摘要:

of the Society for Analytical Chemistry CONTENTS Honorary Member . . . . 105 New Members of Council . . 105 Summaries of Papers “Chromatography” . . . . 108 Report of the Analytical Methods Committee 1968 . . I I I Papers Accepted for The Analyst I29 Publications Received . . . . 130 Announcements .. .. .. 130 Proc. SOC. Analyt. Chem. Vol. 6 No. 7 Pages 105-130 July 1969 Vol. 6 No. 7 PROCEEDINGS OF July 1969 THE SOCIETY FOR ANALYTICAL CHEMISTRY President of the Society T S West Hon. Secretary of the Society W. H. C. Shaw Hon. Treosurer o f the Society G. W. C. Milner Hon. Ass stant Secretaries of the Society D. I. Coomber; D. W. Wilson Secretary Miss P. E. Hutchinson 9/10 SAVILE ROW LONDON WIX IAF Telephone 01-734 6205 Editor 1. B A t t r i l i Telephone 01-734 34L9 Proceedings is published by The Society for Analytical Chemistry and distributed t o 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 Ofice Blackhorse Road Letchworth Herts. (NOT through Trade Agents) price 0 The Society for Analytical Chemistry 5s. post free. Remittances MUST accompany orders. Methods for the Analysis of Non-Soapy Detergent (NSD) Products bY G. F. LONGMAN B.Sc. F.R.I.c. & J. HILTON B.Sc. A.R.I.C. (Unilever Research Laboratory Port Sunlight) Society for Analytical Chemistry Monograph No. I -+- This Monograph describes in detail the methods of analysis developed i n Unilever’s Laboratories for the identification and assay of components of NSD Products. -0- Available ONLY from The Society for Analytical Chemistry Book Department 9/10 Savile Row London WIX IAF (Not through Trade Agents) Price 15s. or U.S. $2.00 Post free A remittance made out t o “Society for Analytical Chemistry” should accompany every order. Members of the Society may purchase copies at the special price of Ss. post free.

ISSN:0037-9697    

DOI:10.1039/SA96906FX023

出版商:RSC    

年代:1969

数据来源: RSC

摘要:

