262 REPORT OF THE ANALYTICAL METHODS COMMITTEE, 1957 [Vol. 83 Report of the Analytical Methods Committee 1957 EACH of the two preceding annual Reports of the Analytical Methods Committee of the Society for Analytical Chemistry covered the work of one year. This present Report, however, reviews the three years that have elapsed since the Committee was reorganised as a self-supporting unit of the Society. ’This over-all account of the Committee’s work is given because many of the subscribers to the Trust Fund, who so generously responded to the Society’s appeal at the end of 1954, initially promised donations for three years to establish the Committee’s work. GENERAL REVIEW In the early part of 1957 the Committee was very sorry to lose, through resignation, Dr. J. K. Nicholls and Mr.N. L. Allport, both of whom had been valued members for many years, and the opportunity is taken here to thank them for all their help. The Committee was glad to welcome in June Mr. E. Q. Laws and Mr. C. Whalley as their successors. PROGRESS OF WORK- Originally the secretarial work of the Committee itself and each of its sub-committees and panels was undertaken voluntarily by one of the members, all of whom had full-time duties in their own spheres of work. Not only had it become necessary to relieve members of the onus of this secretarial work, but it became increasingly difficult to extend the field of investigation and a central paid secretariat became essential. This led to the Appeal to Industry to put the Committee on a sound financial basis. The present arrangement of having a small technical secretariat office within the Society’s offices has been much appreciated by committee members and has facilitated co-ordination and enabled quicker progress to be made.Further, because the office also acts in an editorial capacity, the time between the completion of the collaborative work of a committee and the publication of its reports has been greatly reduced. These advantages have been well demonstrated by the rapid progress of work by the Joint Committee on Methods for the Analysis of Trade Effluents set up by the Society and the Association of British Chemical Manufacturers in 1954. In view of Industry’s need for recommended methods, the priority given to this work has maintained a steady output and ensured that the methods appeared in print as soon as possible after they were approved.The effort has been well rewarded, since tlhe Joint Committee with its four working panels completed its entire programme (much of it entailing collaborative experimental work) by the end of 1957 and has published in The Analyst no less than 46 methods since the beginning of 1956. These, together with the remaining 6 methods just completed, are being collected and will be published in the Spring of 1958 as a complete volume of some 150 pages. The Analytical Methods Committee itself has published 3 reports of original collaborative work carried out by its sub-committees-one of these, “The Estimation of Vitamin B,,,” was published in The Aua2yst in 1956 and the other two, “The Determination of Linalol in Essential Oils” and “The Determination of Small Amounts of Total Organic Chlorine in Solvent Extracts of Vegetable Material,” iin 1957.In other sub-committees, collaborative experimental work is still in progress, but lit is expected that the results of some of this will be ready for publication in 1958. The arrangement for investigating analytical problems by collaboration between two or more organisations, as exemplified by the work on the analysis of trade effluents, proved to be so satisfactory that another Joint Committee, this time with the Pharmaceutical Society, was set up in March, 1956, to prepare standard methods of assay of crude drugs and kindred materials, such as those that are used widely in commerce, but for which there are no standard or official methods at present in force.This Joint Committee immediately appointed four working panels to investigate chemical methods for digitalis, capsicum (capsaicin content), anthraquinone drugs and rauwolfia, respectively. A fifth panel, to investi- gate methods for the assay of lonchocarpiis and derris, was appointed in July, 1957. All five panels are actively engaged in experimental work and it is interesting to note that eachNay, 19583 REPORT OF THE ANALYTICAL METHODS COMMITTEE, 1957 263 panel has, from the first, turned its attention to a thorough study of the active ingredients of the crude drugs. Further evidence of the value of joint investigations by several organisations has been the recent agreement by the Society (represented by the Analytical Methods Committee) to collaborate with the Association of British Insecticide Manufacturers and with the Scientific Sub-committee on Poisonous Substances used in Agriculture and Food Storage of the Ministry of Agriculture, Fisheries and Food to test methods of analysis for pesticides residues in foodstuffs.In this investigation, the secretarial work is to be undertaken by the Ministry and ad hoc working panels are to be appointed when methods are considered ready for collaborative trial. More detailed accounts of the work of the various Joint Committees, sub-corninittees and panels are given later in this Report. ANALYTICAL METHODS TRUST- The Committee is fortunate in having Mr. Justice Lloyd-Jacob as Chairman of the Analytical Methods Trust; it owes much to his direction of its financial affairs and to his lively interest in the