variation in composition that might result from differences in dietary habits the presence of trade wastes and the ease with which sewage underwent changes in com- position caused by the activity of micro-organisms.Consequently it was necessary to use empirical methods of analysis that attempted to measure all the organic matter. The chemical methods of measurement were the permanganate value chemical oxygen demand and organic carbon. The permanganate value had the disadvantage that only a small proportion of the organic matter in sewage was oxidised whereas in some trade wastes the proportion oxidised was much larger. It therefore became difficult to make valid comparisons between the relative strengths of sewage and trade wastes on the basis of this test alone. Chemical oxygen demand suffered less from this disadvantage but both with sewage and trade waste a proportion of the organic matter that was oxidised under the conditions of the chemical oxygen demand test (reaction of the sample at the boil with dichromate and sulphuric acid) was not oxidised by biological treatment at a sewage purification works.The content of biologically oxidisable matter in a sample containing polluting matter could be determined by means of the test for biochemical oxygen demand. In this test the proportion of the dissolved oxygen in a dilution of the sample and the oxygenated water used up in 5 days at 20" C in the oxidation of organic matter by the bacteria present multiplied by the dilution factor was taken as a measure of the content of biologically oxidisable material. This test had several disadvantages the main objections were the artificial conditions introduced by the dilution and the cessation of the test before the process of biological oxidation had been completed.Another test consisted of the direct measurement of the oxygen absorbed by the polluting liquid when it was shaken in a closed system in the presence of excess oxygen. The sample could for this purpose be mixed with a culture of organisms or with activated sludge (which was a mixture of organisms and organic matter derived from sewage organic matter) in order to accelerate the rate of oxidation. Warburg or other forms of respirometer could be used for such a manometric measure of oxidisability. One of the advantages of the biological method of determining organic matter was that the rate of oxidation of sewages or trade wastes could be determined as well as the possible toxic effects of trade wastes on the oxidation of a standard substance such as glucose in the presence of activated sludge.Examples were given of the results obtained by these various procedures. Dr. Jenkins mentioned that it was important to be able to measure the concentration of toxic substances in trade wastes preferably by chemical methods. One such toxicant was cyanide. However cyanide had different toxic properties depending upon whether it was present either as simple cyanide or complexed with heavy metals or as ferrocyanide. The officially recommended method of separating the ferrocyanide cyanide from the remaining cyanide was to distil the liquid with lead acetate which did not decompose ferrocyanide. However it had been proved that some of the heavy-metal cyanide complexes had not been completely decomposed under these conditions. Attempts had been made to separate the cyanide present as hydrogen cyanide sodium cyanide and potassium cyanide by aeration in a closed system absorbing the evolved hydrogen cyanide in alkali. The recovery was almost complete at pH values of below about 5 but under these conditions heavy-metal cyanides had been decomposed to varying degrees. Aeration for periods of 1 hour at buffered pH values showed that recoveries of cyanide of over 80 per cent. could be obtained but it had been proved that the constituents of the buffer exerted an effect on the recovery values. Dr. Jenkins concluded by saying that the position at present time regarding the separation of free cyanide from the heavy-metal cyanides was far from satisfactory and work on this subject was continuing in his laboratory. However the test was universally used.