July 1969 PROCEEDINGS OF THE SOCIETY Vol. 6 No. 7 FOR ANALYTICAL CHEMISTRY Honorary Member COUNCIL has resolved to elect- as an Honorary Member of the Society. Dr. Alan \;lialsh C.S.I.R.O. New Members of Council DOUGLAS ANDERSON (Chairman of the Scottish Section) is also at present Chairman of the Edinburgh and East Scotland Section of the R.I.C. After graduating with a 13.Sc. in physics with electronics at Edinburgh University in 1945 he joined the R.A.F. and was commissioned in the Technical Branch in 1946. In 1949 he returned to Edinburgh to study chemistry was Medallist in Chemistry (1 949 50 and 5l) Lucas Prizeman (1 950) Hope Prizeman (1952 and 53) graduated with first class Honours was appointed Assistant Lecturer in Chemistry (1954) Lecturer (1955) and is now Senior Lecturer. He was awarded the Ph.D.degree (1956) F.R.T.C. (1900) and D.Sc. (1968) for a Thesis based on his analytical and structural studies of polysaccharides. He is the author of several reviews and of more than 90 original papers on aspects of carbohydrate chemistry spectroscopy chromatography and organic functional-group analysis. He is co-editor v\;ith Professor Belcher of a new Series of Monographs on the latter subject and is a member of the Advisory Board of Talnntn. He is married with four children and regards chem- istry and the examination (oral) of single malts as important hobbies. He joined the Society in 1955 and served on Council from 1960 to G2 with the desirability of changing the image of the Society and of The AmZyst as his main lobby at that time. MR. 13. E. BROOKES was educated a t The Mundella School Nottingham and joined Boots Pure Drug Co.Ltd. in 1930 in the Analytical Department under A. D. Powell and J. A. Egglestone. He obtained the London University external degree in Chemistry in 1941 A.R.I.C. in 1950 and F.R.T.C. in 1955. From 1939 to 1949 he was engaged in the analysis of drugs fine chemicals and galenicals changing to the development of new products. He returned to analysis as a section head in Pharmaceutical Division later becoming head of Pharmaceutical and Chemical Divisions. He became head of Standards Office in 1966 where he is concerned with compiling recording and holding company standards specifications and methods of analysis of pro- ducts packs and raw materials. Mr. Rrooltes has served as a member of Council on 4 occasions past member of The AnaZyst Editorial Committee 1968 SAC Conference Executive Committee and Essential Oils Sub- committee of the Analytical Methods Committee.He is the immediate past chairman of the Midlands Section a member of the Midlands Section Committee and a member of the Finance Committee. He was elected to the Society in 1943. Other committees of which he has been a member include the Assay of Galenicals Organic and Inorganic Chemicals Assay of Tablets and Capsules Committees of the British Pharmacopoeia Pharmacognosy B and Formulary Standards Com- mittees of the British Pharmaceutical Codex Laboratory and Lamp-blown Glassware and Essential Oils Committees of the British Standards Institute and IS0 Essential Oils Corn- mittee Rome 1965. His hobbies include dinghy sailing music of all kinds literature and poetry.105 106 NEW MEMBERS OF COUNCIL [Proc. SOC. Aizalyt. Chevlz. MRS. DOKIS BUTTERWORTH who becomes Public Relations Officer in succession to Dr. P. G. Jeff ery is a Senior Experimental Officer at the National Physical Laboratory Teddington. She was educated at the Charles Edward Brooke Grammar School London. She joined the then Chemical Kesearch Laboratory in 1950 where she trained as a microanalyst under the late Mary Corner. She has remained at this Station throughout its transition first to the National Chemical Laboratory and then to its amalgamation with the National Physical Laboratory. She is now responsible for the Organic hficroanalytical Laboratory of the Station and has a particular interest in the analysis of thermally stable polymeric materials.She has published one paper on this sub- ject. She was awarded an L.R.I.C. in 1963. It was largely due to the encouragement of Mary Corner that she became a member of the Society and of the Microchemistry Group in 1951. She first served on