progress of work.A successful 3-year trial period has been completed-an achievement that would not have been possible without the very generous help during this period from the many sub- scribers to the Trust Fund. Its future work will, however, depend on an assured income; in order to secure this, the Trustees are to appeal to Industry for the continuation of the subscriptions to the Trust Fund. RESEARCH GRANTS- In the past, the work of a committee frequently suffered because members found it impossible to investigate problems fully, since the amount of work involved would have required concentrated research. It was hoped, therefore, that the Trust Fund formed by subscriptions received as a result of the Appeal to Industry in 1954 would be large enough to allow some money to be set aside for research purposes after the secretariat’s expenses had been met.It was most gratifying that the response was such that the first grant could be made a few months after the Com- mittee was established on its new basis, with the result that a Research Scholar was appointed to carry out full-time work for a period of 2 years on a problem frequently encountered by analysts-namely, the causes of losses or accretions of some metals during the destruction of organic matter. Again, at the end of 1957, it was possible to make a second grant to permit full-time research on the investigation of a problem that had arisen in the course of the work of the Joint Committee engaged in devising methods of analysis of trade effluents.In addition to making these specific grants for research, it has been possible to help in the work of the Joint Committee that is investigating methods of assay of crude drugs by the purchase of special materials. As the work of the various committees continues to expand, it is envisaged that further grants for research will be made in the near future. Research scholarship-Mr. T. T. Gorsuch, the Society’s first Research Scholar, was appointed at the beginning of 1956 to work at the Atomic Energy Research Establishment, Harwell, mder the direction of Mr. A. A. Smales, and the Society is grateful to the Director of that Establishment for the facilities afforded there. The research is nearing completion and an account will shortly be published; it is also expected that the results will be of sufficient general interest to be the subject of a paper for presentation at one of the Society’s meetings.The research work has entailed the application of radiochemistry, by means of radioactive tracers as well as gamma spectrometry after neutron activation, (a) to the specific problem of defining the losses that can occur during the preparation of organic materials for trace- element analysis, investigating the causes of these losses and determining the optimum conditions for their elimination, and (6) to the various individual problems that have confronted the Metallic Impurities in Organic Matter Sub-committee in its work. Research on methods for the determination of traces of silver-The grant made recently by the Trustees is being used for research, under the direction of Dr.H. M. N. H. Irving[Vol. 83 at Oxford, to devise a method for the deterniination of traces of silver in the presence of organic matter. This arose from the work of the Joint Committee on Methods for the Analysis of Trade Effluents, which indicated that, in the event of accidental contamination of rivers by silver, a method should be available for determining amounts down to 0-01 parts per million. It was envisaged that the work would take about 6 months. INCOME AND EXPENDITURE- The audited statement of accounts (see Appendix I) for the financial year ending October 31st, 1957, shows an expenditure of L4774. This figure includes expenses in con- nection with the Research Scholarship (the grant of A600 for research on silver analysis was not approved until after the end of the financial year) and shows an increase of A1419 over last year’s figure.The income from donations for 1957 amounted to A5900 received from 49 subscribers -about L450 less than was received in 1956. Of the organisations that supported the original appeal in 1954, 17 per cent. entered into 7-year Deeds of Covenant and 33 per cent, promised annual donations for a period of 3 years; the remaining 50 per cent. of the subscribers preferred to consider the matter from year to year. In view of the uncertain income derived in this way, the Trustees considered that it would be prudent to build up a reserve during the 3 years whilst the Committee established itself so that the various sub-committees and panels could be assured of the continuance of their work.For this reason, although the Committee’s work has expanded steadily, a reasonable economy has been observed diiring this time and the secretariat staff of three has not been increased. However, after the initial period in which considerable work has been undertaken, as can be seen from the report that follows, the potential value of the Committee’s work to Industry has become apparent and an ever-increasing programme of work must be expected. This can only be done with an assured income. It is hoped that the support given by Industry will continue so that this more ambitious programme can be undertaken with confidence. 264 REPORT OF THE ANALYTICAL METHODS COMMITTEE, 1957 REPORTS OF SUB-COMMITTEES OF THE ANALYTICAL METHODS COMMITTEE ESSENTIAL OILS SUB-COMMITTEE CONSTITUTIOX- G.W. Ferguson, B.Sc., Ph.D., F.R.I.C. A. J. M. Bailey, B.Sc., F.P.S., F.R.I.C. D. Holness, R.A. H. T. Islip, B.Sc., F.R.I.C. P. McGregor, B.Sc., A.H.