摘要:

Proceedings of the Society for Analytical Chemistry CONTENTS Proc. SOC. Analyt. Chem. Vol. 7 No. 7 Pages 101-138 Third SAC Conference . . . . 101 New Members of Council . . 101 Summaries of Papers “Recent Advances in Pharma- ceutical Analysis with Special Reference to Microchemical Techniques” . . .. . . 104 “Presentation of Particle-size Distributions” . . . . 113 Methods Committee 1969 . . I14 Report of the Analytical Obituary . . .. . . . . 134 Membership Changes . . . . 134 Papers Accepted for The Analyst I35 Publications Received . . . . 135 Notices . . . . . . . . 136 Forthcoming Meeting Back cover July 1970 Vol. 7 No. 7 July 1970 PROCEEDINGS THE SOCIETY FOR ANALYTICAL CHEMISTRY OF President of the Society T. S. West Hon. Secretary of the Society W. H. C. Shaw Hon. Treasurer of the Society G.W. C. Milner Hon. Assistant Secretary of the Society D. 1. Coomber Secretary Miss P. E. Hutchinson 9/10 SAVILE ROW LONDON WIX IAF Telephone 01-734 6205 Editor J. B. Attrill Assistant Editor Miss C. M. Richards Telephone 01-734 3419 Proceedings is published by The Society for Analytical Chemistry and distributed to all members of the Society and t o subscribers with The Analyst subscriptions cannot be accepted for Proceedings alone. Single copies may be obtained direct from the Society’s Distribution Agents The Chemical Society Publications Sales Office Blackhorse Road Letchworth Herts. (NOT through Trade Agents) price 0 The Society for Analytical Chemistry 5s. post free. Remittances MUST accompany ordkrs. THE SOCIETY FOR ANALYTICAL CHEMISTRY A Special Meeting of the Society in conjunction with its Special Techniques Group will be held on Monday August loth 1970 at 3 p.m. in Lecture Theatre C Mechanical Engineering Department Imperial College Exhibition Road London S.W.7. at which Professor G. G. Guilbault (Lowisiana State University in brew Orleans U.S,A .) will lecture on “Use of Fluorescence Assay Procedures in Analytical Chemistry” fore this Meeting the Analytical Research School of Imperial College has organised Professor Guilbault’s subject will Members of the Society a seminar a t I 1 a.m. in the Chemistry Department. be “Enzyme Electrode Probes for Analysis in Clinical Chemistry.” and their guests will be welcome to attend this seminar.

ISSN:0037-9697    

DOI:10.1039/SA97007FX025

出版商:RSC    

年代:1970

数据来源: RSC

摘要:

THE SOCIETY FOR ANALYTICAL CHEMISTRY Forthcoming Meeting August Monday 10th LONDON SOCIETY Special Meeting in conjunction with the Special Techniques Group. “Use of Fluorescence Assay Procedures in Analytical Chemistry” by Professor Lecture Theatre C Mechanical Engineering Department Imperial College G. G. Guilbault. Exhibition Road London S.W.7; 3 p.m. Printed by W Heffer &Sons Ltd Cambridge England

ISSN:0037-9697    

DOI:10.1039/SA97007BX027

出版商:RSC    

年代:1970

数据来源: RSC

摘要:

July 1970 Vol. 7 No. 7 New Members of Council RONALD BELCHER Professor of Analytical Chemistry at the University of Birmingham and a retiring Vice-president is now one of the elected Ordinary Members of Council. He was awarded the Society’s Gold Medal in 1968; a brief biography and a portrait were published on that occasion (Proceedings 1968 5 235). DR. D. BETTERIDGE Lecturer in Chemistry at the University College of Swansea and retiring Chairman of the Western Section is now an Ordinary Member of Council; a short biography and a portrait appeared in Pyoceedings 1968 5 111. He is at present engaged on research into the application of photoelectron spectroscopy to analysis. 101 102 NEW MEMBERS OF COUNCIL [PYOC. SOC. Analyt. Chem. MR. E. BISHOP was educated at Allan Glen’s School and took Firsts in Chemistry and Chemical Engineering at Glasgow University and the Royal College of Science and Technology having collected sufficient prizes and scholarships to provide the necessary books and finance.He also took an A.R.C.S.T. and an A.R.I.C. in 1942 becoming a Fellow in 1960. During the war he served in the Explosives Directorate of the Armaments Research Department until invalided out in 1944 when he became an assistant lecturer in what is now the University of Strathclyde. He moved to a lectureship at King’s College Newcastle-upon-Tyne in the University of Durham in 1946 and from there in 1953 to the University of Exeter where he is now Reader in Analytical Chemistry. The author of some 90 papers in intervals between designing chemistry buildings his research interests centre on the mathe- matical theory of analytical processes electroanalytical chemistry and the kinetics and mechanisms of analytical reactions with a bias towards titrimetry and odd excursions into trace and ultramicro work.He joined the Society in 1948 has twice before served on Council and has served on the A.M.C. since 1959. A past member of the Microchemical Methods Group Committee (and Chairman of its Standards Sub-committee) The Analyst Editorial Committee and the Talanta Editorial Board he is currently Chairman of the Analytical Standards Sub-committee of the A.M.C. and of its Compleximetric Standards Panel of B.S.I. Committee CIC/26/-/I of the University Chemical Colloquium and President of the University of Exeter Chemical Society. He also serves on The Analyst Editorial Advisory Board the Joint Panel on Microchemical Standards and Reagents B.S.I.Committee CIC/-/l the Regional Advisory Board on Further Education the Board of Governors of the North Devon College of Technology and as a Titular member of IUPAC Commission V-5 on the Analytical Sub-committee of the British National Committee for Chemistry. A former youth and social worker deacon and lay preacher when the rare opportunity arises he enjoys music ballet pre-renaissance literature wines the countryside swimming and playing village cricket. DR. W. T. ELWELL has been attached to the Analvtical Laboratories of I.C.I. for the whole of his working career and is currently Chief Analyscof Imperial Metal Industries a subsidiary of I.C.I. Before going to the Midlands in 1955 he had been in the Company’s Billingham Laboratories for over 25 years during which time he qualified by examination for both the Associate- ship and the Fellowship (Branch H) of the R.I.C.For several years he was a part-time Lecturer (Hons. B.Sc.) at the Constan- tine Technical College Middlesbrough was associated with the formation of the Teesside Section of the R.I.C. and its Treasurer for many years. Since coming to the Midlands he and his I.M.I. colleagues have been responsible for over 60 external publications and 5 books (excluding subsequent editions and reprints) the latest “Analysis of the New Metals,” he wrote with D. F. Wood. His laboratory was probably the first industrial laboratory to exploit the potentialities of atomic-absorption spectrophotometry and his book with J. A. F. Gidley as a co-author was the first to be published on the subject; it is now in its second edition reprint.He has been a member of the Society for 30 years and has taken an active part in the Midlands Section of the Society for the past 15 years. For example he was its Chairman in 1966-67 sponsored the Elwell award in 1959 and was Secretary and Chairman of the Birmingham International Symposia in 1958 and 1969 respectively. July 19701 NEW MEMBERS OF COUNCIL 1 03 Dr. Elwell has served as a member of Council over two previous periods and in 1967-8 was a Vice-president. He has served on the Analytical Methods Committee and is currently a member of T h e Artalyst Editorial Board The Analyst Executive Committee the Finance Committee and the Third SAC Conference Committee. He was the first Chairman of the Society’s Atomic-Absorption Spectroscopy Group (now Atomic Spectroscopy Group).He is a member of several Analytical Committees e.g. B.S.I. B.N.F.M.R.A. British Chemical Standards and AGARD (a N.A.T.O. Panel for the Analysis of Refractory Metals he is co- editor of its publications). He is an editorial advisor of Artalytica Chimica Acta and an Honorary Lecturer in Chemistry at Birmingham University; he has recently been awarded a Ph.D. degree by that University. MR. G. E. PENKETH was educated at Stockton Grammar School and joined the Billingham Division of I.C.I. in 1945 training as an analyst under the late H. N. Wilson. He obtained an external London University B.Sc. degree in chemistry in 1951 and became an Associate of the Royal Institute of Chemistry in the same year.After 2 years in the Research Department at Billingham working on polyphosphates and other inorganic polymers he joined the Analytical Research Section where he worked mainly on instrumental methods and in particular on spectroscopy and polarography. He was transferred to the Heavy Organic Chemicals Division of I.C.I. on its formation in 1958 where his interest in gas and liquid chromatography developed. From 1960 he spent 18 months on production as a member of a process investigation section and was appointed Section Leader of the Analytical Research Section in 1961. He became Analytical Research Section Manager in 1963 his ap- pointment as Analysis Manager for the Division was made in 1966. He has served on several committees of such bodies as the Institute of Petroleum is a member of the Chemical and Chem- ical Engineering Advisory Committee of Constantine Technical College (now Teesside Poly- technic) and is a second referee for The Chemical Society.During 1967 and 1968 he travelled extensively in Canada and the U.S. as a member of the I.C.I. recruitment team. His interests in analysis are very broadly based and this is reflected in the wide variety of his published papers which range for example from a novel electrode system for cathode-ray polarography to the determination of butadiene polyperoxide. He is married with three children and his hobbies include gardening painting and coin collecting. He is interested in most sports and plays tennis and badminton regularly. CECIL L. WILSON comes from Co. Londonderry which in the light of present day occurrences may have something to do with the survival of the fittest.B.Sc. (1932) M.Sc. (1933) and D.Sc. (1953) of The Queen’s University Belfast he was a Mus- grave Student at Glasgow University awarded the Ph.D. in 1936. There he first met microchemistry (under D. T. Gibson). Return- ing to Belfast (Assistant Lecturer 1935) he introduced micro- chemistry to the Honours course. His first book “An Introduc- tion to Microchemical Methods,” appeared in 1938. Nominally a lecturer at the Sir John Cass College (1939 to 1946) he spent 1940 to 1944 in the Armaments Research Depart- ment. In 1946 he returned as lecturer to Belfast. One of the founder members of the Microchemistry Group in 1944 he was later elected Chairman of the Group for 1951 and 1952. In Belfast he aimed to develop the teaching of analytical chemistry and instituted research in ultramicro inorganic analysis.In 1950 he was appointed a Reader ; from 1958 to 1963 he held a personal Chair in Analytical Chemistry converted in 1963 into an established Chair in Analytical and Inorganic Chem- istry; in 1968 this became an established Chair in Analytical Chemistry. 104 NEW MEMBERS OF COUNCIL [Proc. SOC. Analyt. Chem. A member of the Council of the Society in 1951-52 and in 1966-67 he has been a member of the Programmes Committee since 1966. He was elected an Honorary Member of the Austrian Microchemical Society in 1955 and a Member of the Royal Irish Academy in 1967. He has been Chairman of the Local Section of the R.I.C. and District Member of Council in 1948-51 1954-57 and 1959-60. Since 1952 he has been Document Examiner to the Ministry of Home Affairs Northern Ireland.He has been the co-author of a number of books on analytical and inorganic chem- istry is co-editor of “Comprehensive Analytical Chemistry” and was Editor-in-Chief of Talnnta for 8 years. He is one of the six academic members on the Senate of The Queen’s University and from 1966-1969 was Dean of the Faculty of Science. MR. DAVID W. WILSON was born in Northern Ireland where he received his formal education with additional instruction from poachers poteen distillers and publicans. He was appointed Assistant Lecturer in The Queen’s University of Belfast just before the war and then migrated under the auspices of the Armaments Research Department of the Ministry of Supply first to Stafford- shire (where he had difficulty with the language) and then to London.After the war following a short period with the Northampton Polytechnic (now the City University London) he joined Sir John Cass College (now part of the City of London Polytechnic). He is still there having been appointed Head of the Chemistry Department in 1963 and is increasingly involved with academic policy and administration. While ever grateful for the breadth of his early education in Northern Ireland he regards himself as a Londoner having been privileged to hear the sound of Bow Bells at an early age over 2LO. He joined the Society in 1945 taking a particular interest in the Microchemical Methods Group of which he was Honorary Secretary for 8 years and Chairman in 1963-64. He was elected to Council in 1961 and in 1963 was appointed an Honorary Assist- ant Secretary of the Society with particular responsibility for the Society’s Groups. As a newly elected Vice-president he continues to act as Chairman of the Group Liaison and Policy Committee and he is a member of Council’s Sub-committee on Amalgamation with other Societies. His hobbies include circumventing administrators keeping students and colleagues happy and meeting convivial people; for the last of these he is much indebted to the SAC.

ISSN:0037-9697    

DOI:10.1039/SA970070101b

出版商:RSC    

年代:1970

数据来源: RSC

摘要:

104 NEW MEMBERS OF COUNCIL [Proc. SOC. Analyt. Chem. Recent Advances in Pharmaceutical Analysis with Special Reference to Microchemical Techniques The following are summaries of some of the papers presented at a Joint Meeting of the North of England North East and Scottish Sections with the Microchemical Methods Group held on November 7th and Sth 1969 and reported in the December 1969 issue of Proceedings The Determination of Parts Per Million of Mercury in Eye Drops by Atomic Absorption BY W. H. HARPER CERTAIN pharmaceutical preparations such as eye drops and injection solutions contain phenyl mercury nitrate as a bacteriostat in the region of 10 to 20 p.p.m. The recognised chemical methods for low level mercury determinations were complicated and lengthy as evidenced by the report of the Analytical Methods Committee in 1965.l We therefore used the atomic-absorption method with which we hoped to obtain an accuracy of & 10 per cent.and the advantage of a simplified procedure. (p. 203). (Boots Pure Drug Co. Ltd. Nottingham) July 19701 RECENT ADVAXCES I N PHARMACEUTICAL ANALYSIS 105 Many authors have described the use of mercury vapour equipment for the determination of sub-microgram levels of mercury. This type of equipment was devised by Woodson2 and used by Van Suchtelen et aL3 for air-contamination measurements. Later Pappas and Rosenberg* assayed wheat grain and Wenninger5 analysed paint pigments for mercury with the mercury vapour equipment. The equipment used by them included a train of absorbents for prior removal of interfering substances. Poluektov et aL6 reduced the mercury with tin@) chloride to increase the sensitivity by vapour absorption while Hatch and Ott7 used tin(I1) sulphate for the same purpose in the assay of metals and rocks.Other workers have used the atomic-fluorescence method for low level mercury determinations Winefordner8 and Staab examined the instrumental limits for aqueous solutions of mercury and Vickers and Merrickg determined mercury in urine by using a solvent-extraction procedure to obtain the necessary concentration. By comparison with these methods commercial atomic-absorption equipment with an ordinary long path flame was found to be much less sensitive; it was therefore necessary to pre-concentrate the mercury by solvent extraction. Isobutyl methyl ketone was used to extract the mercury chelated with ammonium pyrrolidine dithiocarbamate.Malissa and SclioffmanlO listed thirty metals that can be treated in this way. INSTRUMENTATION- One was a home-assembled unit consisting of an SP 600 monochromator our own designs of atomiser spray chamber burner D.C. amplifier and mercury source. The second was a standard SP 90 Unicam atomic-absorption instrument. The conditions used with the SP 90 were as follows slit width 0.1 mm; wave- length 253.6 nm ; burner height 10 nim ; acetylene flow 5 cm minute-” air flow 1 litre minute-l; atomiser sample consumption 10 ml minute-I. Two instruments were used for this work. 15m L4 Hg lamp 125W ency about 16 MHz 6.3V a t 0.45A L = 40T tapped a t 10T on Q inch 0.d. Perspex tube L = 20 T on & inch 0.d. Perspex tube L = 60 T on I& inch 0.d.Perspex tube [L fitted inside L4] L = 14 foot pile wound over 1 inch on 5 inch 0.d. Perspex tu Ediswan M B/D be Fig. 1. Radiofrequency supply unit for the atomic-absorption mercury lamp. All coils 26 s.w.g. enamel copper wire close wound 106 RECENT ADVANCES IN PHARMACEUTICAL ANALYSIS [Proc. Soc. AnaZyt. Chem. The actual values used for acetylene and air will depend upon the precise atoiniser dimen- sions which in turn determine the sample consumption. The standard atoinisers supplied with the SP 90 instrument vary considerably in performance particularly in sample uptake. The procedure for both instruments was to adjust the acetylene to the lowest possible flow that would support a laminar flame when solvent solutions are sprayed. A rich luminous flame due to excessive solvent or acetylene constituents will give rise to a high noise level.The mercury source used with the “hybrid” equipment consisted of a modified Siemens mercury lamp coupled to an radiofrequency circuit devised by D. F. C. Crawley of Boots’ Instrumental Research Division (see Fig. 1). This lamp system was superior to the mercurv hollow cathode lamp in performance with the advantage of a very fine intensity control produced by the tuning condenser in the radiofrequency circuitry. METHOD- The method used for the B.P.C. formulations of eye drops which contain only sodium sulphacetamide sodium metabisulphate and phenyl nitrate was straight forward. The mercury in 100 ml of eye drops was chelated with 5 ml of 1 per cent. ammonium pyrrolidine dithiocarbamate and extracted into isobutyl methyl ketone (3 extractions with 5 ml) and the volume adjusted to 20 ml then read against standards prepared in the same way.The more complex proprietary formulations contained ingredients such as cellulose glycerin cetrimide and zinc sulphate which combined to inhibit the phase separation and cause emulsification. Tests carried out with all the ingredients individually seemed to indicate that the solvent volume change due to mutual solubility losses of both phases during the extraction procedure did not vary. Each of these ingredient solutions containing 20 p.p.m. of phenyl mercury nitrate was extracted and absorbances within 5 per cent. of the mean were obtained for all solutions although maximum extraction required 2 hours’ shake-out for the cellulose solution because of its high viscosity.The final method involved extraction with 10 ml followed by 5 ml of isobutyl methyl ketone and dilution to 20 ml in a graduated flask with 2 hours and 1 hour shake-out times respectively. A fixed acid concentration was used for all solutions and results were read against a synthetic standard extracted with the sample under test. The synthetic solution contained 20 p.p.m. of phenyl mercury nitrate with cellulose glycerin and other ingredients that affected the phase separations. RESULTS TABLE I RESULTS ON SAMPLES OF EYE DROPS Phenyl mercury nitrate p.p.m. B.P.C. 10 per cent. sodium sulphacetamide Batch 1 18.0 2 19.0 3 20.6 4 20.0 2 20.0 2 13.0 Batch 1 21.0 2 20.0 B.P.C. 30 per cent. sodium sulphacetamide Batch 1 19.0 Boots Proprietary Formulations (a)* Batch 1 19.0 (4 * * Types (a) and (b) refer to two different methyl cellulose derivatives.With one exception the results obtained with batch samples of eye drops when using the methods above were within the required limits of & 10 per cent. The precision of the method when a statistical test was applied was calculated to give a standard deviation of 5.95 per cent. which for a single determination with a probability of 0.95 was equal to fiducial limits of error of & 13-7 per cent. The work on this paper was carried out with the kind permission of Boots Pure Drug Co. Ltd. I thank Miss M. Langford for her valuable assistance and Mr. D. I;. C. Crawley for his contribution with the electronics. July 19701 RECENT ADVANCES I N PHARMACEUTICAL ,4NALYSIS 107 1. 2. 3. 4. 5. 6. 7. 8. 9. 10. REFERENCES Analytical Methods Committee Analyst 1965 90 515.Woodson T. T. Rev. Sci. Instrum. 1939 10 308. Van Suchtelen H. Warmoltz N. and Wiggerink G. L. Philips Tech. Rev. 1949 11 91. Pappas G. and Rosenberg L. J . Ass. 08. Agric. Chem. 1966 49 782. Wenninger J. and Jones J. H. Ibid. 1963 46 1018. Poluektov N. S. and Zebyukova Z. 2. Annlit. Khim. 1964 19 873. Hatch W. R. and Ott W. L. Analyt. Chem. 1968 40 2085. Winefordner J. D. and Staab R. A. Ibid. 1964 36 165. Vickers T. U. and Merrick S. P. Talaizta 1068 15 873. Malissa H. and Schoffman E. Microchim. A d a 1955 187. The Analysis of Degraded Pilocarpine Solutions BY J. B. MURRAY (Department of Pharmacy Heriot- Watt Universily Edinburgh) PILOCARPIXE was first isolated independently by Gerrardl and by Hardy2 in 18’75 from Pilo- cu@us Jaborandi.In 1897 Petit and Polonovski3 showed the presence of a second alkaloid \vhich was isomeric with pilocarpine and J o ~ e t t ~ confirming the results of the French workers named it isopilocarpine. Pilocarpine lsopilocarpine Today the main source is P. Microl’>hyZZus. Pilocarpine is a peripheral stimulant of the para-sympathetic system. PHARMACOLOGY I t has a miotic action causing contraction of the pupil of the eye and its chief use is for the reduction of the intra-ocular pressure in glaucoma and in detachment of the retina. For this purpose aqueous solutions 1 to 4 per cent. are normally used as eye drops the pilocarpine hydrochloride salt being used in preference to the nitrate as it is more compatible with preservatives. Isopilocarpine is reported to have similar pharmacological properties but is much less active.- CH3\ P i I ocarp ine Pilocarpic acid The molecule consists of an imidazole ring linked to a y-butyrolactone ring by a niethylene bridge. Pilocarpine is reported to isomerise to isopilocarpine on strong heating5 and also in strongly alkaline solutions; however in the middle of the pH range an equilibrium is reported to occur between pilocarpine and pilocarpic acid the pilocarpic acid being formed with the opening of the lactone ring. DETERMINATION OF PILOCARPINE- A large number of methods has been described for the determination of pilocarpine many of which involved the titration of the base use of Volhard’s method to determine the hydrochloride opening of the lactone ring with an excess of hot alkali followed by back- titration or gravimetrically by precipitation of the iodobismuthate etc.but none of these methods for specific to pilocarpine as isopilocarpine and probably other degradation products are also determined. 108 RECEXT ADVAXCES IS PHARMACEUTICAL ANALYSIS [PVOC. SOC. A~znlyt. Chem. In the B.P.C. assay for pilocarpine eye drops an acetate buffer is added to give a pH of 3.7 and to this is added sodium tetraphenylboron. The solution is allowed to stand for 10 minutes and is then back-titrated with cetylpyridinium chloride ; this assay gives the amount of nitrogenous base present and therefore is not specific for pilocarpine. Recently Ander~on~?~ made use of a colorimetric assay in conjunction with polarimetric measurements attempting to differentiate between pilocarpine and isopilocarpine by their specific rotation.However as the method he used involves the use of strong oxidising agents such as hydrogen peroxide and potassium dichroniate it is reasonable to assume that the method would not differentiate between pilocarpine and its primary decomposition products. A colorimetric assay based on an intact lactone ring has been published by Brochmann- Hanssen Schmid and Benmaman in 1965 based on reaction of lactones with hydroxyl- ammonium chloride in the presence of alkali to form hydroxamic acids which produce purple complexes with iron(II1) ion and it is this assay together with polarimetry that we are develop- ing for determination of pilocarpine. Pilocarpine Pilocarpic acid NHzOH 1 3\[-J CH 2 r g z 1 OH ‘NHOH ii NH:OH i -8- R-C-NH I 1 I 0 0 R For the assay add to a solution of the pilocarpine salt (containing about 40 mg per 100 ml 2.e.about 1.5 mg in 4 ml) 1 ml of 1 M hydroxylammonium chloride and 1 ml of 3.5 M sodium hydroxide allow it to stand for 10 minutes then add 2 ml of 3.5 M hydrochloric acid and 1 ml of 0.3 M iron(II1) chloride adjust to exactly 10 ml and after a further 10 minutes measure the absorption against a blank treated as above at 500 nm. Brochmann-Hanssen et aL8 found that above pH 11.4 maximum absorbance was achieved just before 10 minutes and they concluded that the reaction with hydroxylamine is faster than the base-catalysed hydrolyses of the lactone ring. The colour instability of the iron(m) - hydroxamic acid complexes is sometimes a dis- advantage but Brochmann-Hanssen et aL8 found that the percentage fading rate per 10 minutes was 1 per cent.The amount of lactone ring present and also any isopilocarpine are measured quantitatively by this assay and the best way to distinguish between pilocarpine and isopilocarpine in a mixed solution is by polarimetry as follows. The second part of the assay involves making a sample alkaline with ammonia solution extracting it with chloroform (thus eliminating pilocarpic acid which is insoluble in the chloroform) making the solution up to 25 ml with chloroform and measuring the specific rota- tion. A P.E. 141 polarimeter is used. This specific rotation can then be used to determine the porcentage of pilocarpine present in the mixture from a graph. .July 19701 RECENT ADVANCES IK PHARMACEUTIC.\L ANALYSIS 109 This assay has recently been carried out by Raesclilin Etter et al.in a thesisg on degrada- tion of pilocarpine but not in the published worklo in wliicli tlie Brochmann-Hanssen assa>- for the kinetics of degradation of pilocarpine was used. The pH of an unbuffered solution of pilocarpine hydrochloride is about 4 and all the evidence wggests that it is reasonably stable but with a pKa of 6.85 there is only less than 1 per cent. of the free base present. The pH of lachrymal fluid is 7.4 and the eye has a pain tolerance down to about 6.0 and normally the lachrymal fluid can buffer most solutions more or less instantaneously. However with pilocarpine this instantaneous buffering does not occur thus resulting in pain which in turn stimulates fresh tears and it requires several secretions to buffer even 1 per cent. solution.As it is used mainly for treatment of glaucoma where the eJ-cs tend to be dry and it is used over prolonged periods it would seem that buffered eye-drop preparations would be welcomed. Evidence from the l i t e r a t ~ r e l l ~ ~ * ~ l ~ J ~ on the stability of pilocarpine solutions at pH 6.5 to (P(i is conflicting and ranges from a half-life of 34 minutes at a pH of 6.6 at autoclaving temperature to a solution of pH 6-52 after being heated at 100" C for 30 minutes losing only 10 per cent. after storage for 5 weeks (25" C). From the above conflicting evidence we decided firstly to investigate tlie assay methods used and then to make kinetic studies on pilocarpine solutions and from these we hope to foriiiulate a suitably buffered eye-drop solution. As the principal use of pilocarpine is for eye drops the formulation is important.1. 2. 3 . 1. 5. 6. 8. 9. 10. 11. 12. 13. 14. I . KEFEREXCES Gerrard A. W. Phavm. J . 1875 5 865 and 965; 1876 6 237. Hardy E. Bull. Soc. CIELWL. Fv. 1875 24 407. Petit A. and Polonovski M. Ibid. 1897 17 553 554 and 703. Jowctt H. A. D. J. Cliem. SOC. 1900 77 473. Hill 13. I<. and Barcza S. Tetvahedron 1966 22 2889. Alnderson R. A. Can. J. Pharin. Sci. 1967 2 25. .\nderson K. A. and Fitzgerald S. D. ,4ust. J. Piiarin 1967 48 S 57. Brochmann-Hanssen E. Schmid P. and Benmaman J. D. J. Phavne. Scz. 1965 54 781. Baeschlin I<. Thesis of the University of Lausanne May 1968. Baeschlin I<. and Etter J-C. Phavvn. Acta Helv. 1969 44 301 339 and 348. Iiiegalinan S. and Vaughan D. G. j u n . J . A u n ~ v . Phavm. A s s . Pvacf. Plaavm.Edn 1938 119 474 Fagerstrorn K. J . Pharwz. Plzavmac. 1963 15 479. Ulok C. J. Ophthalinologtca Bade 1944 108 217. 'I'rose D. Phavmnzze 1962 17 81. 537 and 665. Some Experience and Problems in Human Metabolic Research BY A. ROBERTSOX ( Winthrop Labovatovies Newcastle azpon Tyne) SOME of the problems that can occur in a metabolic laboratory during the human investiga- tional period of a new drug were indicated. The importance of the early liunian data in relation to submission to official registration authorities was stressed as well as the necessity for close co-operation with the animal metabolic and pliarinacology laboratory. Although direct extrapolation of the absorption metabolism and excretion results from animals to man is not normally applicable the analytical methodology is generally directly transposable.The samples most commonly handled are blood urine and faeces but under certain circum- stances other biological fluids or tissues are examined; blood to give information on drug absorption and half-life within the body; urine to show which metaboiites have been formed and the various detoxication processes that have taken place; and faeces to indicate how much of the unchanged drug has passed through the body. Within this laboratory the main analytical facilities for instrumentation are recording spectrophotometry gas - liquid chroma- tography spectrophotofluorimetry and thin-layer chromatography. 110 RECEST ADVAKCES IS PHARMACEUTICAL ASALYSIS [PVOC. SOC. ,4~zaZyt. CZzenz. The degree of absorp- tion metabolism and excretion can vary with the health and tone of the body; diet before and after medication; the mobility of the subject during the medication period; individual enzyme activity ; individual drug transport rates through biological membranes and the pH of urines and so on.With the selective inbreeding of animals one can produce a relatively standard test species but this unfortunately is not the case with nian. The drug can be presented to the body in several ways orally as a tablet capsule suspen- sion or liquid; topically as a cream or ointment; rectally as a suppository; and intravenously or intramuscularly as a suspension or liquid. With tablets for example there are many factors within the formulation that can significantly affect the absorption of the drug such as drug surface area pharmaceutical excipients the method of compression the degree of disin- tegration of the tablet and dissolution of the drug from the tablet into the biological fluids.I t is therefore essential that during metabolic trials an attempt be made to standardise the presentation of the drug to man and to proceed with the investigation on a sufficient number of subjects to make the results statistically significant and at the same time initiate investiga- tions on the effect of the various formulations. \fTe have had a research interest for many years in a specific new strong non-addictive analgesic now marketed and wished to measure both blood and urine levels of the compound and its metabolites. As this is a relatively low dose drug we looked for the most sensitive procedure and selected gas - liquid chromatography to give an expected sensitivity of 0.01 mg ml-1 of blood.Although a basic procedure was available an extensive period of analytical time was involved in obtaining a technique that was both accurate and reproducible. I t was essential to obtain a suitable internal standard for reference purposes the final niaterial of choice having to be imported under licence being D.D.A. restricted; to establish and confirm that the pH of extraction was critical to within 0.1 of a pH unit; to establish that the small levels of drug extracted were being adsorbed or baked on to glass; and finally to confirm that it was necessary to work with triple-distilled extraction solvents. small evaporating tube with a capillary extension at the base was found to be essential to the efficiency of the operation acting as a small reflux condenser during solvent evaporation and preventing the extracted material from adhering to the side of the tube before chromatographic injection.Another marketed compound a bactericidal agent used in the treatment of urinary tract infection came under metabolic investigation during administration to patients suffering from renal impairment. As the detoxication mechanism was not functioning correctly blood levels tended to increase ; however by rapidly monitoring the blood and urine levels during hospital treatment the administered dose of drug was altered to maintain a therapeutic level in the urine and also to prevent high levels of the drug from developing in the blood stream. This involved close co-operation between the hospital and the metabolic laboratory.\Ye are currently investigating a new anti-inflammatory cornpound that has been developed in recent years. The metabolic pathway was first thoroughly established by urine and blood analyses and during the progress of this research work we recorded that one of the metabolites produced by esterase hydrolysis of the administered compound gave prolonged and therapeutically significant blood levels on ceasing medication when compared with the administration of this metabolite per se. By carrying out a series of experiments in human subjects we were able to establish that the normal medication for this tj’pe of therapy could most probably be reduced from four times daily to twice daily because of prolongation and maintenance of blood levels. Further results being accumulated suggest that the compound is stored in fatty tissue and released by exercise and subject mobility.Buccal absorption studies of this non-ionic compound confirmed that its absorption was not dependent on pH. By exercising subjects after ceasing multiple medication with the compound peak levels of metabolites were measured in the urine after each exercise period for several days after the cessation of therapy. Further work on body storage tissue and fluid distribution and long term therapy is in progress. In conclusion one may suggest that if the synthetic organic chemist and the pharmaco- logist produce more and more active compounds requiring snialler and smaller doses then we may reach a point where our current instrumentation is not sufficiently sensitive to deal with the level of metabolites that one could experience.Radiochemical techniques can obviously increase the level of analytical sensitivity but the basic problems of administration of radioactive tracers to nian will in most cases rule out this procedure. It is just possible The human body is unfortunately a non-standard test medium. July 19703 RECENT ADVANCES IK PHARJIACEUTICAL ASALYSIS 111 that a future therapeutically active new compound could not be used in patients because its absorption metabolism and excretion could not be analytically measured. I t would be an ideal situation if an animal could be found that handled drugs in an identical fashion but this possibility is extremely remote and it appears that we shall have to continue metabolic studies in humans non-standard test mediums though they be.The Application of Gas Chromatography to Official ;1/Ionographs BY J. C. DE.~VIN* (The Phavmacezdical Society of Great Britain 17 Bloornsbwy Square London W.C.1) THE object of Pharmacopoeia1 monographs should be to use the simplest test available; however many of the established methods do not afford the sensitivity or differentiation desired and techniques such as gas chromatography have had to be used. To achieve a degree of universal consistency it is necessary to stipulate in an appendix certain general criteria to which the proposed method should conform and in addition each monograph in which a gas - liquid chromatographic assay is specified should list the conditions under which the particular assay has successfully been carried out as a guide to help individual laboratories.The skill in setting out both these lists of data lies in closely specifying the essentials that must be common to all instruments without imposing requirements that are not universally acceptable. Amongst the variables are included detector columns carrier-gas flow-rate solid support stationary phase temperature and operator. Detector-A certain degree of flexibility should be allowed because ready exchange of detectors is not possible with many types of chromatograph. The flame-ionisation detector sliould be considered as the standard detector for official work. Columns-The length design (coil or U-tube) and material of the column can affect the efficiency of a given separation ; particulars should be specified. Carrier-gas jow-rate-Differently designed detectors require different flow-rates for optimum performance thus making it difficult to specify flow-rates.Solid support-It is possible to specify types mesh and pre-treatment of solid supports that have been successfully used. Stationary phase-It is usual to specify a particular stationary phase in view of its influence on partition coefficients of the constituents of a mixture. Tewzperature-As temperature has an effect upon the partition coefficient of each sub- stituent column temperature is specified for each assay except that when the stationary phase has been changed this temperature may no longer be optimum. \Vith gas and thin- layer chromatography the successful application of the technique depends as much on operator skill as it does on science. Operator-This may be considered the most important factor of all.Gas-chromatographic determinations should conform to certain criteria. (i) Resolution and coZuwn efJiency--The R.P. requires that tlie chromatogram obtained must demonstrate adequate resolution (i.e. greater than 1.0) between measured peaks. The cliromatogram must also demonstrate a minimal column efficiency in that the value of the relationship 16 tR2,/L'\'2 must be not less than 600 (tR is the distance along the base line between the point of injection and a perpendicular dropped from the maximum of the peak produced from the internal standard specification in the monograph; L is the length of the column in metres; and y is the peak width of the peak produced by the internal standard). (ii) Quantitative evaluation of the chromatogram-The U.S.N.F.in its appendix states that the areas are determined by means of an automatic integrator a planimeter or by triangulation. For systems in which equivalent accuracy can be obtained peak heights may be substituted for the band areas. Peak height measurements should only be used however when the symmetry factor is between 0.95 and 1.05. (Using expression yx/2A where y is the width o f the peak at one twentieth of the peak height; A is tlie distance between the perpendicular dropped from the peak maximum and the leading edge of the peak at one twentieth of the peak height.) * present address Lilly lndustries Ltd. Broadway House The Broadway Wimbledon London S.IV. 19. 112 RECENT ADVAXCES I N PHARMACEUTICAL ANALYSIS [Proc. SOC. Analyt. Clzem. Once linearity of response has been established with a calibration graph the assay can be performed routinely by usins an internal standard plus a standard mixture containing the constituent to be assayed and the internal standard only.(iii) Loss on coluwzn-Some loss of sample (about 1 per cent.) by irreversible absorption seems inevitable with the column packing at present available. (iv) Standard deviation-It should be possible to achieve relative standard deviations of better than 3 per cent. (v) Internal standard-The internal standard peak should be free and clearly distinguish- able from peaks due to the component to be measured and its possible decomposition products other components in the sample preparation and solvents. The appendix given in the U.S.P. XVII defines the technique only in very loose terms.The only application is the determination of the ratio of alkyl components in benzalkoniuni chloride based on a procedure by Warrington. The U.S.P. directs that a gas - liquid chromatographic apparatus equipped with a linear programming device be used but the operating conditions are not defined. The method of determining results is based on measurement of peak areas in both test and standard chroxna- t ograin s . The U.S.N.F. XII official at the same time as U.S.P. XVII gave a vague general des- cription and a procedure for determination of alcohol; no indication was given of the possible use of alternative conditions. The first supplement to the N.V. XI1 adopted a more per- missive approach with descriptions under “suitable” conditions although no criteria were offered to define “suitable.” The British Veterinary Codex 1965 also contains an appendix on gas - liquid chroinato- graphy.A description of the fundamentals is absent but a number of lists of materials to be used as solid supports and stationary phases and definitions of retention time and peak area are given. Details are also given of two methods of applying gas - liquid chromatography as a limit test for impurities one of these methods is suitable when a reference sample of each impurity to be determined is available and the other when a single reference substance that is not of the expected impurities is used. The R.P. is permissive in allowing alternative conditions of chromatography to be substituted in a monograph but lays down criteria such as adequate resolution minimal column efficiency and symmetry of peaks.Gas - liquid chromatography is applied in a number of monographs of the B.P.; one of the more difficult situations is that in which unknown impurities are assessed as in the case of halothane. Suitable column conditions are described (with provision for alternative condi- tions) provided resolution and minimal column efficiency can be demonstrated and three solutions used internal standard halothane (to ensure that there is no impurity peak corres- ponding in retention time to the internal standard) and internal standard in halothane. Problems exist in which it is impossible to elute impurities before the main peak and the impurity may be lost in the tail of the high loading of main component making pharma- copoeial standardisation exceedingly difficult. The possibility exists of trapping and re- cliroinatographing the tail section with suitable systems.In the determination of isopropyl alcohol in warfarin sodium (containing either up to 2 per cent. of water determined by Karl Fischer titration or about 5 to 6 per cent. of occluded isopropyl alcohol depending on the production process) three solutions are again prepared. Conditions for chromatography such as length and diameter of column packing material and stationary phase column temperature carrier gas and detector are specified although gas flow-rate is not defined. The British Pharmaceutical Codex refers to the B.P. appendix for general conditions and criteria and the applications of gas - liquid chromatography are confined to the Part VI Formulary Section. In the case of y-benzene hexachloride application the presence of other isomers is limited by7 the requirement that a single peak should be obtained.The other examples in the R.P.C. may be found in the liniment and ointment sections where chloroform camphor and methyl salicylate are determined with methylene chloride or benzyl alcohol as internal standards. The B.P. is the only other compendium with an appendix. ,4 less difficult situation is the measurement of occluded solvent. July 19701 RECENT ADVANCES IN PHAII~IACE~TICAL .\XALI'SIS 113 L4s part of the revision of the B.P.C. tliree particular projects have been investigated. Tliese include the examination of cetyl and cetostearyl alcohol for content of cetyl and stearyl alcoliols in establishing a standard for cetyl alcohol the determination of ephedrine in pre- parations and the determination of certain vitamins in vitamins I3 and C injection B.P.C.Cetyl alcohol-Alcohols were converted into their acetates by reflusing with acetyl chloride and were injected directly on to the column packing in the form of a 50 per cent. solution in acetone with a 1-pl syringe. The area of each peak was integrated and each peak expressed as a percentage of all peaks present up to CIS. Determination of ephedrine-This is now the subject of a joint S.A.C./P.S.G.R. panel but preliminary work has shown that by using columns packed with Carbowax and impregnated i v i t h 5 per cent. potassium hvdroxide on Chromosorb G it is possible to obtain symmetrical peaks of ephedrine. Detemination of vitanzim in vitamins B and C iajertimz-In view of the existing lengthy procedw es for thiamine nicotinamide and pyridoxine a method based on vapour-phase chromatography seemed to be practical. I t is possible to determine nicotinamide and thiamine directly with a column at 210" C packed with X.E.60 on Chromosorb G (results to within & 2 per cent.). Despite many problems in controlling the technique of gas - liquid chromatography to tlie requirements of a legally enforceable standard gas chromatography will play an ever increasing rBle in pharmacopoeia1 standards particularly in limiting impurities but possibly as a primary assay technique.