the Group’s Committee from 1957 to 58 and during this period was responsible for the written history of the Group. She became Honorary Secretary to the Group in 1963 and still holds this Office. In her spare time when chemistry and housekeeping allow she pla~7s bridge (not too badly) and golf (very badly). As Public Relations Officer she hopes to encourage the continued liaison between the Society and Universities and Colleges and to draw to the attention of a11 analytical chemists the work that the Society does on their behalf. DR.A. C. DOCHERTY holds U.Sc. and Ph.L). degrees from Edinburgh University and as an undergraduate won the Crum Brown Medal and a Vans Dunlop Research Scholarship. He specialised in physical chemistry and his research topic was “Thermal Diffusion in Aqueous Solutions.” On leaving University in 1945 he joined I.C.I. in the Research Department at Billingham wJhere he worked on catalytic processes concerned with phenols later moving to the Works where he started up the first T.C.I. high pressure olefin carbonylation plant. During this period he spent 4 months studying chemical engineer- ing at the Massachussetts Institute of Technology. He was later concerned with the use of non-metallic materials such as ceramics glass and plastics for chemical plant construction; such materials are widely used in chemical processes to avoid the corrosion that often occurs with metals.In 1962 he movcd to his present position as manager of the Analytical Group of the Agricultural Division of I.C.I. at Billingham which is responsible for Analytical Research and also for Control Analysis. He has a special interest in the use of automatic methods for the analysis of fertilisers and has published several papers on this subject. He joined the Society in 1962 and was a founder member of the North East Section of which lie was elected its third Chairman this year. He has previously served Council and its Finance and Programmes Committees as an elected member and is a member of The A+zaZyst Editorial Advisory Board and Executive Committee. He is to chair the local Committee responsible for the third SAC Conference which is to be held a t Durham University in 1971.He is interested in Uouth work and for several years he and his wife have run a mixed Youth Club for the Stockton Presbyterian Church. July 19691 NEW MEMBEKS OF COLJNCIL 10 7 DR. J . R. HEWRIDGE was educated a t Lasswade School Midlotliian and Edinburgli Univer- sity where he graduatecl TZ.Sc. with honours in chemistry in 1953 and P1i.D. in analytical chemistry in 11156. In 195% he was appointed an Assistant in the Depart nient of Chemistry at Edinburgh University and since 1956 has been on the Staff of the Chemistry Department of the University of Slieffield where he was promoted t o Senior Lecturer in Analytical and Inorganic Chemistry in 1965. In 1961 he was Visiting- Lecturer at the Polytechnic Institute of Brooklyn N.Y.His chief research interests are in analytical spectroscopy and electrochemistry with special emphasis on metallurgical materials. He is author of two books and author or co-author of some forty research papers and reviews. He was Senior Reporter of the Analytical Section of Annual Reports of the Chemical Society for 1964 and 1965. For many years he was a Regional Scientific Training Officer with the Civil Defence Organisation and is a member of the B.T.S.R.A. Chemical Analysis Committee. He is an F.R.I.C. and was chairman of the local section committee of the R.I.C. in 1866 to 67. He has been a member of the Society since 1955 and is a member of the Education and Training Committee. DR. G. I;. KIRKBRIGHT was born in 1938 in North Wales. He attended the University of Birmingham where he graduated from the School of Chemistry in 1959 and subsequently joined Professor Uelcher’s Analytical Chemistry research group.He secured his P1i.D. degree in 1962 and undertook postdoctoral research in trace analysis with Professor J. H. Yoe at the Univer- sity of Virginia U.S.A. From 1963 to 64 lie held a D.S.I.R./ N.A.T.O. Fellowship and spent some time at the Technische Hochschule in Vienna. Since 1964 he has been a lecturer in the Chemistry Department Imperial College