-W.C., F.R.I.C. J. H. Seager, M.Sc., F.R.I.C. G. E. Smith, B.Sc., F.R.I.C. B. D. Sully, B.Sc., Ph.D., A.R.C.S., F.R.I.C. (Chairman) Analytical and ConsulEing Chemist W. J . Bush & Co. Ltd. Unilever Ltd., Central Perfumevy Department TroFical Products Institute Department of the Government Chemist Yardley G. Co. Ltd. Staffoord Allen & Sons Ltd. A . Boake, Roberts & Co. Ltd. PROGRESS OF WORK- When the Analytical Methods Commit tee was reorganised in 1955, some sub-committees were automatically dissolved and subsequently reconstituted because the scope of work had been broadened.The original Essential Oils Sub-committee, however, continued in being until the report of their collaborative work on methods for the determination of linalol had been completed. This report was eventually published in The Amlyst in May, 1957. The Sub-committee was reorganised in February, 1957, under the Chairmanship of Dr. G. W. Ferguson. One meeting has since been held, and it was considered that the future programme of work would depend somewhat on requests for collaboration from the corre- sponding technical committee of the British Standards Institution. MEAT PRODUCTS SUB-COMMITTEE CONSTITUTION- S. M. Herschdoerfer, Ph.D., F.R.I.C. S. Back, B.Sc., F.R.I.C.(Chairman) T. Wall & Sons Ltd. Crosse & Btackwell Ltd.May, 1958] REPORT OF THE ANALYTICAL METHODS COMMITTEE, 1957 265 British Food Manufacturing Industries Research 0x0 Ltd. Department of the Government Chemist 0x0 Ltd. Miss E. &I. Chatt, B.Sc., F.R.I.C. C. D. Essex, A.M.Inst.B.E., F.R.I.C. J. R. Fraser, B.Sc., A.C.G.F.C., F.R.I.C. H. G. Kees, B.Sc., Ph.D., A.R.C.S., D.I.C., Association F. R. I .C. H. Amphlett Williams, Ph.D., A.C.G.F.C., Public Aizalyst F. R. I .C. 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. Nom-The term 'meat products' to include hydrolysed protein and, if found necessary, fish pastes." PROGRESS OF WORK- The previous Sub-Committee, under the name of the Meat Extracts Sub-Committee, was dissolved in 1855 and reconstituted with extended terms of reference and a title indicative of its wider scope.Collaborative experimental work is being undertaken with particular reference to review- ing the values of the factors for nitrogen for various types of meat, since some dissatisfaction of existing values has frequently been expressed. The need for establishing values within closer limits than hitherto is directly associated with new legislation under the Food and Drugs Act, in which the meat content of sausages and meat pies might be stipulated; in this event reliable tests for compliance with the ,4ct would be necessary. In addition, methods for the determination of starch are under review during the collaborative tests.METALLIC IMPURITIES IN ORGANIC MATTER SUB-COMMITTEE CONSTITUTION- T. McLachlan, D.C.M., A.C.G.F.C., M.I.Biol., Public Analyst L. Brealey, BSc. Boots Pure Drug Co. Ltd. J. C. Gage, R.Sc., Ph.D., F.R.1.C.t Imperial Chemical Industries Ltd. (Industrial Hygiene Laboratories) C. L. Hinton, F.R.I.C. British Food Manufacturing Industries Research A ssociation E. I. Johnson, M.Sc., F.R.I.C. Department of the Government Chemist 'CV. C. Johnson, M.B.E., F.R.I.C. Hopkin & Williams Ltd. I. MacIntyre, M.B., Ch.B. University of London (Post-Graduate Medical R. F. Milton, B.Sc., Ph.D., M.I.Biol., F.K.I.C. Analytical and Consulting Biochemist G. Taylor, O.B.E., F.R.I.C." Public Analyst, Oficial Agricultural Analyst and G.E. Willis, B.Sc., Ph.D., A.R.I.C. Imperial Chemical Industries Ltd. (Dyestufis F.R. I.C. (Chairman) School) Consulting Chemist Dizlision) * Resigned-November, 1957. t Elected-December, 1957. TERMS OF REFERENCE-"TO investigate the determination of small quantities of metals in organic matter." PROGRESS OF WORK- In the course of its work on the methods for both arsenic and lead, the Sub-Committee came to the conclusion that one of the chief reasons for variation in experimental results could be attributed to the losses or retention occurring during the destruction of organic matter. Accordingly it was decided that the reports on the trace metals should be confined to the method of determination of the element with only general reference to the preliminary treatment.Methods for the destruction of organic matter in general, with recommendations for appropriate procedure in particular cases, should be dealt with in a separate report, which is now under consideration. The Sub-Committee came to the conclusion that the use of perchloric acid in the pre- liminary treatment of the sample should be encouraged and it has prepared a note for publication as a guide to the precautions that should be taken and the conditions under which perchloric acid may be used with safety.266 REPORT OF THE ANALYTICAL METHODS COMMITTEE, 1957 [Vol. 83 Investigations into the molydenum-blue method for the determination of arsenic are now in the final stage; after preliminary collaborative tests with simple solutions of arsenic, a series of tests on samples containing organic matter has been carried out and the results compared with those obtained by radiochemical methods at Harwell.A report on the work and on the method is in preparation. Experimental work on the revised method for lead has been completed and it is hoped that the final report will be approved shortly. The recommended methods for the determination of arsenic, lead and copper that were