ISSN:0037-9697    

DOI:10.1039/SA9700700104

出版商:RSC    

年代:1970

数据来源: RSC

摘要:

RECENT ADVANCES IN PHAII~IACE~TICAL .\XALI’SIS 113 Presentation of Particle-size Distributions The following is a summary of one of the papers presented a t an Ordinary Meeting of the Particle Size Analysis Group held on November 25th 1969 and reported in the February 1970 issue of Pmceedings (p. 26). Graphical Yresentatioii of Sizing Aiialyses BY H. HEYWOOD (Chemistry Depavtinent U%iversi!y of Techizologv Lozrgliboroztgh) THE particles in a normal pulverised material extend over a size range of a t least 100 to 1 corresponding to a mass range of one million to 1 ; it is therefore essential to distinguish between the properties of size and mass. The purpose of graphical representation is to show these characteristics in a visual form so that comparisons can easily be made between different powders.The simplest form of graph relates the cumulative percentage by weight undersize with the corresponding particle size; and the preferred method of presentation is to plot size horizontally with zero at the left-hand corner of the graph and cumulative undersize vertically with the zero a t the same corner of the graph. The cumulative undersize scale should be arithmetic but the size scale may be arithmetic or logarithmic. Because of the wide range in particle size the logarithmic scale is generally more appropriate. The speaker discussed the relationship between cumulative and frequency curves for both arithmetic and logarithmic scales of particle size. Methods of presentation that produced graphs approximating to straight lines were introduced in about 1930. The advantage claimed for these is that simple parameters can be used to define the slope and position of the graphs thus facilitating the characterisation and comparison of powders.In the speaker’s opinion however very few sizing analyses follow a straight line for more than a limited size range and it can be shown mathematically that none will be represented by a straight line over the whole size range. Nevertheless these functional scales based on either the probability law or on the Rosin - Rammler law of size distribution are widely used and have certain advantages provided that the experimental points are not forced into a straight line. sequence of slides was shown to illustrate the form of the graphs representing particle systems with a normal Gaussian size distribution ; a log-normal distribution; and a distribution following the Rosin - Rammler law. In all cases the cumulative undersize by weight was plotted against the particle size for arithmetic logarithmic and functional scales.

ISSN:0037-9697    

DOI:10.1039/SA9700700113

出版商:RSC    

年代:1970

数据来源: RSC

摘要:

114 REPORT OF THE ANALYTICAL METHODS COMMITTEE [Proc. SOC. Analyt. Chew. Report of the Analytical Methods Committee 1969 THIS fourteenth Report of the Analytical lllethods Committee of the Society for Analytical Chemistry reviews the progress of work during 1969. Chairman D. C. Garratt Ph.D. D.Sc. Hon.M.P.S. M.Chem.A.. F.R.I.C. (Scientific Adviser Pharmaceutical Society of Great Britain) E. Bishop B.Sc. A.R.C.S.T. F.R.I.C. K. R. Capper B.Pharm. Ph.D. D.I.C. F.P.S. L. E. Coles B.Pharm. Ph.D. F.P.S. M.Ph.A. J. H. Hamencc O.B.E. M.Sc. Ph.D. M.Chem.=l. N. I&'. Hanson BSc. Ph.D. F.R.I.C. F. R. I .C. M.Chem.A. F.K.I.C. F.R.I.C. A. G. Hill F.R.I.C. C. A. Johnson B.Sc. B.Pharm. F.P.S. M.Ph.A. D. T. Lewis C.B. Ph.D. D.Sc. F.R.I.C. G. W. C. Milner DSc. F.R.I.C. A.1nst.P. F.R.I.C. R. F. Milton B.Sc.Ph.D. M.I.Biol. F.R.I.C. W. H. C. Shaw F.P.S. M.Chem.A. F.R.I.C. S. G. E. Stevens B.Sc. M.Chem.A. F.R.I.C. T. S. West Ph.D. D.Sc. F.R.I.C. C. Whalley BSc. F.R.I.C. I<. A. Williams B.Sc. Ph.D. A.Inst.P. M. Inst .Pet . M.Chem. A. F. R. I.C. W. J. Williams B.Sc. Ph.D. A.R.I.C. P. C. Young M.A. D.Phil. M.I.Chem.E. A. F. R. Ae. S. Unicersity of Exeter (Reader in A nalyi ical Director Department of Pharmaceutical Sciences Pharmaceutical Society of Great Britain Public Analyst 0 ficial Agricultural A nalyst Glamorgan County Council PubEic Analyst UBcial Agricultural A nalyst and Consulting Chemist Formerly Industrial Chemist ResearcJa and De- velopment Department Imperial Chemical Industries Ltd. Ckemisiry) Siandards Controller B.D.H. Chemicals Lid. Scienfi$c Director Britzsh Pharmacopoeia Corn- Government Chemist iwiuzistry of Technology G ~ o u p Leader A .E.R.E.Harwell (Honorary Treasurer of the Soczety) Analytical and Consulting Chemist Research Analyst Glaxo Laboratories Ltd. Ccmulting Chemist Professor of A nalytical Chemistry Imperial College (President of the Society) iwanager Staff and Administration Research Department Laporte Industries Ltd. General Chemicals Division naassion (Honorary Secretury of the Society) Analytical and Consulting Chemist Lecturer Bath University of Technology Group Manager BYitidk Standards Tnstitution Secretary P. W. Shallis GENERAL REVIEW It was with considerable regret that the Committee learned of the deaths in December of two men who had done much to further the aims of the Analytical Methods Committee over many years.When the Analytical Methods Trust Fund was set up in 1956 the Officers of the Society invited Mr. Justice Lloyd- Jacob to become Chairman of the Trustees and this he kindly consented to do. His enthusiastic approach to the building up of the Fund and its administration was much admired and his wise counsel in financial and other matters will be sadly missed. The death of Dr. G. W. Ferguson has ended a long association with the Committee and in particular with the work of the Essential Oils Sub-committee. It was in November 1949 that Dr. Ferguson was appointed a member of the Sub-committee and he had remained one ever since taking over the Chairmanship in 1956. During his period as Chairman many July 19701 REPORT OF THE ANALYTICAL METHODS COMMITTEE 115 changes were introduced in the work of the Sub-committee the most recent of which being an investigation of the use of more modern techniques and in particular gas - liquid chromato- graphy to the analysis of essential oils.A considerable amount of work on the application of gas - liquid chromatography to the analysis of essential oils has been carried out reports on much of which were at the time of Dr. Ferguson’s death being prepared for publication. The Committee would like to record its appreciation of the 20 years’ work done by Dr. Ferguson with the Essential Oils Sub-committee; his enthusiasm will be hard to replace. PROGRESS OF WORK- The most tangible measure of progress in the Committee’s work comes with the publication of a report from a Sub-committee although of course other less demonstrable progress is constantly being made.Most Sub-committees have from time to time to carry out investi- gations that are subsidiary to the main project and do not in themselves lead directly to the publication of a report. The speed with which these and in fact any investigations can be carried out is determined by the amount of time that the members all of whom give their services voluntarily are able to spend working on the projects being undertaken by the Sub-Committees. The considerable amount of work carried out by the Sub-committees in a year is a clear indication of the enthusiasm of the members and the Analytical Methods Committee extends its grateful thanks to all persons who assist in any way in ensuring that progress is maintained in the programmes of work of the Sub-Committees.The Fluorine Sub-committee has had an encouraging year after several earlier setbacks. This Sub-committee has divided its work into two separate groups one dealing with micro- gram amounts of fluorine in the final solution and the other with milligram amounts. Both groups have further divided their work into two phases the first of which is to recommend methods for the determination of fluorine in solution and the second to investigate methods for separating the fluorine from its matrix before determination. The Micrograin Group began its work by investigating a zirconium - Solochrome cyanine R method but despite several modifications it was eventually concluded that the repeatability of this method was not sufficiently good for it to be recommended. An investigation was then carried out of the lanthanum - alizarin fluorine blue method applied both in acetate and succinate buffered solution.This work has led to the conclusion that the method applied in succinate buffered solution is a good colorimetric method for the determination of fluoride. A survey of inter- ferences has been carried out and a Report on all the work done is being prepared for publica- tion. The Milligram Group began with a thorough investigation of several published modi- fications of the gravimetric lead chlorofluoride method but all efforts to reduce the large variations in results between analysts were unsuccessful. Attention was then turned to the thorium nitrate titration method under the conditions described by Selig (Analyst 1968 93 118) which makes use of methylthymol blue as indicator for the titration.Comparisons of this procedure with others that have been recommended have shown that it is superior in terms of reproducibility of the end-point and that it is a good method for determining from 2 to 15 mg of fluoride. A study of interferences with the titration is now to be under- taken and it is expected that a Report on the work that the Group has carried out will soon be prepared. ILlr. T. R. F. vc’. Fennell who had been Chairman of the Fluorine Sub-Committee since it was formed in 1965 has had to give up the Chairmanship owing to increasing pressures of other commitments. The Committee was very sorry to learn of Mr. Fennell’s decision and would like to record its sincere appreciation of the enthusiastic and able manner in which he has guided the Sub-committee through its first few years.Mr. Fennell’s association with the Sub-Committee will not however come to an end as he is to remain a member with an interest in the work of both Groups. The ,4nalytical Methods Committee has appointed Dr. E. J. Newman as the new Chairman of the Sub-committee. Four Reports from Sub-Committees were published in The ,4nnZyst during the year three of them from the Prophylactics in Animal Feeds Sub-committee. This Sub-Committee’s remit is to recommend standardised methods for the determination of drugs permitted under the Veterinary Products Registration Scheme for prophylactic use on poultry. The methods recommended by the Sub-Committee are subsequently incorporated as official in the Fertilisers and Feeding Stuffs Regulations. Many difficulties beset the work of this Sub-committee not the least of which is the almost constant introduction of new drugs necessitated by drug 116 [Yroc.SOC. Alznlq’t. Chenz. resistance building up within the animals. Another problem for which there is no immediate solution arises from the frequent changes in feed formulations introduced by the feeding- stuffs manufacturers. Such is the number of different types of feedingstuffs on the market that once an apparently satisfactory method of analysis has been found drug recoveries can be tested on only a limited range of feeds. Even so the very real possibility still exists that changing fashions in medication can cause a drug to be no longer in use by the time a method is recommended. In an attempt to minimise as far as possible the effects of these difficulties the membership of the Sub-committee has been increased in recent years and also includes direct representation from the Compound Animal Feeding Stuffs Manufacturers Xational ,4ssociation Ltd.This has enabled preliminary work on methods of analysis to be carried out more quickly by small groups of members before a full scale collaborative investi- gation by the entire Sub-committee is undertaken and the collaboration of representatives from the feedingstuffs industry ensures ready acceptance of the recommended methods by all interested parties. Recommended methods for two prophylactic drugs were published during the year dinitolmide (Zoalene) and dimetridazole. Both these drugs had occupied the Sub-committee’s attention for several years although dimetridazole had caused more problems.The method now recommended for the determination of dimetridazole is a polarographic one by which good recoveries were obtained by all members in a collaborative investigation. At the end of the year however it was brought t o the Sub-committee’s notice that although this method is satisfactory for the determination of the drug in most types of feedingstuffs on the market there is a strong possibility that it is not applicable in all instances owing to the presence of some ingredient in the feeds that renders the method of extraction of the drug ineffective. The third Report published by the Sub-Committee dealt with a procedure for determining amprolium sulphaquinoxaline and ethopabate when present together in a feeding stuff and makes use of the individual methods for these drugs already recommended.The only other Sub-committee to issue a Report during the year was the Metallic Impurities in Organic Matter Sub-committee. This deals with the determination of small amounts of cadmium in organic matter; during the last 10 years the Sub-committee has now issued Reports on the determination of arsenic copper mercury lead tin zinc and cad- mium together with recommendations on the destruction of organic matter the use of 50 per cent. hydrogen peroxide for the destruction of organic matter and the use of perchloric acid. Currently the Sub-committee is considering methods for the determination of selenium and is also assessing the suitability of modern instrumental techniques for the determination of some of the metals previously dealt with.The activities of the Analytical Standards Sub-committee continue to expand. As well as the work being done by the Sub-committee in completing its programme on acid - base standards before beginning an investigation of redox standards the Cornpleximetric Panel set up just over a year ago has now embarked on a programme of work. The Panel has however suffered an early setback in that pure samples of the indicators xylenol orange and rnethylthymol blue do not seem to be available. Attempts to purify these indicators or to prepare them in a high state of purity have so far been unsuccessful. Further work on this problem is in hand. Early in the year the Sub-committee jointly with the Microchemical Methods Group of the Society set up a Panel to review the specifications for “Reference Substances for Use in Organic Micro-analysis” and “Reagents for Use in Micro-analysis” last published in 1962.This Joint Panel under the Chairmanship of Dr. G. Ingram has made rapid progress and it is possible that the work will be completed during the coming year. All other Sub-committees have continued to make steady progress. The Particle Size Analysis Sub-committee whose main acti\Tity a t present is the compilation of critical reviews of the most widely used instruments and methods of particle sizing has under consideration at present a review prepared by two of its members on the electrical sensing zone method of particle-size measurement (Coulter Principle). I t is expected that this review will be published as Part TI of the Sub-Committee’s series on “The Determination of Particle Size” during the coming year.The Meat Products Sub-committee has devoted its attention during the year largely to the recommendation of methods for the basic analysis e.g. ash moisture and nitrogen of meat products. The determination of specific proteins in both cooked and REPORT OF THE ASALYTICAL METHODS COWHITTEE Further information is awaited on this. July 19701 REPORT OF THE ANALYTICAL METHODS COMMITTEE 117 uncooked products is still of considerable interest and the Sub-committee is in close contact with work that is being carried out. The Fish Products Sub-committee has an equally keen interest in the work on the determination of proteins and is being kept informed of progress. This Sub-committee completed its work during the year on the collection of figures for the nitrogen content of coalfish; a Report for publication is to be prepared.The considerable amount of work done over the last few years by the Essential Oils Sub-committee on the application of gas - liquid chromatography to the determination of constituents of essential oils is being collated as a preliminary step to the preparation of Reports for public a t’ ion. KO new Sub-Committees were set up during the year although it is possible that some may result from the reports of the assessors appointed to advise the Committee on alterations or additions that should be considered for incorporation in the second edition of “Official Standardised and Recommended Methods of Analysis.” The preparation of the second edition is progressing satisfactorily the aim being to publish it in the autumn of 1972.Three new Panels of the Joint Committee with the Pharmaceutical Society have been set up during the year. The first of these is investigating the assay of sympathomin:etic drugs with particular reference to gas - liquid chromatographic methods. Another is to investigate methods for the chemical assay of male fern and the third has been set up to review the Joint Committee’s recommended chemical methods of assay for senna and cascara in relation to different methods of assay that have been proposed by an official body. All three Panels held their first meetings towards the end of the year and each has devised a programme and has begun collaborative work. A 4 Report on “The Assay of Phenothiazine” was published in the October issue of The Analyst. The Panel responsible for this Report investigated several published methods for the assay of phenothiazine and concluded that a gas - liquid chromatographic procedure was the best.After the Panel had prepared its Report for publication a different gas-chromato- graphic method was adopted by the A.O.A.C. In consequence the Panel decided to carry out a collaborative comparison of the two methods which showed that there were no significant differences between the results obtained by either method. The Panel however preferred its own method as the retention time of promethazine hydrochloride used as internal standard in the A.O.A.C. method was considered to be unduly long for use in a method for which it was normal practice to carry out the test in duplicate. The use of chloroform as solvent in the A.0.,4.C.method was also considered to be a disadvantage. The Panel had at one stage used chloroform as solvent but as some difficulty in dispersing liquid preparations of pheno- thiazine was experienced and as pyrolysis products from this solvent gave rise to carbonisation and some slight corrosion of the detector the use of acetone was subsequently adopted. Full details of all the work done by the Panel are included in its published Report. Individual progress reports for all the Sub-committees and Panels together with their constitutions will be found on pages 118 to 129. .