ISSN:0037-9697    

DOI:10.1039/SA9660300021

出版商:RSC    

年代:1966

数据来源: RSC

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,24 OBITUARY [Proc. SOC. Aaalyt. Chem. Obituary ALBERT LESTER WILLIAMS ALBERT LESTER WILLIAMS President of the Association of Public Analysts died on October lst 1965 after a very short illness. It must be rare in the history of an Association to lose through premature death its own President during his term of office and with one as small as the A.P.A. where the President is known intimately to practically all its members the shock at such a loss is all the more personal. Williams was born in Yorkshire in 1902 and was educated at Hanson’s High School in Bradford where he obtained a scholarship to Leeds University. During his training there he attended a course in Food and Drugs which undoubtedly laid the foundation for his future $career. Williams appeared to have adopted his profession at a very early age and instead of proceeding to a degree in the usual way he chose to take the Examination for the Diploma in Food and Drugs of the Institute of Chemistry and to obtain his professional qualification in this manner.He even spent his vacations working in the laboratory of the local public analyst under the late B. A. Burnell. In 1926 he was appointed junior assistant to Mr. J. F. Liverseege the public analyst for Birmingham and some of his colleagues at that laboratory remember him well as a young man full of the enthusiasm that led him to construct in wood glass and metal the numerous “aids to analysis” that make the work of any analyst so much easier. H. H. Bagnall who followed Liverseege as public analyst and Lerrigo who later left the profession of public analyst for other spheres were two of his associates in Birmingham.In 1938 he was appointed Deputy Public Analyst. The opportunity for further advancement came with the retirement of Mr. R. P. Page public analyst for Portsmouth and Williams was chosen by the elected representatives of this famous city to fill his place. He remained there until his death whilst in full harness and at the top of his profession. It is not always easy for a northerner to accommodate himself to a southern city but Williams did so with such success and to the complete satisfaction of his employers that it is difficult to imagine a happier relationship. He was thought of with great esteem both at Committee and Council levels and the Portsmouth Laboratory under his guidance became one of the foremost in the country.Williams was a Rotarian and entered enthusiastically into the social activities in and around Portsmouth. I doubt however whether any of his activities outside his own laboratory and his home gave him greater pleasure satisfaction and scope for service to others than membership of the Association of Public Analysts. He had a knack of getting on with all types of people and this together with his love of argument and discussion combined with unusual persuasive powers made him invaluable to the Association in its endeavour to raise the status of Public Analysts. But for his persistence many of us would have recoiled from the effort involved in preparing the data and marshalling the arguments necessary before a meagre improvement in salaries and conditions of service could be effected.He must often have felt frustrated but he never allowed his feelings to subdue his optimism and his knowledge of the ways in which local government “works” had always been the basis of the advice and guidance that he gave the Association. The same traits of character have proved invaluable in other spheres of