originally published as Analytical Methods Committee Reports have been reviewed by the Sub-committee; that for arsenic (Gutzeit method) has been revised and approved for publication; those for copper and lead were considered to be out of date. The Sub-committee has been greatly assisted by the fundamental research done by Mr. Gorsuch at Harwell under the direction of Mr.Smales and is grateful to them also for their ready co-operation in helping to solve ad hoc problems in the course of the Sub- Committee’s work. DIRECT MICRO-DETERMINATION OF OXYGEN CONSTITUTION- D. W. Wilson, M.Sc., F.R.I.C. G. C. Ackroyd, B.Sc., A.R.I.C. P. R. W. Baker, B.Sc., A.R.I.C. Miss B. B. Bauminger, Ph.D., A.I.R.I., F.R.1 .C. W. T. Chambers, B.Sc., Ph.D., A.R.I.C. A. F. Colson, B.Sc., Ph.D., F.R.I.C. (C hairman) Miss M. Corner, B.Sc., F.R.I.C. R. R. Gordon, Ph.D. G. Ingram, A.R.I.C. F. J. McMurray F. H. Oliver H. J. Warlow C. Whalley, B.Sc., F.R.I.C. I N ORGANIC MATTER SUB-COMMITTEE Sir John Cass College (Department of Chemistry) D.S. I.R., Fuel Research Station Wellcome Research Laboratories Dunlop Research Centre British Rubber Producers’ Research Association Imperial Chemical Industries Ltd.(Alkali D.S.I.R., Chemical Research Labovatory National Coal Board, Central Research Estab- Courtaulds Ltd. Wellcome Chemical Works Parke, Davis & Co. Ltd. D.S.I.R., Fuel Research Station Lapovte Chemicals Ltd. Division) lishment TERMS OF REFERENCE-“TO investigate the Unterzaucher method, and its modifications, for the micro-determination of oxygen.’’ PROGRESS OF WORK- The Sub-committee is nearing the end of its second series of collaborative tests in which, as a result of the preliminary investigation of differences of technique during the first series, the experiments have beeLl designed with the object of reducing the “blank” values and of isolating possible sources of error. Because of the multiplicity of small modifications in technique that have been adopted from time to time by various laboratories, this second series of tests is very lengthy, but it is hoped that it will be possible to formulate a more closely defined technique as a result.TRACE ELEMENTS IN FERTILISERS AND CONSTITUTION- C. J. Regan, BSc., F.R.I.C. S. M. Boden, B.Sc., A.R.I.C. L. Brealey, BSc. S. G. Burgess, B.Sc., Ph.D., F.Inst.Pet., J. H. Hamence, M.Sc., Ph.D., F.R.I.C. R. l?. Milton, BSc., Ph.D., M.I.Biol., F.R.I.C. R. L. Mitchell, BSc., Ph.D., F.R.S.E., F.R.I.C. J. B. E. Patterson, M.Sc., F.R.I.C. (Chairman) N.Inst.S.P., F.R.I.C. FEEDING-STUFFS SUB-COMMITTEE Formerly Chemist-in-Chief, Loadon. County Council Ministry of Agriculture, Fisheries and Food, National Agricultural A dvisovy Service Boots Pure Drug Co.Lld. London County Council Public Analyst, Oficial Agricaltural Analyst and Consulting Chemist Analytical and Consulting Biochemist Macaulay Institute f o r Soil Research (Department of S9ectrochemistry) Ministry of Agriculture, Fishevies and Food, National Agricultural Advisory ServiceMay, 19581 REPORT O F THE ANALYTICAL METHODS COMMITTEE, 1957 267 TERMS OF REFERENCE-“TO devise appropriate methods of analysis (to be recommended for inclusion in the Regulations under the Fertilisers and Feeding Stuffs Act, 1926) for the determination of boron, cobalt, copper, fluorine, iodine, iron, magnesium, manganese, molybdenum, selenium and zinc, which can be expected to be present in fertilisers and. feeding stuffs.” PROGRESS OF W~ORK- The original Sub-committee was not dissolved immediately after the reorganisation of the Analytical Methods Committee because it was hoped that it would be possible to proceed with the programme of work, although members were finding it increasingly difficult to devote sufficient time to the amount of research that was involved. It was apparent that some of the methods that were being investigated by the Joint Committee on Methods for the Analysis of Trade Effluents might be applicable for fertilisers and feeding stuffs and it was decided to wait until these were published.Accordingly, after the appearance of these methods, during the past few months, the position was reviewed by the Analytical Methods Committee with the result that in September, 1957, the Sub- committee was reconstituted under the Chairmanship of Mr.C. J. Regan. Since then 3 meetings have been held and considerable progress has already been made; collaborative experimental work is being carried out to check the suitability of selected published methods (including a number of those recommended for trade effluents) and to make any modifications that may be necessary. VITAMINS The original Vitamins Sub-committee was dissolved at the time when the Analytical Methods Committee was reorganised, but the Panel on Vitamin E continues its investigations. Vitamin-E CONSTITUTIOX- A. L. Bacharach, MA., F.R.I.C. J. Green, B.Sc., Ph.D., F.R.I.C. V. H. Booth, Ph.D. I;. Brown, M.Sc., PI.1.D. A. R. Moss, B.Sc., Ph.D. H. N. Ridyard, B.Sc., A.K.C., F.R.I.C. P. W. Russell Eggitt, B.Sc., Ph.D., R.R.I.C. C.A. Shacklady, B.Sc., A.R.I.C. P. Stross, B.Sc. G. Walley, B.Sc., F.R.I.C. R. J. Ward, B.Sc., S.R.I.C. E. C. Wood, B.Sc., Ph.D., A.R.C.S., F.R.I.C. P. Harris, Ph.D.