London. Dr. Kirkbright is a past member of Committees of the Nuffield Science Foundation Teaching Project and S .A. C. Special Techniques Group. He is currently serving the Society for Analytical Chemistry on Council Publications Policy Committee Education and Training Committee The Amljist Editorial Advisory Board and Executive Committee.He is also actively engaged as co-Chairman of the Technical Committee for the Inter- national Atomic Absorption Spectroscopy Conference to be held this year in Sheffield. He has published over 70 research papers and contributed chapters to two books. His principal research interests are in inorganic trace analysis by atomic and molecular spectroscopic techniques. MR. R. SINAR was educated at Bolton County Grammar School following which he entered pharmacy graduating B.Pharm. from Nottingham University in 1947. After a short period in pharmaceutical industry he joined the firm of Ruddock & Sherratt public analysts and consulting chemists obtaining the old “Branch E” diploma of the R.I.C. while so employed. In 1956 he left to take up an appointment in the Standards Department of Boots Pure Drug Co.Ltd. at Nottingham but returned in 1958 to become a partner in the practice and deputy public analyst. Mr. Sinar is Chairman of the North of England Section of the Society and is a past member of the Midlands Section Committee. He has served on numerous committees such as those of the B.P. B.P.C. B.S.I. and the Association of Public Analysts. He has been Secretary of the Standards Committee of this latter Asso- ciation for the last 10 years. His hobbies are photo- graphy and philately. He joined the Society in 1951. 108 CHROMATOGRAPHY LP'YOC. SOC. Annlyt. Client. MR. J. D. R. THOMAS is Senior Lecturer in Chemistry at the Universitj- of Wales Institute of Science and Technology (U.W.I.S.T.). He has been it iiieniber of tlie Sorietv since 1953 and is a Coninlittee Member of the Western Section and of the Cliroimatograpliy and Electrophoresis Group and is also the Group's past Chairman.Mr. Thomas was educated at Llandovery Graminar School and University College Cardiff. His university studies were broken by war service in the R.A.M.C. (Army Blood Transfusion Service) 2 years being spent in India. He completed his Bachelor's degree at upper second-class honours level in 1950. Following employment with Spillers Limited and Glainorgan County Council Mr. Thomas returned to university in 1952 to take his Diploma in Education. In 1955 and during his first lecturing appointment at the Cardiff College of Technology and Commerce he took his Master's degree under Dr. H. 13. Watson. In 1956 Mr.Thoinas was appointed Lecturer at tlie South East Essex Technical College (now the Barking Regional College level at the Newport and Monmouthshire College of 'Technology in 1958 and at the Welsh College of Advanced Technology (now U.kV.1.S.T.) in 1961. In his approach to teaching Mr. Thomas aims at presenting chemical knowledge through its application to practical areas of daily life and work. In this respect lie is a ltcen advocate of sandwich courses and of the presentation of analytical cheniistrjr as a major brancfi of Chemistry in both teaching and research. He has pioneered courses for the Certificate of Supplementary Study (with the view to L.R.I.C.) in an;zlytical clieniisti-y at Barking and in South Wales and has arranged for a strong emphasis on analytical cliemistry in undergraduate curricula at U.W.I.S.T. He has organised several post-graduate short courses on subjects in analytical chemistry. Mr. Thomas represents the Royal Institute of Chemistry on the Science Advisory Panel of the Welsh Joint Education Committee and is the autlior or co-author of over 40 scientific papers and of 2 books. His curent research interests include ion exchange ion-selective electrodes and cationic halo2en chemistry. For hobbies motoring carpentry home decorating and gardening take pride of pIace. Mr. Thomas is married and has three daughters. He takes part in a wide range of cornmunity activities and is assistant secretary of the Tabernacle Welsli Eaptist Church Cardiff. of Technology) to be followed by appointments at Senior Lecturer ~ ~ ~ ~~