activity too and more particularly in the negotiation with the Trade of various Codes of Practice. He will be sadly missed. In 1962 Williams was elected Vice-president of the Association of Public Analysts and proceeded to the Presidency in 1964. He threw himself whole-heartedly into the extra work involved and in spite of failing health due to recurring attacks of asthma and bronchitis he never flagged and his loyalty to his office and his colleagues was maintained until the very end.He leaves a wife and two sons. D. D. MOIR February 19661 PAPERS ACCEPTED FOR PUBLICATION Changes in the Register of Members NEW MEMBERS 25 ORDINARY MEMBERS Terence Allen M.Sc.(Lond.) ; James Ashley- Jones F.R.I.C. ; John Edward Bagness B.Sc. (Lond.) M.Sc. (Leeds) ; Derrick Phillips Barker A.R.I.C. ; Richard Beeby A.R.I.C. ; Joseph Clair Brown B.Sc.(Lond.) F.R.I.C. ; Alan Calderbank B.Sc.(Lond.) Ph.D.(Cantab.) ; John Arthur Caldwell B.Sc. (Lond.) F.R.I.C. ; Victor Terrell Crowl B.Sc. Ph.D. (Lond.) D.I.C. A.R.C.S. F.R.I.C.; George Edward Peter Elliott Ph.D.(Southampton) A.R.I.C.; Anthony Fewell B.Sc. (Lond.) ; Harold Keith Gelder Dip.Tech. A.R.I.C. ; Geoffrey Horrocks A.R.I.C. A.R.T.C.S. ; Michael David Howarth; Jeremiah Kelleher M.Sc.(Cork) A.R.I.C. ; Hwang Kyohyun; Paul Emmett Luton; John Lewis Martin A.R.I.C.; Albert Ernest Joseph McGill B.Sc.(Q.U.B.) ; Mario Milone Dr.Chem.(Torino) ; Graham Nickless B.Sc. Ph.D. ; Charles Deric Ratcliffe B.Sc. A.R.I.C. ; Geoffrey Arthur Hammond Roberts M.A. B.Sc.(Oxon.) F.R.I.C. A.F.Inst .Pet. ; Brian Rogers B.Sc. (Lond.) A.R.I.C. ; Walter Sidney Sebborn B.Sc.(Lond.) A.R.I.C.; Alan Dalton Scott B.Sc. Ph.D.(Lond.) F.R.I.C.; Henry James Scullion B.Sc. A.R.I.C. F.R.S.S. ; Wilhelm Simon Dipl.Ing.-Chem. E.T.H. Dr.sc. techn. ; Terence Brain Smallwood L.R.I.C. ; James Edward Stanfield M.A. B.Sc. (Oxon.) ; Colin George Taylor M.Sc. Ph.D.(Lond.) A.R.I.C. ; David George Westmoreland B.Sc.(Manc.) ; Derek Albert Whitlock ; Johan Gunnar Widmark Dr. (Stockholm) ; John Raymond Wool- dridge B.A.(Cantab.) M.Sc.(Lond.).JUNIOR MEMBERS Barry Kenneth Cooke; Christopher Alan Dawes; Arthur William Alan Leek D.L.C. ; Barry Nicholls. DEATHS We record with regret the deaths of Ronald Moxon Roger Tully Postlethwaite Stephen Matthew Austin Whettem. Papers Accepted for Publication in The Analyst THE following papers have been accepted for publication in The Analyst and are expected to appear in the near future. “A Precise Coulometer,” by J. C. Quayle and F. A. Cooper. “Precise Coulometry The Titration of Pure Sodium Carbonate,” by F. A. Cooper and “Simultaneous Determination of Iodine and Bromine in Urine by Neutron-activation “The Determination of the Zirconium Oxide of Rutile with Alizarin Red S.,” by N. B. “Quasi-Quantitative Separation of Paraffins and Olefins,” by J. A. Spence and “The Collection of Fractions Separated by Gas - Liquid Chromatography,” by M. D. D. “An Automatic Apparatus for the Determination of Titanium,” by C. L. Denton and “The Determination of Water in Lubricating Oils by a Near-infrared Spectrophotometric “The Effect of Particle Size on Back-scattered X-ray Correction Methods in On-Stream “Micro Determination of Inorganic Phosphorus in Plasma,” by B. B. Bauminger and “The Micro Determination of Cyanide,” by S. Baar. “Spectral Characteristics of Eugenol,” Report prepared by the Essential Oils Sub- J. C. Quayle. Analysis,” by A. G. Souliotis and E. P. Belkas. S t anton. M. Vahrman. Howlett and D. Welti. J. Whitehead. Method,” by B. D. Pearson. X-ray Fluorescence Analysis,” by K. G. Carr-Brion. G. Walters. committee of the Analytical Methods committee.