%X.4LYTIC.4Id METHODS TRUST- The full extent of the response to the A4ppeal to industry for further funds launched by the Trustees in September 1968 became known during the year. The Trustees are fairly well satisfied with the result when it is considered that the Appeal was made at a time when the financial climate had caused many organisations to restrict their charitable giving.The total sum received from donations during the year was l3963 which was approximately ,52200 more than in 1968. Some 20 new Deeds of Covenant have been entered into which together with continuing uncovenanted donations will ensure an income from this source of over l2500 for the next 2 years. The total number of subscribers in the year was 51 com- pared with 20 in 1968. ANNUAL ACCOUNTS- The audited statement of accounts for the year ended October 31st 19G9 is shown in Appendix I and a list of subscribers to the Trust Fund during the year is gilren in Appendix 11. 118 REPORT OF THE ANALYTICAL METHODS COMMITTEE [Proc.SOC. A IzaZ-yt. Chem. REPORTS OF SUB-COMMITTEES OF THE ANALUTICAL METHODS COMMITTEE ANALYTICAL STANDARDS SUB-COMMITTEE CONSTITGTION- E. Bishop B.Sc. A.R.C.S.T. F.II.1.C. (Chairman) I<. Archer BSc. P. R. W. Baker M.Sc. A.R.I.C. A. G. Hill F.R.I.C. E. J. McLauchlan M.Sc. I’h.D. A.R.I.C. R. G. Monk B.Sc. Ph.D. A.R.C.S. D.I.C. J. M. Skinner B.Sc. Ph.D. F.R.I.C. A.R.I.C. W. I. Stephen B.Sc. Ph.D. F.R.I.C. J. T. Yardley BSc. F.R.I.C. P. W. Shallis (Secretary) University of Exeter (Depnvtmeizt of Chewisfry) Lapovte Titanium Lid. Wellcome Research Laboratories B.D.H. Chemicals Ltd. National Physical Laboratory U.K.A.E.A . Atowaic Weapons Research Estab- Imperial Chemical Industries Ltd. (Agricultural University of Birmingham (Departnaent of Hopkin & Williams Ltd.lishment Division) Chemistry) TERMS OF REFERENCE-“TO examine existing analytical standards and to select suitable substances. ” PROGRESS OF WORK- The primary concern of the Sub-committee during the year has been to complete its work on acid - base standards. Three acids salts were under investigation sodium hydrogen diglycollate potassium hydrogen phthalate and potassium bi-iodate but by the beginning of the year the decision had already been taken that the quality of the potentiometric titration curves for the first two of these was too poor to allow accurate assays to be carried out. On the other hand the potentiometric titration curve for potassium bi-iodate was particularly satisfactory but doubts existed about the stoicheiometry of this compound. The presence of chloride in the material was suspected to be the cause of its lack of stoicheiometry but further work showed that this was not so.In consequence in the absence of any knowledge of the reason for its deviation from stoicheiometry the Sub-committee has concluded that potassium bi-iodate cannot be recommended for use as a standard in acid - base titrimetry. Full details of the work done on these acid salts will later be included in a Report from the Sub-committee. Other substances that have come under consideration are tris(hydroxymethy1)amino- ethane 4-aminopyridine hydrazine sulphate sodium tetraborate oxalic acid dihydrate and calcium hydrogen malate. Collaborative investigations on four of these compounds are still in hand in the hope that it will be possible to classify them as secondary standards (grade E) or possibly as working standards (grade D).The other two sodium tetraborate and calcium hydrogen malate have however been dropped from consideration. The variable isotopic abundance of boron had long been known to affect the molecular weight of sodium tetraborate but more seriously the Sub-committee has become aware of doubts that exist about the consistency of the sodium-to-boron ratios in the commercially available material. In conse- quence it has reluctantly been decided that sodium tetraborate cannot be recommended as a standard. No work has been undertaken on calcium hydrogen malate as this substance is not available commercially in a sufficiently pure form to warrant further investigation. I t is expected that the work currently being undertaken will complete the Sub-committee’s investigation of acid - base standards and the next phase of work will be consideration of standards for use in redox titrimetry.The Compleximetric Standards Panel of the Sub-committee has now completed its first full year of work and details are given below. During the year a Panel was formed jointly with the Microchemical Methods Group of the Society to revise the specifications for “Reference Substances for Use in Organic Micro-analysis” and “Reagents for Use in Micro-analysis.” Details of the constitution and work of this Panel are also given below. July 19701 REPORT OF THE ANALYTICAL METHODS COMMITTEE 119 COMPLEXIMETRIC STANDARDS PANEL CONSTITUTION- E. Bishop B.Sc. A.R.C.S.T. F.R.I.C. (Chairman) H. Bennett B.Sc. A.R.I.C. A. G. Hill F.R.I.C. R. G.Monk B.Sc. Ph.D. A.K.C.S. D.I.C. E. J. Newman B.Sc. Ph.D. F.R.I.C. TV. I. Stephen B.Sc. Ph.D. F.R.I.C. IV. J . Williams B.Sc. Ph.D. A.R.I.C. C. Woodward B.Sc. Ph.D. D.I.C. F.R.I.C. P. W. Shallis (Secretary) University of Exeter (Department of Chemistvy) British Ceramic Research Association B.D.H. Chemicals Ltd. l7.K.A.E.A . Atomic Weapons Research Estab- Hopkin & Williams Ltd. University of Birmingham (Department of Bath University of Technology Imperial Chemical Industries Ltd. (Agriculfuval A. R. I. C. lishment Chemistry) Division) PROGRESS OF WORK- As a preliminary stage of its work the Panel members carried out literature surveys to ascertain what work had previously been done on standards for use in compleximetry. From this survey it was decided that the most promising approach would be to investigate the use of bismuth lead mercury zinc cadmium calcium and magnesium either as the pure metals or pure salts with xylenol orange or methylthymol blue as indicator.An attempt was first made to establish the stability constants of the metal - indicator complexes but so far this has not been achieved owing to the inability to obtain pure samples of the indicators. ,411 attempts to purify or to prepare these indicators in a pure form have proved unsuccessful and this approach has for the time being been abandoned. Dithizone is an indicator that can be obtained in a pure form and work is now to be undertaken to establish the optimum conditions for the titration of pure zinc and cadmium with EDTA with dithizone as indicator. JOINT PANEL WITH THE MICROCHEMICAL METHODS GROUP CONSTITUTION- G.Ingram M.Sc. Ph.D. A.R.I.C. (Chairman) S. Bance B.Sc. F.R.I.C. F. H. Oliver L.R. I.C. P. R. W. Baker XSc. A.R.I.C. E. Bishop B.Sc. A.R.C.S.T. F.R.I.C. D. J. Bucknell A.R.I.C. A. G. Hill F.R.I.C. P. \V. Shallis (Secretary) Portsmmth PoZytechnic M a y G. Baker Ltd. Parke Davis & Co. Ltd. Il’ellcome Research Laboratories Uniuersity of Exeter (Department of Chemistry) Hopkin G. Williams Ltd. B.D.H. Chemicals Ltd. Representing the Microchemical Methods Group- Representing the Analytical Standards Sub-Committee- Representing manufacturers of reagevlt chemicals- PROGRESS OF WORK- The Panel set up to review and revise the specifications for “Reference Substances for Use in Organic Micro-analysis” and “Reagents for Use in Nicro-analysis,” held its first meeting in February.These specifications prepared by a Committee of the then Microchemistry Group of the Society were published in The Analyst in 1962. Rapid progress has been made by the Panel in its review. Most of the reference sub- stances contained in the last list are to be retained with in some instances minor modifica- tions to the specification or methods of test. A few new additions are under consideration which in some instances will replace substances previously recommended. Improvements in the specifications for certain analytical-reagent grade materials have made it necessary to retain many of the previously recommended reagents in the list. Speci- fications for some additional reagents that are used in newer microchemical techniques are under consideration. There is a possibility that the work of this Panel will be completed by the end of the year.120 COSSTITUTIOS- REPORT OF THE ASALYTICAL METHODS COMMITTEE ;Piroc. SOC. Analyt. Chem. ESSENTIAL OILS SUB-COMMITTEE (The late) G. W. Ferguson B.Sc. Ph.D. F.R.I.C. J. A%. Bailey B,Sc. -4.R.I.C. I<. Field M.Sc. Ph.D. J. H. Greaves B.Sc. F.R.I.C. A. M. Humphrey \V. S. A. Illatthews A.R.I.C. J. Ridlington B.Sc. A.R.I.C. J. H. Seager M.Sc. F.R.I.C. B. D. Sully B.Sc. Ph.D. A.R.C.S. F.R.I.C. G. Watson BSc. F.R.I.C. P. W. Shallis (Secretary) (Chairman) A nalytical and Consulting Chenzist Rowntree & Co. Ltd. IUinistry of Technology Laboratory of the Proprietary Peiyumes Ltd. Bush Boake Allen Ltd. Ministvy of Overseas Development Tropica Pvoducts Institute I.F.F. (Great Bvitain) Ltd. Yardley G. Co.Ltd. Bush Boake -4 llen Ltd. Cocker Cheinical Co. Lid. Government Chemist TERMS OF REFERENCE-('TO examine new methods of analysis applicable to the study of essential oils and to develop techniques for the determination of their more important constituents. " PROGRESS OF WORK- It was with considerable regret that members learned of the death of Dr. Ferguson shortly after a meeting of the Sub-committee in December. He had been a member of the Sub-Committee for 20 years almost 14 of them as its Chairman. Duriag his association with the work of the Sub-committee Dr. Ferguson had seen many changes in the approach to the analysis of essential oils and it was under his Chairmanship that the current programme of work on the investigation of the application of gas - liquid chromatography to the analysis of essential oils was begun.His enthusiastic approach to the many problems encountered in this field of analysis will be sadly missed. Much work was done by the Sub-committee during the year towards completing the work on the three projects that it had in hand. A gas-chromatographic approach to the determination of cineole in oils in which it was a minor constituent had earlier proved very successful giving results considerably better than would be expected by the o-cresol method. This work has now been extended to oils in which cineole is a major constituent and again very good results have been achieved. A Report on this work is now to be prepared. Further work on the determination of cedrol in Cedarwood oil and of geraniol in Citronella oil by gas - liquid chromatography has also been undertaken.The results of this work have been collated and it has been decided that a further collaborative test on both problems under more rigidly defined conditions should complete the work. Reports for publication will then be prepared. A little work has also been done on the gas-chromatographic determination of the major constituents of clove oils and this will be followed up when the other work has been completed. FISH PRODUCTS SUB-COMMITTEE COWSTITUT ION- S. M. Herschdoerfer Ph.D. F.R.I.C. F.I.F.S.T. M. R.S. H. (Chairman) J. H. Bushill D.Sc. F.R.I.C. F.R.S.H.* C. B. Casson BSc. F.R.I.C. W. T. Little B.Sc. Ph.D. J . A. Lovern Ph.D. D.Sc. F.R.S.E. F.R.1.C.t T. McLachlan D.C.M. A.C.G.F.C. M.I.Biol. M.Chern.A. F.R.I.C. F.I.F.S.T. F.R.S.K. R. McLayS D. J. Ward F.R.I.C.F.I.F.S.T. R. E. Wcston B.Sc. M.Chern.A. F.R.I.C. M. L. Windsor Ph.D. A.R.I.C. P. W. Shallis (Secretary) * Resigned October 1969. 4 Resigned March 1969. Appointed March 1969. T . Wall 6% Sons (Ice Cream) Ltd. Formerly J . Lyons & Co. Ltd. J . Ilyons & Co. Lid. Unzlevev Reseavch Laboratory (Colworth) Minist2.y of Technology Torry Research Station Public Analyst iMinistry of Technology Torry Research Station Birds Eye Foods Ltd. ,Miitistry of Technology Laboratory of the Afinistry of Techiiology €€umber Laboratory Government Chemist July 19701 REPORT OF THE ANALYTICAL METHODS COMMITTEE 121 TERMS OF REFERENCE-‘‘(^) To establish the essential characteristics of fish and differences in those characteristics caused by decomposition or other changes. (6) To recommend methods for determining the amounts of fish present in food products.NoTE-The term ‘fish’ to include shellfish and crustaceans.” PROGRESS OF WORK- IVork was completed during the year on the collection of analytical results for the nitrogen content of coalfish. As had been done previously when a nitrogen factor for cod was under consideration results obtained on fish landed over a period of more than 12 months were collected so that any evidence of seasonal variation in nitrogen content could be seen. The obtaining of sufficient analytical results on coalfish on which to base a recommendation was not so easy as had been the case with cod as in 4 consecutive months in the period covered no fish were landed that were available to members of the Sub-committee and the number of fish landed in some months was sparse.However the collated results show no real evidence of seasonal variation and a Report for publication is to be prepared recom- mending an average nitrogen factor for coalfish of 2.90 per cent. With the completion of work on coalfish the Sub-committee has now dealt with only two of the many species of fish used for manufacturing purposes. As mentioned above greater difficulty in obtaining sufficient information was experienced for coalfish than for cod and the Sub-committee realises that when less common species are dealt with so this problem will increase. In consequence the Sub-Committee is currently collecting the available data relating to the nitrogen contents of all the important species of fish. TVhen this has been completed the possibility of publishing the information as a guide will be considered.The Sub-committee is no nearer to a solution to the problem of the determination of milk protein in fish products than it was a year ago. However in addition to the work that is being done by a member of the Meat Products Sub-Committee on the determination of proteins in cooked and uncooked products by a haemagglutination method the Sub- committee’s attention has more recently been drawn to the possibility of determining the milk powder content of a product by means of its orotic acid content. The orotic acid content of milk powder is claimed to be reasonably constant and some members are to explore this possibility further. FLUORINE SUB-COhf MiTTEE COXSTITUTION- 1.. 13. F. \V. Fennell B.X.* E. J. Newman BSc. Ph.D. F.II.1.C.t 13.Belcher Ph.D. D.Sc. F.R.I.C. F.1nst.F.S H. A. Foner BSc. A.R.I.C.+ J. I<. Foreman B.Sc, F.R.I.C. G. S. Goff H. Green L.R.I.C. R. J. Hall F.I.M.L.T. Ministry of l?gricuZt.ttre Fisheries aizd Food W. C. Hanson F.R.I.C. K. F. Milton B.Sc. Ph.D. M.I.Biol. F.R.I.C. B. T. Saundersong J. M. Skinner B.Sc. Ph.D. F.K.I.C. R. Waspe B.Sc.f C. A. Watson A.R.E.C. J. E. Whitley BSc. Ph.D.$ P. \V. Shallis (Secretary) LWiizisfry of Technology Royal A i r c ~ a j t Esfab- Hopkiiz & Williams Ltd. U+zivevsi@ of Birmiizgham (Professor of A nalyt- ical Chew istry) Geological Sztrvey of Israel h!linistry of Technology Laboratory of the Governmeizt Chemist Lincoln Electric Co. L f d . 3ritisJb Cast Iron Research A ssociatiopz lishmed National Ap*iczrlfwal A dvisory Servict. Fisons Fertilisers Lid.Analytical and Consulting Biochemist Sir John Cass College Imperial Chemical Industries Ltd. (Agric&wal Formerly Laporte Acids Ltd. Nopkiiz & IVilliams Lid. Scottish ResrarcJL Reactor Centre Diz:ision) * Chairman to October 1969. t Chairman from October 1969. Corresponding member. 5 Appointed October 1969. 