ISSN:0037-9697    

DOI:10.1039/SA9690600105

出版商:RSC    

年代:1969

数据来源: RSC

摘要:

CHROMATOGRAPHY Chromatography The following are summaries of some of the papers presented at a Joint Meeting of the Scottish Section and the Chromatography and Electrophoresis Group held on April 25th 1969 and reported in the May issue of Proceedings (p. 7 7 ) . Non-aqueous Ion Exchange of Weak Organic Acids BY J. D. R. THOMAS (Chemistvy Department Univevsity of Wales Institute of Scicncc and Technology Cavdif CF2 5LN Wales) WATER is by no means the only solvent from which ion exchange can take place; as long as ions are present ion exchange can be expected to occur. There are several liquids with high dielectric constants in which electrolytes can dissolve and dissociate and in which most of the common ion exchangers are stable. Many organic compounds are sufficiently ionisable when dissolved in such liquids to permit ion-exchange sorption by strongly basic or strongly acidic ion-exchange resins as appropriate.These liquids frequently have the facility of overcoming the insolubility limitations often encountered with organic compounds in purely aqueous systems. Methanolic media have proved useful for the ion-exchange separation of weak organic acids With phenols as an example elution with amine - acetic acid buffer solutions in July 19691 CHROMATOGRAPHY 109 methanol gives an ion-exchange separation pattern parallel to the aqueous pKa values of the weakly acidic phenols. This is illustrated by a scheme described by Logiel for the isolation of crude 2,4-dichlorophenol. In this the sample was dissolved in 0.2 per cent. v/v triethyl- amine in methanol (pH = 9.2 as measured by pH meter) and loaded on to a column of DeAcidite FF (acetate form) ion-exchange resin.Elution with a solution containing 200 ml of 0-2 per cent. v/v triethylamine acetate in methanol per litre of 0.2 per cent. v/v triethyl- amine in methanol (pH 8.6) released 9-chlorophenol (PKa = 9-38) while elution with 0.2 per cent. v/v triethylamine acetate in methanol (pH = 8.0) released 2,4-dichlorophenol (pKa = 7.51). The more strongly acidic 2,6-dichlorophenol (PKa = 6-79) and 2,4,6-trichloro- phenol (pKa = 6.41) were released on elution with 0-2 per cent. v/v acetic acid in methanol (pH = 3.5) and 5 per cent. v/v acetic acid in methanol respectively. As an alternative to using amine - acetic acid buffer systems Skelly2 effected the same separation by using a longer column of an equivalent resin Dowex 2 in conjunction with gradient elution.In this procedure the phenolic mixture was sorbed on the column from methanolic solution and the gradient elution effected by replenishing a reservoir of eluent initially composed of methanol with 0.2 per cent. v/v acetic acid in methanol. The elution order was ~3-chlorophenol ; 2,4-dichlorophenol; and 2,6-dichlorophenol. A final elution with 5 per cent. v/v acetic acid in methanol released 2,4,6-trichlorophenoI. When the pKa values of the phenols are very close the separation problem is much more intricate and fixed concentration elution is ruled out because of the amount of experimentation required. However with a rigorous combination of the use of amine - acetic acid buffer solutions in methanol and gradient elution it is possible to separate phenols of closely similar PKa.Thus after loading a column of DeAcidite FF (acetate form) with a mixture of wz- o- and $-nitrophenols in 4 per cent. v/v triethylamine in methanol resolution is obtained by a gradient-elution procedure involving replenishment of a reservoir of 4 per cent. v/v of M triethylamine acetate in methanol together with 80 ml of M triethylamine in methanol and 10 ml of acetic acid per litre. The first phenol to be released is wz-nitrophenol (pK = 8.39) followed by o-nitrophenol (pKa = 7-22) and $-nitrophenol (pKa = 7.15). The above principles of ion-exchange separation of weakly acidic systems can be extended to the very weakly acidic cresols (pKa = 10.10 to 10.33) and xylenols (PKa = 10.20 to 10.62) although the buffer systems must now include the more basic diethylamine instead of tri- ethylamine.The medium has to be very basic for the xylenols to be sorbed by the DeAcidite FF resin and for this reason a PKa of about 10.5 is considered to represent the limit to which the method of inducing ionisation by amines in methanol can be pushed in practice. Sorption by ion-exchange resins from non-aqueous media clearly provides a valid separa- tion dimension. Apart from the strict ion-exchange mechanism which is probably charac- teristic of the above separations this can be brought about by a physical mechanism through the sorption facilities offered by the polar sites on the resin phase. Such sorption need not be dependent on an ionising mediuni and in this respect the extraction and recovery in four separate fractions of naphthenic acids alkylphenols pyrrolic compounds and nitrogen bases from non-ionising petroleum products with macroporous ion-exchange resins are worth n ~ t i n g .~ The availability of macroreticular resins with their large pores of up to 1000 A diameter and of oleophilic resins capable of appreciable swelling in most organic solvents permits a confident prediction favouring a spectacular extension of separations with ion-exchange resins in a much wider range of polar and non-polar media. REFERENCES 1. Logie D. Analyst 1957 82 570. 