ISSN:0037-9697    

DOI:10.1039/SA9660300024

出版商:RSC    

年代:1966

数据来源: RSC

摘要:

26 PUBLICATIONS RECEIVED [Proc. SOC. Analyt. Chew. Notices BRITISH STANDARDS INSTITUTION DRAFT SPECIFICATIONS A FEW copies of the following draft specifications issued for comment only are available to members of the Society and can be obtained from the Secretary Society for Analytical Chemistry 14 Belgrave Square London S.W.l. Draft Specification prepared by Sub-committee LBC/l l/l-Microchemical Apparatus D 65/14478-Draft B.S. Specification for Carbon and Hydrogen Combustion Train Draft Specification prepared by Sub-committee CIC/ll/2-Food Colouring Matters D 65/14532-Draft B.S. Specification for Channel Black for Use in Foodstuffs. Draft Specification prepared by Sub-committee PVC/lB-Ready Mixed Oil Paints. D 66/432-Draft B.S. Specification for Permissible Limit of Lead in Low-lead (Drafting).(Pregl Type) (Revision of B.S. 1428 Part Al). (Non-Coal-Tar) . Paints and Similar Materials. February 19661 NOTICES 27 MIDLANDS SECTION ELWELL AWARD 1967 THE object of this award is to encourage young Midland scientists in the profession of ana- lytical chemistry. Entries are invited for the annual competition for the Elwell Award from any scientist including those engaged in full-time post-graduate studies under the age of 30 working or residing in the area covered by the Midlands Section of the Society for Analytical Chem- istry; vix. south of but including Stoke-on-Trent and north of but excluding Carmarthen. The Award consisting of a silver trophy will be retained for one year by the candidate deemed by a panel of referees to have submitted the best paper dealing with some aspect of analytical chemistry.In addition the successful candidate will receive a gift of scientific books of his own choice to the value of 10 guineas; the runner-up will receive scientific books t o the value of 3 guineas. Papers submitted should describe in a form suitable for presentation at a local Section Meeting work in which he or she has been actively associated though not necessarily entirely responsible. The basic requirement is that the contribution should advance even in a small way existing knowledge of analytical chemistry. Selected papers will be presented at a Meeting of the Section during January 1967 and the name of the successful candidate will be announced on the same evening. The closing date for entries is October 7th 1966 and the latest date for submission of papers is October 28th 1966.Entry forms and other particulars may be obtained from M. L. Richardson A.R.I.C. A.C.T. (Birm.) Honorary Secretary Midlands Section of the Society for Analytical Chemistry c/o John & E. Sturge Ltd. Lifford Chemical Works Lifford Lane Kings Norton Birmingham 30. PURE AND APPLIED CHEMISTRY THE OFFICIAL JOURNAL OF THE INTERNATIONAL UNION OF PURE AND APPLIED CHEMISTRY VOLUME 10 No. 2 1965 THIS issue contains the Plenary Lectures presented at the International Symposium on Microchemical Techniques held in Pennsylvania U.S.A. August 22nd to 27th 1965. The following lectures were presented “Microchemistry-the present and the future,” by P. J. Elving ; “Identification and determination of unusual functional groups,” by E. Sawicki; “Recent microtechniques in forensic science,” by P.L. Kirk; “The status and future of chemical microscopy,” by Maria Kuhnert-Brandstatter ; “Organic Microanalysis in Japan- past and future,” by T. Mitsui; “Microtechniques in the modern laboratory of chemical chemistry,” by S. Natelson ; “Photometric titrations,” by H. Flaschka ; and “Techniques in organic microsynthesis,” by V. Horiik. In addition it contains a report prepared by the Commission on Microchemical Tech- niques on “Recommended Test Substances for the Microdetermination of Various Elements and Functional Groups in Organic Compounds.” Pure and Applied Chemistry is published irregularly four issues per volume at E6 ( $18.00) per volume. Reprints may be purchased; all inquiries should be addressed to the publishers Butterworths 4-5 Bell Yard Temple Bar London W.C.2.SYMPOSIUM ON PYROLYSIS - GAS CHROMATOGRAPHY PARIS 1966 THE Symposium on Pyrolysis - Gas Chromatography will be held at the Ecole Polytechnique 17 rue Descartes F 75-Paris 5 on September 15th and 16th 1966. It will deal with the use of pyrolysis - gas chromatography in the analysis of non-volatile organic compounds mainly high polymers. Financial assistance for travel will be available from the organisers of the Symposium to authors of accepted papers from abroad. An abstract (not more than 500 words long) of the proposed paper will be required before June 15th 1966. Enquiries concerning the Symposium and registration and abstracts should be sent to Dr. G. Guiochon Ecole Polytechnique 17 rue Descartes F 75-Paris 5. Papers are invited on all aspects of pyrolysis - chromatography. 28 [Proc. SOC. Analyt. Chem. THE SOCIETY FOR ANALYTICAL CHEMISTRY announces the publication of “ANALYTICAL ABSTRACTS” DECENNIAL INDEX 1954 to 1963 This cumulative Index for Volumes I to 10 will be published in mid-1966 in two parts- Author and Subject sections Further details will be available shortly

ISSN:0037-9697    

DOI:10.1039/SA966030026b

出版商:RSC    

年代:1966

数据来源: RSC