* (Chairmarz) (Honorary Technical Secvetary) Panel Consulti pig Chemist Vitamins Ltd. i?Wedical Research Council, Dun% hrutritional Laboratory Foot-azd-Mouth Disease Research Institute Roche Products Ltd. Research A ssociation of Byitisla Flour Millers Sfiillers Ltcl. J . Bibby & Sons Ltd. Bvitish Drug Houses Ltd. Unilever Ltd. Medical Research Council, Dunn Nutritional PLiblic A ~ a l y s t aqzd Consulting Chenzist Distillation Products Industries, Rochester, New Labovatory York, U.S.A. * Corresponding member. TERMS OF REFERENCE (OF ADVISORY PANEL)--I ‘To survey the methods already proposed for the estimation of Vitamin E and to recommend to the [Vitamins] Sub-committee a standard method or methods.” PROGRESS OF WORK- During the year the Panel has been engaged in working out the manipulative details of a procedure for the differential micro-analysis of tocopherols in natural oils and in complex samples, such as poultry meals.The method involves a paper-chromatographic separation of the tocopherols, after puri- fication, followed by their individual assay by a modification of the Emmerie-Engel colorimetric method. Although a considerable amount of manipulative skill is required, the Panel is of the opinion that the method has many advantages; it is hoped that the final recommendations will be published soon as a Report.268 REPORT OF THE ANALYTICAL METHODS COMMITTEE, 1957 [Vol.83 REPORT OF THE A.B.C.M. - S A C . ,JOINT COMMITTEE ON METHODS FOR THE ANALYSIS OF TRADE EFFLUENTS MAIN COMMITTEE CONSTITUTION- Representing the Associatio.lz of B v t i s h Chemical Manufacturers- H. N. Wilson, F.R.I.C.* Imperial Chemical Industuies Ltd. (Billingham J. G. Maltby, B.Sc., F.R.I.C.* Distillers Co. Ltd. F. G. Broughall, B.Sc., F.R.T.C. Midland T a r Distillers Lid. D. C. Garratt, Ph.D., D.Sc., F.R.I.C. Boots Pure Drug Co. Ltd. I. S. Wilson, M.Sc., Ph.D., A.R.I.C. Monsanto Chemicals Ltd. Representing the Society f o r ,4 nalyticul Chemistry- J. H. Hamence, M.Sc., Ph.D., F.R.I.C.8 Public Analyst, Oficial Agriczcltural Analyst and L. Klein, 1\9.Sc., Ph.D., M.Inst.S.P., F.R.I.C. Mersey River Board C.J. Regan, B.Sc., F.R.I.C. Formerly Chemist-in-Chief, London County J. G. Sherratt, BSc., F.R.I.C. Public Analyst and Consulting Analytical Chemist N. T. Wilson, F. K.I. C. Imperial Chemical Industries Ltd. (Alkali I<. A. Williams, B.Sc., Ph.D., A.Inst.P., M Inst.Pet , ( C h airman) Division) (Secretary) Consulting Chemist Council Division) Analytical and Consulting Chemist F.R.I.C. J. S. Evans Miss C. H. Tinker, B.Sc. , Ph.D., A.R.I.C." * Members of the Publications Sub-committee, to which J . B. Attrill, M.A., F.R.I.C., Editor of The Analyst, has been co-opted. TERMS OF REFERENCE-"TO devise and recommend methods of analysis as applied to trade effluents, specifying in each case their applicability and limitations, but not the interpretation of the results of such tests as would be used to decide on the quality of an effluent." PANEL 1 : ORGANIC MATTER-GEKERAL CONSTITUTION- Federation of British Indwtries Secretary to the Analytical Methods Committee C.J. Regan, B.Sc., F.K.I.C. G. S. Clements, A.R.C.S., F.R.I.C. W. M. Cameron, M.Inst.S.P., F.R.I.C. (Chairman) (Secretary) 'CV. T. Lockett, M.Sc. T. B. Moore, B.Sc. A. E. J. Pettet, B.A. I. S. Wilson, M.Sc., Ph.D., A.R.I.C. Miss C. H. Tinker, B.Sc., Ph.D., A.R.I.C. Formerly Chemist-in-Chief, London County Public Health Department, London County M a i n Drainage Department, Middlesex County Formerly of the M a i n Drainage Department, North Thames Gas Board D.S.I.R., Water Pollution Research Laboratory Monsanto Chemicals Ltd. Secretary to the Analytical Methods Committee COM'PZCZ'I Council Council Middlesex County Coumil PANEL 2 : METALLIC CONTAMINANTS CONSTITUTION- N.T. Wilkinson, F.R.I.C. R. Belcher, Ph.D., DSc., F.Inst.F., F.R.I.C. D. C. Garratt, Ph.D., D.Sc., F.R.I.C. J. H. Hamence, M.Sc., Ph.D., F.R.I.C. J. G. Sherratt, B.Sc., F.R.I.C. Miss C. H. Tinker, B.Sc., Ph.D., A.R.I.C. (Chairman) (Secretary) Imperial Chemical Industries Ltd. (Alkali University of Birmingham (Department of Boots Pure Drug Co. Ltd. Public Analyst, Oficial Agricultural Analyst and Public Analyst and Consulting Analytical Chemist Secretary to the Analytical Methods Committee Division) Chemistry) Consulting Chemist PANEL 3 : NON-ME:TALLIC CONTAMINANTS CONSTITUTION- F. G. Broughall, B.Sc., F.R.I.C. Midland Tar Distillers Ltd. (Chairman)May, 19581 REPORT OF THE ANALYTICAL METHODS COMMITTEE, 1957 269 Public Analyst and Oficial Agricultural Analyst; South Essex Waterworks Co.Wallace E Tiernan Ltd. W. G. Carey, F.R.I.C. G. U. Houghton, M.Sc., Ph.D., F.R.I.C. E. A. W. Whitlock, B.Sc., A.R.I.C. Consultant (Deputy: J. F. Malpas, B.Sc., A.R.I.C.) PANEL 4: PHYSICAL TESTS CONSTITUTION- J. G. Sherratt. BSc., F.R.I.C. L. Klein, M.Sc., Ph.D., M.Inst.S.P., F.H.I.C. G. A. Vaughan, F.R.I.C. K. A. Williams, B.Sc., Ph.D., A.1nst.P. Miss C . H. Tinker, B.Sc., Ph.D., A.R.I.C. Public Analyst and Consulting Analytical Chemist Mersey River Board Coal T a r Research Association Analytical and Consulting Chemist Secretary to the Analytical Methods Committee (Chairman) M.Inst.Pet., F.R.I.C. (Secretary) PROGRESS OF WORK- With the passing of the Rivers (Prevention of Pollution) Act in 1951 it became obvious that there should be accepted methods of analysis available in the event of dispute arising as to the composition of trade effluents.The Federation of British Industries Legislation Committee, therefore, asked the Association of British Chemical Manufacturers to investigate the position and to take the necessary steps to implement the work of approving or devising suitable methods of analysis. The result of the investigation was the formation of this Joint Committee of the Associa- tion and the Society for Analytical Chemistry, with