122 REPORT OF THE ANALYTICAL METHODS COMMITTEE [Proc. SOC. AnaZyt. Chem. TERMS OF REFERENCE-"TO investigate methods for determining fluorine and to recommend standardised methods for its determination at all levels in both organic and inorganic materials." PROGRESS OF WORK- ,4fter some earlier disappointments the Sub-Committee is now able to report considerable success in its work. The activities of the Sub-Committee are divided into two working groups one dealing with the determination of microgram amounts of fluorine and the other with milligram amounts.Both groups have concentrated in the first instance on providing reliable standardised methods for determining fluoride in solution before investigations of methods of separation and procedures for determining fluorine in different types of materials are undertaken. The Microgram Group has now completed an investigation of the alizarin fluorine blue method in succinate buffered solution. The results by this method have been found to be more reproducible than when the usual acetate buffered solution is used. Statistical assess- ment of the results has indicated that it is a good method for the determination of from 2 to 40 pg of fluoride in solution. To complete this phase of the work a study of interferences from ions present in the final solution has been carried out.This together with details of the work carried out by the Group on both the alizarin fluorine blue method and earlier on a zirconium- Solochrome cyanine R procedure are to be included in a Report for publication. The Milligram Group has carried out an investigation of the thorium nitrate titration procedure under the conditions recommended by Selig (Analyst 1968 93 118). Comparison of this procedure in which methylthymol blue is used as indicator with the previously accepted procedure have shown it to be much superior in sharpness of the end-point and it has been found to be a good titrimetric method for the determination of up to 15 mg of fluoride in solution. An investigation of interferences in the final solution is now to be carried out and when this is done a Report for publication will be prepared which will also include details of the earlier work done by the Group on the lead chlorofluoride method.Both groups expect soon to begin investigations on methods for separating fluorine for determination. Another project planned is a collaborative comparison of fluoride ion-selective electrodes which will involve members of both groups of the Sub-Committee. MEAT PRODUCTS SUB-COMMITTEE CONSTITUTION- S. M. Herschdoerfer Ph.D. F.R.I.C. F.I.F.S.T. J. C. Casey* W. B. Chapman RSc. M.Chem.A. F.R.I.C. P. 0. Dennis B.Sc. F.R.I.C. H. C. Hornsey F.R.I.C. A. J. Kidney B.Sc. Ph.D. A.R.C.S. R. A. Lawrie Ph.D. D.Sc. F.R.I.C. F.I.F.S.T. T. McLachlan D.C.M. A.C.G.F.C. M.I.Biol. A. McM. Taylor B.Sc.Ph.D. F.R.I.C. G. \Valley B.Sc. F.1I.I.C. R. E. \Veston B.Sc. M.Cheni.A. F.R.I.C. E. F. Williams O.B.E. M.A. F.1I.I.C. I<. A. Williams B.Sc. Ph.D. A.Inst.P. M.Inst.Pet. M.Chem.A. F.R.I.C." P. W. Shallis (Secretary) * Appointed February 1969. T. Wall ci;- Scns (Ice Cream) Ltd. Meat Research Insfifule Greater London Couwcil Brooke Bogqd 0x0 L f d . J . Sainsbury L f d . T. Wall & Sons (Meat & Handy Foods) Ltd. University of Notlingham (Food Science Lnborn- tories) Public A nalyst C. Shippnwz L f d . Unilever L f d . Mil.zistry of Technology Labmatory of the J . Sainsbury Ltd. A nalyfical and Coil Pulting Ckenaist M. R.S.H . (Chairman) M.Chem.A. F.R.I.C. F.I.F.S.T. F.R.S.13. Government Chemist TERMS OF REFERENCE-('(a) 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." July 19701 REPORT OF THE ANALYTICAL METHODS COMMITTEE 123 PROGRESS OF WORK- The year under review has seen the Sub-committee’s attention devoted mainly to the consideration of methods that are to be recommended for the basic analysis of meat products. Standardised methods for determining moisture ash nitrogen and chloride have been dealt with and methods for nitrate nitrite creatine creatinine fat phosphate and starch have still to be considered. It is intended that these methods shall be available for inclusion in the second edition of “Official Standardised and Recommended Methods of Analysis,” and will constitute a section relevant to the analysis of all meat products rather than just meat extracts as contained in the first edition.The definition for legal purposes of lean meat as meat trimmed free from visible fat has been under consideration by the Sub-committee. It is recognised that in any meat product an analyst can determine only the “chemical” lean meat content and the “chemical” fat content and that what appeared to be required was a factor that could be used to convert “chemical” lean meat into butchery lean meat. As much data as possible has been collected relating to the fat content of meat trimmed free from visible fat and it is obvious from the collated figures that the range of fat contents is so large that no scientifically acceptable factor could be proposed. The Sub-Committee is therefore considering publishing the figures it has collected with the statement that no recommendation can be made.No real progress can yet be reported with regard to the work being carried out in one laboratory on the determination of specific proteins in both cooked and uncooked meat products by a haemagglutination method although work is still in progress. Details of an alternative electrophoretic approach have recently been published and this also will be investigated in the hope that it can provide an easier method for use in most laboratories. METALLIC IMPURITIES IN ORGANIC MATTER SUB-COXMITTEE CONSTITUTION- L. E. Coles B.Pharm. Ph.D. F.P.S. M.Ph.A. W. Cassidy B.Sc.Tech. M.Chem.A. F.R.I.C. J. C. Gagc B.Sc. Ph.D. F.R.I.C. M.Chcm.A. F.R.I.C. (Chairman) R. A. Hoodless B.Sc. Ph.D.Miss E. 31. Johnson M.Sc. A.R.I.C. D. A. Lambie B.Sc. F.R.I.C. Ii. 117. Liebmann Dr.Phil. F.R.I.C. R. F. Milton B.Sc. Ph.D. M.I.Biol. F.R.I.C. E. J. Newman B.Sc. Ph.D. F.R.I.C. W. L. Sheppard M.Sc. F.R.I.C. G. B. Thackray B.Sc. M.Chem.A. F.R.I.C. C. A Watson A.R.I.C.* P. W. Shallis (Secretary) * Appointed October 1969. Public A nalyst and 0-jicial Agricultural Analyst Deputy Public Analyst Imperial Chemical Industries Ltd. (Industrial Ministyy of Technology Laboratovy of the British Food Manufacturing Industries Research The Radiochemical Centre Metal Box Co. Ltd. Analytical and Consuliing Biochemist Hopkin & Williams Ltd. Unilever Ltd. Public A nalyst Hopki$t G. TVillinnzs Lld. Hygiene Laboratories) Government Chemist A c ;ocia tion TERMS OF REFERENCE-“TO investigate the determination of small quantities of metals in organic matter.’’ PROGRESS OF WORK- A Report from the Sub-committee on “The Determination of Small Amounts of Cadmium in Organic Matter” was published in the December issue of The Analyst.In this Report a spectrophotometric dithizone procedure is recommended together with alternative polaro- graphic and atomic-absorption procedures all of which proved satisfactory in collaborative tests carried out by the Sub-committee. The possible recommendation of atornic-absorption procedures for other metals is also under consideration and a Report on the determination of copper by atomic-absorption spectroscopy is to be prepared. A collaborative comparison of the Sub-Committee’s recommended molybdenum blue method for determining arsenic (Analyst 1960,85,629) with the silver diethyldithiocarbamate 124 REPORT OF THE ANALYTICAL hfETHODS COMMITTEE [PTOC.SOC. A?znlJ)t. Che??C procedure (B.S. 4404 1968) was begun during the year. Certain difficulties associated with the grade of zinc to be used for hydrogen generation in the silver diethyldithiocarbamate method have been encountered and the solutions obtained after wet digestion of organic matter have not in all instances proved to be satisfactory for the determination of arsenic. This work is still continuing. The determination of small amounts of selenium in organic matter has again been under consideration. Attempts to apply published procedures involving the use of the reagents 2-mercaptobenzoic acid and 2-mercaptobenzothiazole were unsuccessful. Attention has now been turned to a more recent method published by R.J. Hall and P. L. Gupta (AnaZyst 1968 94 292). This method which makes use of the reagent 2,3-diaminonaphthalene is claimed to be capable of determining down to 0.005 p.p.m. of selenium on a 5-g sample. A collaborative investigation of this method is to be undertaken PARTICLE SIZE ANALYSIS SUB-COMMITTEE CONSTITUTION- E. Q. Laws B.Sc. F.R.I.C. (Chairman) T. Allen M.Sc. Ph.D. R. de B. Ashworth &l.Sc. Ph.D. F.R.I.C. D. G. Beech Ph.D. V. T. Crowl BSc. Ph.D. F.R.I.C. A.R.C.S. I. C. Edmundson B.Pharm. M.P.S. C. G. L. Furmidge B.Sc. Ph.D. F.R.I.C. M. J . Groves M.Pharm. Ph.D. M.P.S. M.I.Biol.* H. Heywood Ph.D. D.Sc. A.C.G.I. M.I.M.E. M.I.C.E. J. F. Hinsley F.I.M. F.1nst.P. R. Howes B.Sc.T K. Marshall B Sc. B. Scarlett MSc. Grad.1nst.P. J . P.Stuart B.Sc. Ph.D. C. R. G. Treasure BSc. Grac1.Tnst.P. P. W. Shallis (Secretary) D.I.C. * Appointed March 1969. Resigned June 1960. $ Appointed November 1960. Formerly Mi% is t ~ y of Tech .Izology L a bor n to r y Uiziziersity of Bradford Minislvy of Agriculture Fisheries and Food Piud Pathology Laboratory Britislz Ceramic Reseavcla Associatioiz Paint Research StntioiL of the Govermzent Chemist Glnxo Laboratm ies Ltd. L‘SheIl” Research L f d . Chelsea College o f Science and TechnoIcgji Loztghboroztgh Unicersity of TethncIcgy Edgar AIle2z 6% Co. L:d. Chesterford Park Reszarch Station University of Bradjord Lowgk borough University of Techn olcgy Miitistry of Techizology Warren Spring Laborafovy Loztghbovoztgh University of Techwology TERMS OF REFERENCE-(‘TO study methods of particle size analysis to survey available instruments and to evaluate them with regard to their principles of operation and fields of application.” PROGRESS OF WORK- Work has continued during the year on the compilation of further parts of the Sub- Committee’s series of critical reviews on methods of particle size analysis.Part I of this series a critical seview of sedimentation methods was published just over a year ago and the report has been in considerable demand. Part I1 will be a critical review of the principles instrumentation and application of the electrical-sensing zone method of particle size analysis. This will cover the Coulter counter and other similar instruments and is being prepared on behalf of the Sub-committee by two of its members. A complete draft of the review has been considered by the Sub-committee and the authors are now dealing with the points raised before submitting a revised draft for discussion.Critical reviews of other instruments and methods that are intended to be incorporated in Part I11 of the series are under con- sideration. The possibility of carrying out further collaborative tests of some of the more widely used methods of particle sizing was the subject of further discussion during the year. One of the major problems associated with the arrangement of these tests is the provision of a suitable standardised powder and as yet no satisfactory sample has been found; this matter is still being pursued. July 19701 REPONT OF THE ANALYTICAL METHODS COI\;IMITTEE 125 PROPHYLACTICS IN ANIMAL FEEDS SUB-COMMITTEE CONSTITUTION- S.G. E. Stevens B.Sc. M.Chem.A. F.R.I.C. R. J. Anderson BSc. A.R.I.C. M. D. Beach B.Sc. F.R.I.C." A. G. Croft B.Sc. A.R.I.C. C. E. Dodd A.R.1.C.t G. Drewery B.Sc. M.Chem.A. F.R.I.C. J. Hartley B.Sc.f§ R. S. Hatfull M.Chem.A. F.R.I.C. F.R.S.H. S. P. Hayes F.R.I.C.3 J. S. Leahy M.A. A.R.I.C. I. McLachlan J. Markland B.Sc. M.Chem.A. F.R.I.C. D. H. Mitchell B.Sc. R. C. Spalding M.A. M.Chem.A. F.R.I.C. J. A. Stubbles BSc. C. B. Stuffins F.R.I.C.11 R. E. Weston B.Sc. M.Chem.A. F.R.I.C. Ministry of Technology Laboratory of the D. R. Williams B.Sc. Ph.D. F.R.I.C.3 D. R. Wraige B.Sc. F.R.I.C.7 P. W. Shallis (Secretary) * Co-opted for work on organic arsenicals. f Appointed September 1969. $ Appointed June 1969. $ Representing the Compound lZnirnal Feeding Stuffs Manufacturers National Association Ltd.,/ Resigned September 1969. 7 Resigned June 1969. Consultiitg CheiniTt Cooper Technical Bureau Lennig Chemicals Ltd. Spillers Ltd. J . Bibby Agriculture Ltd. Merck Sharp & Dohme Ltd. R H M Agricultural Research and Advisory Ser- Public A nalyst Sikock & Lever Feeds Ltd. Huntingdon Research Centre Dow Chemical Co. (U.K.) L f d . Public A nalyst Burroughs Wellconze & Co. Public A nalyst M a y G. Baker Ltd. J . Bibby Agriculture Ltd. Government Chemist (Chairman) vices Ltd. Unilevev Ltd. R H M Agricu1fitral Research and Adcisory Ser- vices Ltd. TERMS OF REFERENCE-"TO investigate and recommend analytical methods for substances to be used against helminthic protozoal bacterial and fungal diseases including mixtures of those substances. ' ' PROGRESS OF WORK- Three Reports from the Sub-Committee were published in The A~zaEyst during the year.These Reports contained recommendations on the determination of dimetridazole and dini- tolmide (Zoalene) in animal feeds and also on the determination of amprolium sulpha- quinoxaline and ethopabate when present together in animal feeds. A polarographic method is recommended for the determination of dimetridazole and as indicated in the published Report good recoveries of the drug from the different types of feedingstuffs examined were obtained. Since publication however the Sub-Committee's attention has been drawn to the fact that one member had received for analysis a sample of feedingstuff containing dimetridazole on which no polarographic wave for the drug could be obtained. Enquiry has elicited the fact that the main difference between this feedingstuff and those previously examined by the Sub-committee was that it contained a bentonite-based hardening in- gredient.On the supposition that adsorption of the drug on the bentonite from which it could not then be extracted by the aqueous acid treatment recommended might be the cause of the difficulty preliminary extraction with organic solvents followed by recovery of the drug and subsequent determination by the Sub-Committee's method is to be investigated in the hope that this will solve the problem. The Sub-committee has decided not to recommend spectrophotofluorimetric methods for the group of hydroxyquinolate drugs under investigation. Work on the determination of these drugs decoquinate methyl benzoquate and statyl by gas - liquid chromatography is in hand in one of the collaborating laboratories and the results of this work are awaited.Work is still in hand on methods for determining carbarsone and clopidol (meticlorpindol) and it is expected that this work will be completed during the coming year. A method for the determination of nifursol (3,5-dinitrosalicylic acid 5-nitrofurfurylidene hydrazide) is to be investigated next. 126 COXSTITUTION- REPORT OF THE ANALYTICAL METHODS COMMITTEE [Proc. SOC. 3mZyt. Chern. PUBLICATIONS SUB-COMMITTEE D. C. Garratt Ph.D. D.Sc. Hon.M.P.S. M.Chem.A. F.R.I.C. (Chairman) J. B. Attrill M.A. F.R.I.C. J. H. Hamence RI.Sc. Ph.D. M.Chem.A. S. G. E. Stevens BSc. M.Chem.A. F.R.I.C. S. C. Jolly B.Sc. B.Pharm. M.P.S. F.R.I.C. Chairman A naly fical Methods Comiiaiftee Editor The Analyst Member A naly f ical iWethods Committee Member A nalytical Methods Committee ,4 ssistant Director Department of Pharmaceutical (Secretary and Editor) Sciewes Pliarmaceutical Society of Great F.R.I.C.Britain PROGRESS OF WORK- A second edition of “Official Standardised and Recommended Methods of Analysis” is planned for publication in the autumn of 1972. All the Society’s recornmended methods of analysis that are still valid and in use will be included’ together with an up-to-date version of the bibliography of official standardised and recommended methods. Reports from the assessors appointed by the Sub-committee to advise on the continuing suitability of the methods recommended by the A.M.C. indicated that many methods will not require modification. Consideration is currently being given to those methods that will require modification.Arrangements have now been made for the compilation of all the sections of the bibliography. REPORT OF THE P.S./S.A.C. JOINT COMMITTEE ON METHODS FOR THE EVALUATION OF DRUGS MAIN COMMITTEE I<. R. Capper Ph.D. B.Pharm. F.P.S. D.I.C. J. C. Deavin B.Pharm. M.P.S. J. W. Fairbairn B.Sc. Ph.D. F.P.S. F. Fish B.Pharm. Ph.D. F.P.S. D. C. Garratt Ph.D. D.Sc. Hon.M.P.S. A. L. Glenn B.Sc. B.Pharm. Ph.D. F.P.S. C. A. Johnson B.Sc. B.Pharm. F.P.S. F.R.I.C. W. Mitchell B.Sc. Ph.D. F.R.I.C. Hon.M.P.S. R. F. Phipers B.Sc. Ph.D. F.R.I.C. J. M. Kowson ?rl.Sc. Ph.D. F.P.S. F.L.S. R. Sinar B.Pharm. B.Sc. F.P.S. RI.Chem.h. I<. L. Smith F.P.S. W. H. Stephenson F.P.S. D.B.A. M.Ph.A. S. G. E. Stevens BSc. M.Chem.h. F.R.I.C.A. F. Scott B.Sc. A.R.I.C. P. W. Shallis (Secretary) F.K. I .C. (Chairman) M.Chem.A. F.II.1.C. M. Ph. A. F.R.I.C. F.K.I.C. Pharmaceutical Society of Great Britain Phavmaceutical Society of Great Rtitain Universit-y oj Londo’z (Professor of’ Phannacog- University of Stirathclyde Chairman A nalytical -Methods Committee of the University of London (School of Pharmacy) British Pharmacopoeia Commissioiz Bush Boake Allen Ltd. Cooper Technical Bureau University of Bradford (Pro fessor of Pharmacy) Analytical and Consulting Chemist Boots Pure Drug Co. Ltd. Boots Pure Drzig Co. Lid. Consulting C A& i ~ i i st Geigy (U.K.) L f d . nosy 1 S.A .C. TERMS OF REFERENCE-“TO prepare standard methods for the evaluation of drugs their preparations and of kindred materials.” PROGRESS OF WORK- One Report from a Panel of the Joint Committee was published during the year.This was the Report from Panel 8 which had previously been disbanded on the assay of pheno- thiazine. Several different proposed methods for the assay of phenothiazine were investigated by the Panel before a gas-liquid chromatographic method was established as being the best. After the Panel had completed its work and while its Report was being prepared details of a different gas -liquid chromatographic method that had been adopted by the A.O.A.C. were published. In consequence the Panel arranged a collaborative comparison of this method with its own method and it was found that there was no significant difference between the results by the two methods. Full details of all the work done by the Panel are included in its Report which was published in the October issue of The Analyst.July 19701 REPORT OF THE ANALYTICAL METHODS COMMITTEE 127 Collaborative tests involving measurements of mass volume and light absorption have been carried out by Panel 10 which is investigating the accuracy and precision of analytical techniques in the context of pharmaceutical analysis. Such has been the number of results returned in these tests that statistical evaluation of them has become a major project and is unfortunately not yet complete. Much interesting information is expected from this Panel and its findings are eagerly awaited. Panel 11 is investigating the assay of sympathomimetic amines. Gas - liquid chromatography appears to be a promising technique for this group of drugs and preliminary collaborative work has been started.The chemical assay of male fern is the concern of Panel 12 and as the first stage of its work a published thin-layer chromatographic method is being investigated. Panel 13 has been set up to re- consider the Joint Committee's recommended chemical methods for the assay of senna and cascara with regard to the different methods that have been proposed for inclusion in the European Pharmacopoeia. A collaborative comparison of the proposed European Pharma- copoeia method for cascara with the Joint Committee's method is being undertaken first. Some other possible subjects for new panel work are under consideration. Three new Panels were set up during the year. PANEL 10 ACCURACY AND PRECISION IN PHARMACEUTICAL ANALYSIS CONSTITUTION- A. L. Glcnn B.Sc.B.Pharni. Ph.D. F.F.S. (Chaivman) A. I;. .?idamson B.Sc. Ph.D. F.R.I.C. F. Bailey L.R.I.C. I<. Al. Ba.;tow B.Sc. F.R.I.C. P. F. G. Boon B.Sc. A.R.I.C. E. G. Brickell F.R.I.C. C. Campbell B.Sc. F.R.I.C. P. Cleevely B.Sc. F.R.I.C. C. Daglish B.Pharm. Ph.D. 3f .C.I.C. F.P.S. J . C. Deavin B.Pharm. M.P.S. D. H. Dorken B.Pharm. M.P.S. F.R.I.C. ilf. J . R. Healy E. F. Hersant B.Pharm. Ph.D. F.R.I.C. F.P.S. D. \V. Houghton B.Sc. J . P. Jefferies B.Sc. F.R.I.C. C. A. Johnson B.Sc. B.Pharm. F.P.S. F.R.I.C. IT. P. Jones F.P.S. F.R.I.C. R. E. King A.R.I.C. C. A. MacDonald B.Sc. F.R.I.C. A. J . Middleton B.Pharni. M.P.S. A.R.I.C. D. H. Mitchell BSc. A. R. Moss B.Sc. Ph.D. A. IT. C. Peacock B.Pharin. F.P.S. G. F. Phillips M.Sc. F.R.I.C. A. R. I. C. M.Ph.,4. C. Radford L. R. Rowe B.Sc. Ph.D.A.R.C.S. D.I.C. 35. L. Sheppard A.R.I.C. D. 0. Singleton B.Sc. F.R.I.C. F. R. Soer M.Sc. A.R.I.C. A. F. Stott B.Sc. A.R.I.C. A. E. Theobald Ph.D. F.R.I.C. C. H. Thorpe BSc. A. J. Woodgate B.Sc. A.R.I.C. J. Wragg B.Sc. F.R.I.C. P. JV. Shallis (Secretary) University of Londoz (School of Pharmacy) Il'inthrop Laboratories Iinperial Chemical Indaistvies Ltd. (Phavmaceuti- cal Division) Burroughs Wellcosne & Co. Ciba Laboratories Ltd. iWonsanto Chemicals Ltd. E. R. Squibb & Sons Ltd. Nicholas Products Ltd. Reckitt G. Sons Ltd. Phavinaceutical Society of Gveat Britain Smith ICline (I; French Labovatovies Ltd. AW.R.C. Clinical Research Centre iWay & Baker Ltd. G. D Seavle & Co. Ltd. Glaxo Laboratories Ltd. Bvitish Pharmacopoeia Coinwission Cyanamid of Great Britain Ltd. Abbott Labovatovies Ltd.Evans iWedica1 Reseavch Labolatovies Parke Davis & Co. Burvoughs Wellcome 6- Co. Roche Products Ltd. Ri k er L abo ratovies IZlinisti/y of Technology Labovatory of the Eli Lilly & Co. Ltd. Allert & Hanbuvys Ltd. Goveviiwient Chemist Rozissel Laboratories Ltd. Upjohn Ltd. Merck Sharp G. Dohme Ltd. Geigy ( U.R.) Ltd. (Phavmaceuticals Division) Chelsea College of Science and Technology (Phar- macy Department) B .D .H. Pharmaceuticals Ltd. Bush Boake Allen Ltd. Boots Pure Drug Co. Ltd. 128 [Proc. SOC. Analyt. Chem. TERMS OF REFERENCE-"(^) To evaluate the accuracy and precision obtainable from estab- lished methods of pharmaceutical analysis under normal conditions of quality control. (ii) To investigate ways of improving accuracy and precision in pharmaceutical analysis." REPORT OF THE ANALYTICAL METHODS COMMITTEE PROGRESS OF WORK- Two collaborative tests have been carried out by the Panel the first designed to provide information on the errors involved in weighing and transferring a solid sample and the second to provide information on the errors involved in the measurement of volume by means of flask pipette and burette. Such was the number of results returned in this test that computer processing has had to be undertaken. For various reasons this task has taken considerably longer to perform than was anticipated and as yet has not been completed. It is intended that when processing of the results is finished a report on the work will be prepared. The Panel will then meet to consider the report and to arrange a further programme of work.PANEL 11 C.L.C. APPLIED TO THE ASSAY OF SYMPATHOMIMETIC DRUGS CONSTITUTION- J. C. Deavin B.Pharm. M.P.S. (Chaivman) J. S. Foster B.Sc. A.R.I.C. M. Mitchard B.Pharm. Ph.D. A.R. I.C. D. H. Mitchell B.Sc. R. Sinar B.Pharm. B.Sc. F.P.S. M.Chem.A. R. N. Thornhill B.Sc. D. A. Wheeler M.Sc. -4.R.I.C. P. W. Shallis (Secretary) Pharmaceutical Society of Great Britaiii Boots Pure Dmg Co. Ltd. Chelsea College of Science and Technology Burrouglzs Wellcome & Co. Agaalytacal and Consulting CJLemist Snatth Kline G. Fvench Laboratovies Ltd. Smith 6 Nepplzew Research Ltd. F.R.I.C. TERMS OF REFERENCE-"TO investigate the assay of sympathomimetic amines with particular reference to gas - liquid chromatographic methods." PROGRESS OF WORK- The Panel held its first meeting towards the end of the year and decided that gas- liquid chromatography appeared to offer the best approach to providing a standardised method for determining these drugs.A preliminary programme of work on investigating a published procedure has been arranged and the first drug to be considered is to be ephedrine. PANEL 12 ASSAY OF MALE FERN CONSTITUTION- F. Fish (Chairman) R. Hardman B.Sc. B.Pharm. Ph.D. F.P.S. D. Ritchie Ph.D. M.P.S. A.R.I.C. E. J. Shellard B.Pharm. Ph.D. F.P.S. F.L.S. A. J. Woodgate B.Sc. A.R.I.C. P. VV. Shallis (Secretary) University of Strathclyde Bath University of Technology Macfarlan Smith Ltd. Chelsea College of Science and Teciaaology Bush Boake Allen Ltd. F.R.I.C. TERMS OF REFERENCE-"TO investigate the assay of male fern and male fern extracts with particular reference to chromatographic methods." PROGRESS OF WORK- The official assay method of the British Pharmacopoeia does not distinguish between the active and inactive phloroglucides present in male fern and its extracts.A more specific assay method is required and at its first meeting the Panel decided to investigate a two- dimensional thin-layer chromatographic method capable of separating the active flavaspidic acid from the numerous other constituents especially the inactive filicic acid which is a major component of the mixture. Preliminary work on this method is being undertaken. July 19701 REPORT OF THE ANALYTICAL METHODS COMMITTEE PANEL 13 ASSAY OF CASCARA AND SENNA COXSTITUTION- D. C. Garratt Ph.D. D.Sc. Hon.M.P.S. M.Chem.A. F.R.I.C. (Chairman) C. Daglish B.Pharm. Ph.D.M.C.I.C. F.P.S. ,4. R. I. C. Pharmaceutical Society of Great Brifain Reckitt 6 Sons Ltd. 129 J. C. Deavin B.Pharm. M.P.S. J. W. Fairbairn B.Sc. Ph.D. F.P.S. F.L.S. P. A. Linley B.Pharm. C. A. -l/acDonald BSc. F.R.I.C. M. H. Ransom Mrs. S. Richens F.P.S. A. J. Woodgate B.Sc. A.R.I.C. P. 5V. Shallis (Secretary) Pharmaceutical Society of Great Britain University of London (Professor of Pkcarmacog- University of Bradford Evans Medical Research Laboratopies William Ransom 6 Sons Ltd. British Pharmacopoeia Commission Bush Boake Allen Ltd. F.R.I.C. nosy) TERMS OF REFERENCE-~~TO review the Joint Committee’s recommended methods for the assay of cascara and senna with reference to the different methods proposed from other official sources.” PROGRESS OF WORK- Chemical methods of assay for cascara and senna have been recommended by the Joint Committee as a result of the work done by Panel 3 which has subsequently been disbanded.More recently methods have been proposed for inclusion in the European Pharmacopoeia that are different from those recommended by the Joint Committee; and in consequence it has been decided that collaborative comparisons of the methods should be carried out to ascertain whether or not the methods proposed for inclusion in the European Pharmacopoeia were at least as acceptable as the Joint Committee’s methods. The assay method for senna had already been accepted for inclusion in the European Pharmacopoeia but the method for cascara had not reached the acceptance stage and the Panel decided at its first meeting to investigate the cascara assays first.A collaborative investigation of the two methods is now in hand. 130 REPORT OF THE ANALYTICAL METHODS COMMITTEE [P?’OC. sot. AnaZyt. Chem. APPENDIX I YEAR ENDED OCTOBER ~IsT 1960 THE SOCIETY FOR ANALYTICAL CHEMISTRY ANA4LYTICAL METHODS TRUST ACCOUNTS FOR THE Income and Expenditure Account fur the Year ended Octcber 31st. 1969 Subscriptions and Donations from Industry . . Interest Received From Investments . . .. . . From Bank Deposits. . .. .. Books (Heffers) . . .. .. Book Department . . . . .. Sales Income Tax Refunds Covenanted subscriDtions 1967-68. . Investments 1967-68 . . .. DEDUCT Rent Light Salaries Maintenance Printing and Expenses of Meetings . . .. Postage . . * . .. .. Audit Fee . . . . .. .. Sundries . . . . .. .. Heat and Telephone . . of Office Equipment .. Stationerv . . .. .. .. . . .. Book Department Stock a t 31.10.68 . . .. Printing of A.M.C. Publications Book Department Salaries . . Book Department Postage . LESS Stock a t 31.10.69 . . . . .. .. .. .. .. . . .. .. .. . . .. .. .. .. * . .. .. .. .. . . . . . . .. .. .. .. .. .. .. . . I . .. .. * . .. .. * . .. * . .. . . . . .. .. .. .. .. . . .. .. .. * .. .. I . .. .. .. I I . .. .. . . * . .. ,. . . .. .. .. . . .. .. * . .. .. .. .. .. .. . . . . .. .. .. .. . . . . .. .. .. .. .. .. .. 1200 257 249 59 1765 - 1060 L 486 246 - 151 152 1071 3643 91 282 244 118 37 40 5526 705 3963 732 - 1308 303 6306 6231 196s 1768 356 479 234 3346 452 142 6777 ?4 - - 1056 3145 2 277 280 63 37 23 4 883 1840 242 260 90 2432 - I_- 1200 1232 -- 6115 Excess of Income over Expenditure for the year ended October 1969 transferred to Accumulated Fund .. .. .. .. 31st .. July 19701 REPORT OF THE ANALYTICAL METHODS COMMITTEE Balance Sheet at October 31st 1969 Current Assets Stocks of Books Unsold . . .. 0 . .. I . Sundry Debtor The Society for Analytical Chemistry . . .. Cash a t Banks Barclays Bank Ltd. On Current Account . . . I .. .. On Deposit Account . . . . .. . . Swindon Corporation . . . . .. .. . . DEDUCT CURRENT LIABILITY The Society for Analytical Chemistry . . 1 . .. NET CURRENT ASSETS . . .. .. .. .. Investments (at costj per Schedule (Market Valuc L17,819) Financed by Accumulated Fund Balance November lst 1968 . . .. .. .. Less Loss on sale of Investments during year . . .. 0 . .. .. . . . . .. .. .. .. . . .. * . 1 . .. . * . . . . . . .. Add Excess of Income over Expenditure for the year ended October 31st 1969 .. .. .. .. .. .. Signed on behalf of the Analytical Methods Trust Fund D L L 1060 165 4 5000 6220 148 131 1968 L 1200 75 35s 5073 - 6706 - 608 1 17,913 6706 17,921 @3,994 24,627 708 24,627 23,055 90 23,919 c- i a #3,994 23,965 662 24,627 W. KENT- JONES (Chairman) G. \V. C. MILNER (Honorary Treasurer) Auditors’ Report to the Trustees of the Society for Analytical Chemistry Analytical il-lethods Trust U7e have examined the above Balance Sheet which in our opinion gives a true and fair view of the state of affairs of the Trust Fund a t October 31st 1969 and it is in accordance with the Books kept by the Trustees. We have verified the Investments and cash balances and found them to be in order. 65 Southampton Row London W.C.1. December 31st 1969. (Signed) RIDLEY & CO. Chavtered Accouiztants Auditors. 132 REPORT OF THE ANALYTICAL METHODS COMMITTEE [Proc. SOC. Analyt. Chew Schedule of Investments held at October 31st 1969 Net income fo year to 31.10.69 67 Held 3 1.10.68 at cost 2550 Held 3 1.10.69 a t cost 2550 Market values 3 1.10.69 2573 Nominal amount 700 &I000 Burmah Oil Co. Ltd. A 1 Ordy Stock Units . Burmah Oil Co. Ltd. New 84% Loan (A700 paid- Balance due A175) . . . . . . 250 Debenhams Ltd. 10s. Ordy Shares . . .. 2300 Distillers Co. Ltd. 10s. Ordy Shares . . . . 1900 Courtaulds Ltd. 5s. Ordy Shares . . . . * . 600 300 500 83 Eagle Star Insurance Co. Ltd. 10s. Ordy Shares . . Eagle Star Insurance Co. Ltd. Bonus Issue 1 2- Philip Hill Investment Trust Ltd.'& Ordy Sharii Hill Samuel & Co.Ltd. 5s. Ordy Shares (Sold 20.6.69 . . 11.7.69 for L l O l 13s.) . . . . . . . . 375 I.C.I. Ltd. A 1 Ordy Stock Units . . . . . . for A363 4s. 5d.) . . .. .. Morris & David Jones Ltd. Ordy Shares . . for A1033 10s. 3d.) . . . . 11.7.69 for L516 7s. 9d.) . . . . A310 19s. 3d.) . . . . for A604 12s. 10d.) . . . . . . . . A2198 6s. 8d.) . . .. . . . . . . 125 I.C.I. Ltd. It;l Ordy Stock Units (Bought 11.7.69 1000 M. & G. Fund of Investments Trust Income Units 2200 660 Rank Hovis McDougall Ltd. Ordy Stock Units. . 464 Renold Ltd. A1 Ordy Stock Units (Sold 11.7.69 300 Royal Insurance Co. Ltd.'&. Stock Units (Soid 1200 Venesta Ltd. 5s. Ordy Shares (Sold 11.7.69 fir. 400 Wharf Holdings Ltd. Ord; 'Share's' (Sold 11.7.69' Sl5 Unilever 5s. Ordy Shares (Bought 11.7.69 for ..700 2466 747 2411 2547 875 2351 33 1 2501 2565 - 2466 747 2411 2547 - 74 9 80 51 - 60 7 - 607 - 650 - 12 101 736 2 28 - 736 - 998 363 575 101 2 1001 353 489 1128 866 - 575 1012 1001 - 6 44 35 855 30 735 11 872 9 706 28 2198 2139 &17,92 1 - L17,819 - A17,913 July 19701 REPORT OF THE ANALYTICAL METHODS CO3IMITTEE APPENDIX I1 SUBSCRIBERS TO THE TRUST FUND DURING 1969 133 Abbott Laboratories Ltd. Albright & Wilson Ltd. Aspro - Nicholas Ltd. Associated Portland Cement Manufacturers Beecham Group Ltd. Boots Pure Drug Co. Ltd. Bovril Ltd. The British Aluminium Co. Ltd. The British Arkady Co. Ltd. British Glues & Chemicals Ltd. British Petroleum Co. Ltd. British Titan Products Co. Ltd. Central Electricity Generating Board Courtaulds Ltd. The Distillers Co. Ltd.Geigy (U.K.) Ltd. The Glaxo Group A. Guiness Son Cyr Co. Ltd. H. J. Heinz Co. Ltd. Hopkin & Williams Ltd. Imperial Chemical Industries Ltd. Kellogg Company of Great Britain Ltd. Laporte Industries Ltd. J. Lyons 82 Co. Ltd. Marks & Spencer Ltd. Ltd. Merck Sharp & Dohme Ltd. The Metal Box Co. Ltd. J. Mackintosh & Son Ltd. Organon Laboratories Ltd. Brook Bond 0x0 Ltd. Parke Davis 82 Co. Pfizer Ltd. The Pharmaceutical Society of Great Britain Cavenham Foods Ltd. Procter & Gamble Ltd. Quaker Oats Ltd. Ranks Hovis McDougall Ltd. Reckitt 8t Colman Ltd. Riker Laboratories Ltd. Koche Products Ltd. J. Sainsbury Ltd. Sandoz Products Ltd. Smith Kline & French Laboratories Ltd. Smith & Nephew Ltd. Spillers Ltd. John 82 E. Sturge Ltd. Unilever Ltd. Wallace & Tiernan Ltd. The Wellcome Foundation Ltd. Weston Research Laboratories Ltd. J. Wyeth & Brother Ltd.