2. Skelly N. E. Analyt. Chew. 1961 33 271. 3. Webster P. V. Wilson J. N. and Franks M. C. Analytica Chiw. Acta 1967,38 193. Molecular-sieve Chromatography BY D. M. W. ANDERSON MOLECULAR-SIEVE chromatography must now be regarded as an important analytical tech- nique broadly applicable to both organic and inorganic materials of any molecular weight.(Chemistvy Defiavtment The Univevsity Edinburgh EI-19 3 J J ) 110 CHROMATOGRAPHY [Proc. SOC. Analyt. Chew. Several factors may have contributed to the slowness of analytical chemists in general to appreciate the potential of this development in chromatography. First of all the early developments and applications involved biopolymers and the results were not published in the recognised analytical journals indeed even today a major difficulty in this field is data retrieval from a vast range of uncommon journals. In the speaker’s opinion a second factor involved the introduction in 1959 of the inappropriate term “gel filtration.’’ The technique is not restricted to the use of gels and it is not as normally used a “filtration” process.I t is clearly a form of column (or thin-layer) chromatography a suitable porous support material with pores of a size appropriate for the separation to be achieved gives a column whose effective path-length is short for large molecules and long for small molecules. All the well- known tricks and general experimental principles applicable in all branches of chromato- graphy must be applied when the optimum combination of parameters for a particular separation must be found. When the imprecise nature of the term “gel filtration” was realised several alternative terms such as “exclusion chromatography,” “gel (permeation) chromatography” and “steric chromatography,” were introduced. No other analytical technique has ever been known by such a perplexing variety of names particularly when some authors indicated (whether intentionally or not is immaterial) that a new technique was implied by the alternative name proposed.In the past 6 months there has been however a noticeable swing towards the term “molecular-sieve chromatography,” first proposed in 1962. This term does not in any way restrict the technique to the use of the classical zeolite type molecular-sieves porous silica ceramics and glasses ; cross-linked poly- glucans (dextran gels starches and celluloses) ; agar and agarose gels; and cross-linked poly- acrylamide polymethacrylate and polystyrene preparations are all currently in use. Some of these supports are hydrophilic some hydrophobic ; some of the hydrophilic molecular- sieves can be converted into hydrophobic types by chemical modification and vice versa.Aqueous systems and a wide range of organic solvents can therefore be used as eluents. Quantitative results can be obtained if the chromatographic columns can be calibrated in terms of valid adequately characterised standards. A wide range of these is available commercially for work with proteins polystyrenes and dextrans. Proteins are not acceptable standards for say polysaccharides and vice versa; but for reasons that are obscure neutral highly branched dextrans (polymers of glucose) serve as useful standards for work with com- pletely different types of polysaccharide e.g. acidic polymers based on sugars other than glucose. The experimental results can be plotted graphically in many ways; a recent innova- tion has been to plot a function (M x log [TI) of the hydrodynamic volume against the elution volume and this is claimed to give a “universal calibration” that appears to hold for a wide variety of substances.Many papers dealing with theoretical aspects of the separation process have been pub- lished in the last 6 months. I t is now generally agreed that very few separations on mole- cular-sieves depend solely on separations by molecular weight size or shape ; the simple differential column-length model is an over-simplification. Other factors such as adsorption charge transfer and 7 ~ - and H-bonding are also frequently involved and elution may not necessarily be in the order of decreasing molecular size i.e. the largest molecules are not invariably eluted first. As new molecular-sieves become available it is important that their performance be assessed for each specific purpose.There are no universal rules; the best sieve for one parti- cular separation will not be the best for all others. The position is already complicated by the fact that two different types of porous glass differing in their chromatographic characteristics are at present offered commercially and a similar situation also exists for agarose gels; the “bead-gelled” products differ in performance (in some ways advantageously and vice versa) from the “granules” obtained by physical disintegration of a gel. At present molecular- sieves are available for all molecular weights up to 150 x lo6 (the present upper limit for agarose gels). The rigid type molecular-sieves clearly have several advantages over gels and future advances appear to lie with the former. Although this chromatographic technique is already in use for a vast range of materials there is still great scope for its development in all branches of analytical chemistry. For a time it was all most confusing.