the terms of reference quoted above, and the first meeting was held in March, 1954. In view of the urgent need for recommended methods it was decided that they should be published individually in The Analyst as soon as they were deemed satisfactory, rather than waiting until a complete collection had been made.Since this procedure would produce a haphazard collection of methods, it was also decided that they should subsequently be arranged and published as an integrated volume. Because the existing literature on the analysis of trade effluents was found to be scant, the Joint Committee’s task proved to be more arduous than had at first been envisaged and, although the majority of methods that have been recommended are based on existing ones, it was usually found necessary to make modifications to take into account the possibility of interference by a number of substances under very varying conditions. Consequently, it was imperative that before such modified methods could be finally recommended, they should be subjected to check tests by panel members.Some methods, on the other hand, had to be specially devised with a good deal of attendant experimental work. It is gratifying to report that, after just over 3& years of unremitting and intensive work by its four panels, the Joint Committee’s programme was completed at the end of 1957’. Practically all of the methods have been published in The AnaZyst since January, 1956. The remaining six methods have only just been completed and approved and are being included directly in the book, publication of which is expected before the end of April, 1958. They will, however, also appear in The Analyst. Mention has already been made in the General Review section of this Report of the research that is proceeding under the direction of Dr.Irving to devise a method that is sensitive enough for determining minute traces of silver in the presence of organic matter. It was considered advisable to include a method for silver because of its extreme toxicity to fish, although it is very unlikely that it will be a common contaminant in view of its economic value. Because many laboratories have to undertake the analysis of sewage effluents as well as trade wastes, cognisance has been taken of the methods recommended by the Ministry of Housing and Local Government in their publication “Methods of Chemical Analysis as Applied to Sewage and Sewage Effluents’’ (Second Edition, 1956) and, where possible, similar methods (modified as necessary to cover the special requirements for trade effluents) have been recommended.This need for uniformity is especially desirable where empirical methods are used and permission was, therefore, obtained from H.M. Stationery Office for reproduction in full of the methods for the determination of biochemical oxygen demand and of dissolved oxygen.270 REPORT OF THE ANALYTICAL METHODS COMMITTEE, 1957 REPORT OF THE P.S. - S.A.C. JOINT COMMITTEE ON METHODS OF ASSAY OF CRUDE DRUGS [Vol. 83 WAIN COMMITTEE CONSTITUTION- Representing the Pharmaceutical Society of Gveat Britain- K. R. Capper, Ph.D., B.Pharm., F.P.S., D.I.C. R. Higson, F.P.S. W. Mitchell, BSc., Ph.D., F.R.I.C. R. E. Stuckey, Ph.D., DSc., F.P.S., F.R.I.C.Representing the Society for Analytical Chemzstry- C. A. Johnson, BSc., B.Pharm., F.P.S., A.R.I.C. H. C. Macfarlane, A.R.T.C.S., F.R.I.C. D. Watt, F.P.S. D. C. Garratt, Ph.D., D.Sc., F.R.I.C. Representing the Tropical Products Institute-- A. J. Feuell, BSc., Ph.D., A.R.I.C. Pharmaceutical Society of Great Britain Ministry of Health, Supplies Division Staflord Allen & Sons Ltd. British Brug Houses Ltd. Boots Pure Drug Co. Ltd. Analytical and Consulting Chemist T. & H. Smith Ltd. Chairman of the Analytical Methods Committee (Chairman) (ex oficio) Tropical Products Institute Miss C. H. Tinker, BSc., Ph.D., A.R.I.C. (Secretary) TERMS OF REFERENCE--“TO prepare standard methods of assay of crude drugs and kindred materials.” PROGRESS OF WORK- As mentioned in the General Review section of this Report, this Joint Committee of the Pharmaceutical Society and the Society for Analytical Chemistry was set up in March, 1956.Five working panels have been appointed so far, and the progress of their work is reported individually below. Other panels will be appointed from time to time, when urgent problems present themselves. CONSTITUTION- PANEL 1 : Digitalis j!”~Z4?‘ea-CHEMICAL METHOD Professor H. Brindle, MSc., F.P.S., F.R.I.C. G. E. Foster, BSc., Ph.D., F.R.I.C. G. J. Rigby, MSc., Dip-Bact. J. M. Rowson, MSc., Ph.D., F.P.S. K. L. Smith, M.P.S. Professor J. P. Todd, Ph.D., F.P.S., F.R.I.C. Miss A. M. Parry, BSc. Emeritus Professor of Pharmacy, Univevsity of Weilcome Chemical Works University of Manchester (Department of Phar- Pharmaceutical Society of Great Britain Boots Pure Drug Co.Ltd. Royal College of Science aPzd Technology, Glasgow (School of Pharmacy) (Chairman) Manchester macy 1 (Secretary) TERMS OF REFERENCE-“TO investigate chemical methods for the assay of digitalis and its preparations and to attempt to correlate them with the biological method of assay.” PROGRESS OF WORK- As a preliminary to its work the Panel is comparing the figures for potency of the drug as obtained by standard biological methods with those obtained by chemical methods for the determination of the total active glycosides to find out whether any correlation exists. Collaborative tests have been carried out on two samples of digitalis leaf, one being a “good” leaf