ISSN:0037-9697    

DOI:10.1039/SA9700700114

出版商:RSC    

年代:1970

数据来源: RSC

摘要:

134 OBITUARY [PYOC. SOC. Analyt. CJzem. Changes in the Register of Members KENr MEMBERS ORDIXARV ~~IENBERS Eric Addison B.Sc.(Lond.) ; Philip Andrew B.Sc. Ph.D.(Manc.) ; Keven Ashburn; john Maxwell Bather M.Sc.(Liverpool) F.R.I.C. ; Peter Joseph Birch; Sicolaas Andreas lgnatius Maria Boelrij k Ph.D. (Amsterdam) ; Adam Zygmunt Britten M.Sc. Ph.D. (Manc.) ; Peter Malcolm Brown B.Sc.(Lond.) ; Ian Edward Burrows X.Sc. Ph.D.(Lond.) ; Solian La1 Chawla M.Sc.(India) A.M.I.1.Chem.E. ; David Clayton R.Sc.(Leeds) ; Patricia Creed; Cyril Cresswell A.R.I.C. ; John Tribbeck Dax,ies R.Sc.(Lond.) A.R.I.C. ; Anthonv Fisher B.Sc.(Lond.) ; Michael Freeman M.Sc.(Lond.) ; MTil.liarn Peatman Hayes B.Sc.(Lond.) M.Sc. Ph.D.(Nottingham) M.Chem.X. F.K.I.C. ; Geoffrey Charles Havward M.A.(Oxon.) Ph.D. (Lond.) ; John Aitken Holgate M.B.C1i.B. MSc. (Leeds) ; Richard Anthony Hoodless B.Sc. Ph.D.(Soton) ; Vincent VC’illiam Howells B.Sc.(Cardiff) M.Cheni.A. A.R.I.C. ; John Xorgan Jenkins; Philip Owen Kane B.Sc. Ph.D. (Lond.) A.R.C.S. ; L-pananda Karunatilake B.Sc.(Ceylon) ; James Jackson Kay A.K.I.C. ; Eric John Kempster K.Sc.(I,ond.) ; Alfred George Kendall R.A.(Keele) A.R.I.C. ; Leo Levi B.Sc. Pfi.D.(Montreal) ; Michael John Manning; Keith Marshall B.Sc.(Lond.) M.P.S. D.B.A. ; Willvs Frederick Mason; Alan John Kewbery ; Keith Albert Newman R.Sc.(Lond.) M.Ph.A. A.R.I.C. ; George Russell Kugent ; Michael Edward Peover B.Sc. Ph.D. (Lond.) ; Roger Perry R.Sc. Ph.D. A.R.I.C. ; Mannuel July 19701 PUBLICATIONS RECEIVED 135 Pina; William John Poling A.R.I.C. ; Pamela Margaret Scriven B.Sc.(Lond.) L.R.I.C. ; Shantilal Khetshi Shah B.Sc. (Lond.) ; Arthur Francis Smith A.R.I.C. ; Albert Sommerauer Dipl.Ing.Chem. Dr.sc.techn. ; Frank Trowell F.R.I.C. ; Trevor David White B.Sc. (Lond.) ; Derek William Whymark M.Sc. (Strathclyde) L.R.I.C. JUNIOR MEMBERS Alan Geoffrey Davies ; Francis Martin Davies ; Kenneth James Haswell ; Henry Kegg ; Marianne Hudson Kirk B.Sc.(Lond.) ; Keith Simpson M.Sc.(Liverpool) ; Linda Vogt B.Sc. STUDENT MEMBERS E’ouad Al-Sulimany B.Sc.(Saudi Arabia) ; Ajit Vaman Dangi B.Sc.(Bombay) M.Sc.(Lond.) ; Geoffrey Malcolm Ranger L.R.I.C. ; David John Smith B.Sc.(Lond.).

ISSN:0037-9697    

DOI:10.1039/SA970070134b

出版商:RSC    

年代:1970

数据来源: RSC

摘要:

July 19701 PUBLICATIONS RECEIVED 135 Publications Received The publications listed below have been received by the Editor of The Analyst in which journal Book Reviews will continue to appear. ORBITALS AND SYMMETRY. By D. S. URCH. Pp. 256. Harmondsworth Baltimore and Victoria Penguin Books Ltd. 1970. Price 25s. INORGANIC ENERGETICS. By W. E. DASENT. Pp. 165. Harmondsworth Baltimore and Victoria Penguin Books Ltd. 1970. Price 20s. ORGANOMETALLIC COMPOUNDS METHODS OF SYNTHESIS PHYSICAL CONSTANTS AND CHEMICAL REACTIONS. Edited by MICHAEL DUB. Pp. viii + 343. Formula Index to the Second Edition of Volumes I to 111. Prepared by MICHAEL DUE and KICHARD W. WEISS. Berlin Heidelberg and New York Springer-Verlag. 1969. Price DM 72; $19.80. MICROANALYSIS BY THE RING-OVEN TECHNIQUE. Br DR. HERBET WEISZ. Second Edition. Pp. x + 170. Oxford New York Toronto Sydney and Braunschweig Pergamon Press. 1970. Price 60s.; $8.00. METHODS OF BIOCHEMICAL ANALYSIS. Edited by DAVID GLICK. Volume 18. Pp. viii + 421. New York London Sydney and Toronto Interscience Publishers a division of John Wiley & Sons. 1970. Price 160s. HE DESTRUCTION OF ORGANIC MATTER. By T. T. GORSUCH. Pp. viii + 151. Oxford New York Toronto Sydney and Braunschweig Pergamon Press. TEOKIA Y PRACTICA DE LA CROMATOGRAPHIA EN FASE GASEOSA. By LUIS GASCO SANCHEZ Pp. xxiv + 549. Madrid Ediciones J.E.N. 1970. Price 715 pesetas. Covering the Literature from 1937 to 1964. 1970. Price 55s. ; $7.50.

ISSN:0037-9697    

DOI:10.1039/SA970070135b

出版商:RSC    

年代:1970

数据来源: RSC

摘要:

136 NOTICES [Proc. SOC. Analyt. Chem. Notices Second Particle Size Analysis Conference 1970 THE following programme subject to minor alterations has been arranged for the Second Particle Size Analysis Conference to be held at the University of Bradford in September. SCIENTIFIC PROGRAMME Wednesday September 9th 9.30 a.m. 9.45 a.m. Introduction and Address of Welcome by L. S . Bark (University of Salford). Plenary Lecture by Professor H. Heywood (Loughborough University of Technology). “ The Origins and Developments of Particle Size Analysis.” APPLICATIONS OF PARTICLE SIZE ANALYSIS Chairman Mr. L. S. Bark. 11.15a.m.- 1. “High Temperature Oxidation of Stainless Steels A Study of the Distribution of 12.45 p.m. Spalled Oxide Particles,” by S. J. Barker and J. M. Francis (Research and Develop- ment Department Central Electricity Generating Board Berkeley Nuclear Laboratories Berkeley Glos.).“The Effect of Particle Size on the Consolidation of Powders During Compaction,” by J. A Hersey and J. E. liees (Pharmaceutical Research Sandoz Ltd. Basle CH 4008 Switzerland). “Centrifugal Elutriation of Particles in Liquid Suspension,” by F. J. Colon J . W. van Heuven and H. M. van der Laan (Central Technical Institute TNO Delft The Netherlands). 2. 3. 4. Withdrawn Chairman Mr. J. C. Williams. 5. 2.30 p.m.- 3.45 p.m. “Particle Size Analysis of Airborne Particles Smaller than 0.3 p i in Diameter,” by J. Heyder C. Roth and W. Stahlhofen (Gesellschaft f u r Slrahlenforschuzg m.b.h. Abtezlung fur Biophysikalische Strahlenforschung FrankfurtlMain). “An Assessment of the Langer Acoustical Counter,” by I.Sinclair P. J. Lloyd and B. Scarlett (Chemical Engineering Department Loughborough University of Technology Loughborough Leics.) . “An On-stream Particle Size Analyser for Mill Pulps,’’ by J . H. Talbot and D. J. Jacobs (Physical Sczences Laboratory Chamber of Mines of South Africa Johannesburg South Afvica) . 6. 7. Chairman Mr. B. Scarlett. 4.15 p.m.- 5.30 p.m. 8. 9. 10. “Emulsion Particle Size Measurement from Interference Colours,” by G. C. N. Cheesman “Measurement of Pigment Dispersion in Paints and Printing Inks,” by W. Carr (Pigments “Particle Size Analysis by Diffraction of Light,” by J . H. Talbot (Physical Sciences (Revertex Ltd. Harlow Essex). Divisioit Geigy ( U. K.) Ltd. Roundthorn Estate Wythenshawe Manchester) . Laboratory Chamber of Mines of South Africa Johannesburg South Africa).Thursday September 10th MICROSCOPY AND SEDIMENTATION METHODS Chairman Dr. M. J . Groves. 11. 10.45 a.m. 12. 9.30 a.m.- “A Statistical Description of Particulate Systems,” by B. Scarlett (Chemical Engineering Department Loughborough University of Technology Loughborough Leics.). “Small Particle Measurements on the TMC Particle Measurement Computer System,” by J. L. Dwyer D. A. Manalan and R. R. A. Morton (Millipore Corporation fnc. and Bausch and Lomb Inc. U.S.A.). “Autoniatic Sedimentation Size Analysis Instrument,” by W. P. Hendrix and C. Orr jun. (Micromeritics Instrument Corporation and Georgia Institute of Technology Atlanta Ga. U.S.A.). 13. THE SOCIETY FOR ANALYTICAL CHEMISTRY Chairman Professor H. Heywood. 11.45 a.m.- 12.45 p.m. 14. 25.“Performance of a New X-ray Sedimentometer,” by L. Svarovski and T. Allen (Post- graduate School of Powder Studies University of Bradford Bradford 7 Yorks.). “Determination of Particle Size Distributions of Mortar Materials,” by S. Berg and E. Koefoed (Institute for Silicate Industries The Technical University of Denmark 2800 Lyngby Denmark). “Determination of Specific Surface and Surface - Volume Shape Coefficient with the Wide-angle Photosedimentometer,” by T. Allen (Postgraduate School of Powder Studies University of Bradford Bradford 7 Yorks.). “Particle Size Distribution of Fine Powders with Wide Size Range and Containing Ultra-fine Particles,” by A. Muta and S. Watanabe (Central Research Laboratory Hitachi Ltd. Tokyo Japan). 16. 17. Chairman Dr. Tng. K. Leschonski. 2.30 p.m.- “Studies into the Settled Volumes of Precipitated Materials,” by D.Dollimore and 3.15 p.m. G. B. McBride (Department of Chemistry and Applied Chemistry University of Salford Salford 5 Lancs.). “The Effect of Cluster Instability in Suspensions on Particle Size Analysis Measurements with the Cahn Balance,” by R. Davies and B. H. Kaye (I.I.T. Research Institute 10 West 35th Street Chicago Illinois U.S.A .). 20. “Settling Rate of Individual Particles in Suspension,’’ by B. Koglin (Institut f u r Mechanische Verfahrenstechnik University of Karlsruhe W . Germany). 18. 19. Chairman Dr. J. A. Hersey. 21. 4.15 p.m.- “Theoretical and Experimental Investigations of Sedimentation Balances,” by K. 5.30 p.m. Leschonski and W. Alex (Institut f u r Mechanische Verfahrenstechnik University of Karlsruhe W.Germany). “Sedimentation of Stratified Suspensions Above the Stokes’ Range,” by J. Brezina (Institut f u r Mechanische Verfahrenstechnik University of Karlsruhe W . Germany). “Particle Size Analysis by Homogeneous Centrifugal Sedimentation,” by P. J. Lloyd B. Scarlett and I. Sinclair (Chemical Engineering Department Loughborough Univer- sity of Technology Loughborough Leics.). 22. 23. Friday September 1 lth COULTER PRINCIPLE AND SURFACE AREA MEASUREMENTS Chairman Mr. M. W. G. Burt. 10.45 a.m. 9.30 a.m.- 24. “The Effect of Particle Size Shape and Concentration on the Response of a Coulter Counter,” by P. J. Lloyd B. Scarlett and I. Sinclair (Chemical Engineering Depart- ment Loughborough University of Technology Loughborough Leics.). “Standard Calibration Materials for the Coulter Counter,” by J.G. Harfield and W. M. Wood (Coulter Electronics Ltd. High Street South Dunstable Beds.). “The Study of Surface Properties with the Flow Microcalorimeter,” by C. E. Templer (Microscal Ltd. 20 Mattock Lane Ealing London W.5). 25. 26. Chairman Dr. T. Allen. 11.15 a.m.- 12.45 p.m. 27. 28. “The Preparation of Powder Beds by a Centrifugal Compaction Technique,” by M. W. G. Burt and C. ,4. Fewtrell (A.W.R.E. Aldermaston Berks.). “A Reliability Study on the Surface Area Analysis of Polymeric Materials by a Dynamic BET Method,” by A. J. Behringer and R. C. Ackerman (Xerox Corporation Roches- ter N.J. U.S.A.). “A Performance Reliability Study on the Model C Coulter Counter in the Characterisa- tion of Polymeric Materials,” by D. F. Alliet and A. J. Behringer (Xerox Corporation Rochester N .J. U.S.A.). “The Correlation of Electron Microscope Data with Coulter Counter and Surface Area Results in the Characterisation of Polymeric Matcrials,” by A. J. Behringer D. F. Alliet and R. C. Ackerman (Xerox Corporation Rochester N . J. U.S.A.). 29. 30. THE SOCIETY FOR ANALYTICAL CHEMISTRY Chairman Professor D. C. Freshwater. 2.15 p.m.- 3.00 p.m. 31. 32. 33. “A New Instrument for the Automatic Presentation of Total Surface .%rea,” by R. Naley and R. W. Lines (Coulter Electronics Ltd. H i g h Street South Dunstable Beds.). “Surface Area Measurement by a Simple Diffusion Apparatus,” by N. G. Stanley-Wood (Postgraduate School of Powder Studies Univevsity of Bradford Bradford 7 Yovks.). “Anomalies in the Interpretation of Surface Areas for Porous and Aggregated Particles by the Permeability Method,” by D.Dollimore J. Dollimore and P. Spooner (Department of Pure and Applied Physics University of Salford Salford 6 L a n a . ) . Chairman Mr. L. S. Bark. 3.30 p.m.-.- 4.30 p.m. 4.30 p.m. Closure of Conference. Plenary Lecture by Dr. Ing. K. Leschonski (Kavlsruke W . Gerwany). “Present and Future State of Particle Size Analysis.” THIRD ROMANIAN NATIONAL CONFERENCE ON ANALYTICAL CHEMISTRY THE Chemistry Department of Romanian Kational Council of Engineers and Technicians will sponsor the Third National Conference on Analytical Chemistry from September 22nd to 26th 1971 in Brasov-Romania. The following sessions are planned electrometric methods ; optical methods ; and separation methods. Further information on this meeting is available from the secretary Dr. Constantin Luca Consiliul Xational a1 Inginerilor si Tehnicienilor Conferinta de Chimie Analitica Calea Victoriei 118 Bucuresti Romania. Printed by W Heffer &Sons Ltd Cambridge England

ISSN:0037-9697    

DOI:10.1039/SA9700700136

出版商:RSC    

年代:1970

数据来源: RSC