ISSN:0037-9697    

DOI:10.1039/SA9690600108

出版商:RSC    

年代:1969

数据来源: RSC

摘要:

111 July 19691 REPORT OF THE ANALYTICAL METHODS COMMITTEE Report of the Analytical Methods Committee 1968 THIS thirteenth Report of the Analytical Methods Committee of the Society for Analytical Chemistry reviews the progress of work during 1968. Chairman D. C. Garratt Ph.D. TI.%. Hon.M.P.S. M.Chem.A. F.K.I.C. (Scienti$c Adviser Phavmar-eutical Society of Gveat Britain) E. Bishop B.Sc. A.K.C.S.T. F.R.1.C. I<. 13. Capper B.Pharrn. €’h.D. D.I.C. V.P.S. I,. E. Coles R.Pharm. I’h.D. F.P.S. F.R.I.C. J. H. Hamence O.B.E. M.Sc. Ph.D. M.Chem.A. N. W. Hanson B.Sc. Ph.D. F.R.T.C. F.R.I.C. M.Ph.A. M.Chem.A. F.R. L.C. A. G. Hill F.R.I.C. C. A. Johnson B.Sc. H.Pharm. F.P.S. F.K. I.C. A. G. Jones R.Sc. F.K.I.C. M.Ph.R. U. T. Lewis C.R. Ph.D. I).Sc. F.R.I.C. G. W. C. Milner D.Sc. A.Tnst.P. F.R.T.C.K. 1;. Milton B.Sc. Ph.D. M.I.Biol. F.K.T.C. W. H. C. Shaw F.P.S. F.K.I.C. M.Chem.A. S. G. E. Stevens B.Sc. M.Chem.A. F.R.I.C. C. Whalley B.Sc. F.K.I.C. Univevsity of Exetev (Keadev in Analytical Chemistvy ) Divectov Depavtment of Pharmaceutical Sciences Pharmaceutical Society of Gveat Britain Public Analyst Oficial Agvicultuval Analyst Glamovgan County Council Public Analyst Oficial Agvicultuval Analyst avld Consulting Chemist Sndustvial Chemist Research and Development Depavtment Impevial Chemical Industvies Ltd. Chief Analyst R.D.H. Chemicals Ltd. Scienti$c Divectov Bvitish Phavmacopoeia Com- Chief A nalyst Jmpevial Chemical Tndustvies Ltd. Govevnment Chemist Ministvy of Technology Gvoup Leadev A.E.R.E. Havwell (Honovavy A aalyticnl and Consulting Biochemist Reseavch Analyst Glaxo Labovatovies Ltd.(Ho,novavy Secvefavy of the Society) Consulting Chemist Managev Staff and A dmin,istvation Heseavch Depavtment Laporte Industries Ltd. Geneva1 Chemicals Division mission Plastics Division (Pvesident of the Society) Tveasurev of the Society) K. A. Williams B.Sc. Ph.D. A.Inst.P. M.Inst.I’et. \V. J . Williams B.Sc. Ph.D. A.R.l.C. P. (‘. Young M.A. D.Phil. M. L.Chem.E. Analytical and Consulting Chemist Lecturer Bath Univevsity of Technology Group Manager Rvitish Standavds Institution M.Chem.A. F.R.I.C. A .F.R.Ae.S. Secretary P. W. Shallis GENERAL REVIEW The Committee extends its grateful thanks to two members Dr. S. G. Burgess and Mr. E. Q. Laws who resigned during the year coincident with their retirement from professional employment. It is with pleasure that the Committee acknowledges the continuing association of Mr.Laws with its activities through his Chairmanship of the Particle Size Analysis Sub- Committee. Two new members were welcomed in April when Council appointed Dr. W. J. Williams and Dr. P. C. Young to membership of the Committee. The appointment of Dr. Young of the British Standards Institution ensures close liaison with this body in respect of the agreement made in 1967 whereby the B.S.1. refers to the Analytical Methods Committee any requirements it may have associated with general methods of analysis. PROGRESS OF WORK- A year of steady progress in much of the work currently being undertaken can be reported. Four separate Reports from Sub-Committees and one from a Panel of the Joint Committee with the Pharmaceutical Society were published in The Analyst during the year.This latter Report on “The Chemical Assay of Cascara Dry Extract Cascara Tablets and Cascara Bark,” is particularly noteworthy as it is the first standardised chemical method of assay for cascara preparations to be proposed. 112 REPORT OF THE ANALYTICAL METHODS COMMITTEE [P?’OC. S O C . AYtaZyt. C/ZeWL. The Particle Size Analysis Sub-Committee was formed in 1961 to study methods of particle size analysis and to survey and evaluate available instruments. From the beginning the Sub-committee decided to handle its work in 3 distinct stages. The first stage was to collect information relevant to particle sizing and the available instruments and to cIassify the many methods with regard to the principles involved. This stage was completed when in March 1963 the Sub-committee’s “Classification of Methods for Determining Particle Size” was published in The Analyst.The preparation of critical reviews of the various apparatus and techniques that had been included in the published “Classification” forms the second stage of the work and the first significant step towards reaching this objective was taken in September with the publication of “The Determination of Particle Size. I. A Critical Review of Sedimentation Methods.” This booklet is the result of more than 2 years’ work and in its preparation the experience of the members of the Sub-committee with regard to sedimentation methods has been fully utilised. In the few instances when no member had experience of a particular sedimentation technique experts from outside the Sub-committee were consulted and the Committee would like formally to record its gratitude to these workers for the assistance they have rendered.Sales of this booklet have been particularly good and this is heartening to the members of the Sub-committee who are currently engaged in prepar- ing further reviews covering other techniques and apparatus. The third stage of the work is the evaluation of instruments and techniques by means of collaborative experiments. Some work on these lines has already been undertaken but difficulties have been encountered particularly in respect of laying down precisely standardised conditions for the test and for sampling and in the provision of a satisfactory sample for analysis. Further work that it is hoped will overcome these problems is in hand.In March 1963 the first edition of the Committee’s collection of standardised methods of analysis was published under