and the other a “poor” leaf (as determined by biological assay).Determinations of the glycoside content by several chemical methods have yielded good agreement between laboratories, but so far these show no correlation with the biological assay. As it appears that several glycosides are responsible for the total activity of the drug, and others are inactive, methods involving chromatographic separation and estimation of the total primary glycosides are now being studied. It is by no means certain that existing biological methods give a true indication of the potency of the leaf and it is hoped to arrange for information on this point to be obtained from clinical tests, and by comparison of different methods of biological assay.May, 19581 REPORT OF THE ANALYTICAL METHODS COMMITTEE, 1957 271 The Panel is most grateful to Messrs.F. Hoffmann - La Roche & Co. Ltd. A.G. for a gift of 10 g of pure digitoxin to be used as a reference standard a t a later stage in the work. CONSTITUTION- PANEL 2 : CAPSICUM-CAPSAICIN CONTENT H. B. Heath, M.B.E., B.Pharm., F.P.S. E. A. Elsbury, F.R.I.C. C . A, MacDonald, B.Sc., F.R.I.C. G. R. A. Short, F.P.S. D. 0. Singleton, B.Sc. Miss A. M. Parry, B.Sc. Staflord Allen & Sons Ltd. Parke, Davis G. Go. Ltd. Evans Biological Institute W . J . Bush & Co. Ltd. Beecham Maclean Ltd. (Chairman) Miss B. M. Luckett w. J . ~ u ~ h tj, co. Lta. (Secretary) TERMS OF REFERENCE-~TO investigate methods of assay of capsicum and capsicum products with particular reference to the determination of the capsaicin content .” PROGRESS OF WORK- Several published methods have been critically examined and after an appreciable amount of collaborative work considerable progress has been made towards the establishment of a satisfactory method of determining the capsaicin content of chillies and also of oleoresins prepared from them.This consists in two alternative procedures for the isolation of capsaicin, one chromatographic and the other by alkali extraction, after which the capsaicin content is calculated directly from the extinction value. A confirmatory colorimetric method has, after considerable modification, also been found to be acceptable. It had been hoped that this method would give results sufficiently accurate to quote an extinction value for the coloured capsaicin complex, but this has not proved to be so and it is, therefore, necessary to prepare a standard absorption curve at the same time as the test.The possibility of finding an alternative synthetic standard to avoid constant handling of capsaicin is still under consideration. Future work will be concerned with the application of the methods to paprika, tinctures and other preparations containing capsaicin. CONSTITUTION- PANEL 3 : ANTHRAQUINONE DRUGS J. M. Rowson, M.Sc., Ph.D., F.P.S. J . W. Fairbairn, B.Sc., Ph.D., F.P.S., F.L.S. Pharmaceutical Society of Great Britain University of London, School of Pharmacy (Chairman) F.R.I.C. C. W. H. A. Johnson, B.Sc., B.Pharm., F.P.S., A.R.I.C. Mitchell, B.Sc., Ph.D., F.R.I.C. A. Ryan, B.Sc., F.R.I.C. Boots Pure Drug Go. Ltd. Stafford Allen tj, Sons Ltd. Westminster Laboratories Ltd.Allen G. Hanburys Ltd. W. Smith, B.Sc., F.R.I.C. Miss A. M. Parry, B.Sc. (Secretary) TERMS OF REFERENCE-“TO investigate methods for estimating the purgative activity of drugs and preparations of drugs containing anthraquinone derivatives with a view to recommending standard methods of assay.” PROGRESS OF WORK- Collaborative work is being carried out on samples of both Alexandrian and Tinnevelly senna pod and a comparison is being made between the sennosides content found by chemical methods and the activity determined by biological assay. PANEL 4: RAUWOLFIA CONSTITUTION- C. A. Johnson, B.Sc., B.Pharm., F.P.S., A.R.I.C. T. Davies, B.Sc., A.R.I.C. F. G. Farrell, B.Pharm., M.P.S., A.R.I.C. J. J. Lewis, M.Sc., F.P.S. A. W. Peacock, B.Pharm., F.P.S. Miss A.M. Parry, B.Sc. Boots Pure Drug Co. Ltd. CIBA Laboratories Ltd. Pharmaceutical Society of Great Britain University of Glasgow (Department of Materia Riker Laboratories Ltd. (Chairman) Medica and Therapeutics) (Secretary)272 REPORT OF THE ANALYTICAL METHODS COMMITTEE, 1957 [Vol. 83 TERMS OF REFERENCE-"TO investigate methods of assay for rauwolfia and its preparations with particular regard to the content of reserpine and related alkaloids." PROGRESS OF WORK- The main problems confronting the Panel in formulating a suitable assay procedure are the considerable number of alkaloids present in rauwolfia as well as the large number of species of rauwolfia in which distribution of the alkaloids varies. The first year's work has been devoted to the study of RauuoZJia serpentina, which is one of the major commercial sources and for which there is a method published in the B.P.Codex, 1954. It has been decided to seek to establish a method indicating the com- mercial value of the sample as a source of reserpine, rather than to devise a method that would show correlation with the biological activity of the whole root. Two approaches to the problem have so far been considered, both of which are based on published methods. Good progress is being made in the investigations on one of these, a colorimetric method, which it is hoped may prove suitable for recommendation while investigations into a more specific and fundamental method continue. Preliminary exploratory work on the ultra-violet absorption characteristics of reserpine and rescinnamine and of the acids produced as decomposition products showed the second method to be basically unsound because of the rapid deterioration of one of the acids when exposed to light.The cause of this deterioration is now being studied and it is hoped that valuable information may emerge regarding the mechanics of the reaction. The Panel is grateful to Messrs. CIBA Laboratories Ltd. and Messrs. Riker Laboratories Ltd. for generous gifts of samples of pure alkaloids and of RauwoZjia serpentina for use in the Panel's work. PANEL 5 : LONCHOCARPUS AND DERRIS CONSTITUTION- R. F. Phipers, BSc., Ph.D. R. Buckley, B.Sc., A.R.I.C. J. A. Dawson, B.Sc., A.R. I.C. W. E. Drinkwater, F.R.I.C. R. V. Foster, M.Sc., A.R.I.C. S. C. Jolly, B.Pharm., B.Sc., F.P.S., A.R.I.C.J. T. Martin, B.Sc., D.Sc., F.R.I.C. D. V. Richmond, B.Sc. (Chairman) W. M. Seaber, B.Sc., F.R.I.C. F. H. Tresadern Miss A. M. Parry, B.Sc. (Secretary) The Cooper Technical Bureau Plant Protection Ltd. Tropical Products Institute Boots Pure Drug Co. Ltd. The Cooper Technical Bureau Pharmaceutical Society of Great Britain University of Bristol (Long Ashton Research University of Bristol (Long Ashton Research Salamon & Seaber Stafford Allen & Sons Ltd. Station) Station) TERMS OF REFERENCE-"TO investigate methods of assay of derris, lonchocarpus and their preparations, with particular reference to the determination of their rotenone content ," PROGRESS OF WORK- At the Panel's first meeting in July, 1957, it was agreed that, although methods exist for use in trade transactions in derris and lonchocarpus, the agreement between different analysts' results is unsatisfactory.No collaborative work had been done on the latter, which is now the main material of commerce and there is a need for a reference method for determining the true rotenone content of the sample. Collaborative work on gravimetric methods for the determination of rotenone has begun.May, 19581 REPORT OF THE ANALYTICAL METHODS COMMITTEE, 1957 -- L11,768 -_I 273 Current Account . . . . 4493 - 142 In Hand .. .. .. - 11,493 L9861 L11,768 - APPENDIX I THE SOCIETY FOR ANALYTICAL CHEMISTRY ANALYTICAL METHODS TRUST ACCOUNTS FOR THE YEAR ENDED OCTOBER 3 1 s ~ , 1957 Income and Expenditure Account for the Y e a r Ended October 31st.1957 1956 L L 630 2274 81 168 62 26 21 83 3345 - 525 2634 ,56504 - , 5 L Rent, Light, Heat and Telephone . . . . 289 Salaries . . .. . . 2630 Office Equipment . . 487 Printing and Stationery 184 Travelling Expenses . . 20 Expenses of Meetings . . 107 Audit Fee . . . . 21 Postage and Petty Ex- penses . . . . . . 78 Scholarship Grant . . 958 Excess of Income over Expenditure for the year ended October 31st, 1957, transferred to Accumulated Fund 1164 L5938 - 3816 __I 1956 , 5 L 150 6344 6494 __ 7 2 1 10 - - ,56504 - Accumulated Fund 1956 1956 jt: Legal Expenses in connection with 93 formation of the Trust . . .. Balance carried to Balance Sheet . . 10,854 L - 9690 l9783 - L10,854 - L L Subscriptions from In- dustry as a result of Appeal : Received in 1955 for 1957... . . . 150 Received during 1957 5750 - 5900 Interest from Invest- ments : Received gross . . 7 Received net . . 2 Income Tax re- coverable . . .. 1 - 10 28 Bank Deposit Interest . . ,55938 - L 4 6779 Balance a t October 31st, 1956 . . 9690 Analytical Chemistry Research Balance a t October 31st, 1955 3 70 transferred . . .. .. Excess of Income over Expenditure for the year ended October 31st, 2634 1957 . . . . . . . . 1164 Fund- - ,59783 - L 10,854 I L9861 -[Vol. 83 274 REPORT OF THE ANALYTICAL METHODS COMMITTEE, 1957 Report of the Auditovs to the Trustees of The Society for Analytical Chemistry Analytical Methods Trust Fund We have examined the above Balance Sheet which in our opinion gives a true and fair view of the state of affairs of the Trust a t 31st October, 1957. 10 New Court, Lincoln’s Inn, LONDON, W.C.2. 4th March, 1958. (Signed) RIDLEY, HESLOP & SAIKER, Chartered Accountants, Auditors. Schedule of Investments at October 31st, 1957 Market Income Value Received Nominal Amount cost 31.10.57 Gross Ceylon Government 3:y0 Stock, 1959 . . . . 100 61 79 3 3+y0 Conversion Stock . . .. .. .. 100 83 63 4 3&y0 War Stock . . .. .. .. . . 100 100 61 3 L244 k203 L l O _____ --- - --- APPENDIX I1 SUBSCRIBERS TO THE TRUST FUND DURING 1957 Albright & Wilson Ltd. The Associated Ethyl Company Ltd. Bakelite Ltd. Baker Perkins Ltd. J. Bibby & Sons Ltd. A. Boake, Roberts & Co. Ltd. Boots Pure Drug Co. Ltd. Borax Consolidated Ltd. The British Aluminium Co. Ltd. The British Arkady Co. Ltd. British Celanese Ltd. The British Drug Houses Ltd. British Glues & Chemicals Ltd. Brotherton & Co. Ltd. Cadbury Brothers Ltd. Central Electricity Authority The Distillers Company Ltd. Dunlop Research Centre Esso Development Co. Ltd. Ferranti Ltd. Fisons Ltd. Glaxo Laboratories Ltd. Arthur Guinness, Son & Co. (Park Royal) Ltd. H. J. Heinz Ltd. Hopkin & Williams Ltd. Huntley & Palmers Ltd. Imperial Chemical Industries Ltd. Laporte Chemicals Ltd. J. Lyons & Co. Ltd. Macfarlane, Lang & Co. Ltd. John Mackintosh & Sons Ltd. Marmite Ltd. May & Baker Ltd. The Metal Box Company Ltd. The Millers’ Mutual Association Monsanto Chemicals Ltd. 0x0 Ltd. Peek, Frean & Co. Ltd. Procea Products Ltd. Reckitt & Colman Ltd. Research Laboratories, General Electric Co. Rowntree & Co. Ltd. “Shell” Research Ltd. Stafford Allen & Sons, Ltd. John & E. Sturge Ltd. Tate & Lyle Ltd. Unilever Ltd. Vitamins Ltd. Weston Research Laboratories Ltd. (formerly Allied Bakeries Research Laboratories Ltd.) Ltd.