the title “Official Standardised and Recommended Methods of Analysis.” Such has been the demand for this book that early in 1968 it became out of print. The “Supplement” to the first edition that was published in 1967 although replacing the “Bibliography of Official Standardised and Recommended Methods of Analysis” con- tained in the first edition contains only those of the Committee’s standardised methods published since 1963. In consequence the Committee has considered the preparation of a second edition of the work and it has been decided that a publication date of autumn 1972 shall be aimed for. The Committee is pleased to announce that Mr. S. C. Jolly has again undertaken to compile and edit the book.A glance at the literature of analytical chemistry shows the state of improvement in both technique and instrumentation that is constantly being proposed and for this reason the Committee is aware that some of its standardised methods especially those published many years ago may no longer be the best that could be recommended. In consequence all the methods in the first edition are being reviewed and for this purpose expert Assessors have been appointed to advise the Committee on the con- tinuing suitability of the methods or to suggest revisions or replacement of the methods when appropriate. At the end of the year the recommendations of some of the Assessors were available and from these it was apparent that some methods should be replaced and that some additional work would be needed before the incorporation of new recommendations in the second edition.The Fertilisers and Feeding Stuffs Regulations 1968 which came into operation in July contain the methods of analysis recommended in 1963 by the Additives in Animal Feeds Sub-committee and more recently by the Prophylactics in Animal Feeds Sub-committee. This latter Sub-Committee’s Report on “The Determination of Furazolidone in Feeds” was published in the June issue of The Azalyst and work is still continuing on methods of analysis for other prophylactic drugs contained in the Regulations for which no recommendations have yet been made. Instrumental methods of analysis are constantly under consideration by this Sub-committee and work was completed during the year that will lead to the recommen- dation of a polarographic method for the determination of dimetridazole.Spectrofluorimetry is also under consideration as the only method so far found for determining some drugs that have recently been accepted for use under the Veterinary Products Registration Scheme. It is hoped however that some satisfactory alternative method will be found as few labora- tories have the facilities for spectrofluorimetric analysis. The Compound Animal Feeding Stuff!; Manufacturers National Association Ltd. which is directly represented on the Sub- committee has requested that recoveries of drugs from pelleted and other modified feeds July 19691 REPORT OF THE ANALYTICAL METHODS COMMITTEE 113 should be investigated by the recommended methods as treatment of the feed after medica- tion has in some instances been known to affect adversely the recoverability of the drug.The Sub-Committee however suggested that in view of the many difficulties met during investigations of those methods of analysis problems associated with feeds treated after medication should be investigated by the feedingstuff s industry. In consequence the industry is to arrange collaborative work on pelleted feeds and will make the results available for incorporation in the published Reports with or without comment by the Sub-committee. Two Reports from the Meat Products Sub-Committee were published in the July issue of The Analyst. These were “Nitrogen Factor for Blood” and “Nitrogen Factor for Barley” and recornmended average figures for use in the analysis of black pudding.The Sub- Committee’s work on mutton and lamb is not yet complete but it is hoped that a reliable average factor can be recommended in the coming year. The desirability of an analytical method for the determination of connective tissue in meat products has come under considera- tion and the Sub-Committee has concluded that this would warrant a full-time research project. The Fish Products Sub- Committee has in the absence of success in the development of a method for determining fish content by way of the isolation and measurement of fish fibres continued with tlie collection of analytical results for the nitrogen content of coalfish. Gas - liquid chromatography is a technique that has occupied the Essential Oils Sub- Committee during the year. The application of this technique to the determination of various constituents of essential oils has shown that in many instances this method can provide more reliable results than are obtained by the classical methods.The preparation of Reports for publication on the determination of cineole in cineole-containing oils and of cedrol in Cedar- wood oil is under consideration. The Metallic Impurities in Organic Matter Sub-committee is also currently investigating some instrumental methods. Atomic-absorption spectrometry and polarography are both of undoubted value in determining small amounts of certain metals and these possibilities are being explored. This Sub-committee’s final Report on tin under the title “The Determination of Small Amounts of Tin in Organic Matter. Part 11. Amounts of Tin from 30 to 150 pg” appeared in the June issue of The Analyst.Of the elements not yet dealt with in Reports from the Sub-committee work on cadmium and selenium is currently in hand. The Fluorine Sub-Committee has been encouraged by the results of some of its investiga- tions in 1968. The group investigating the determination of microgram amounts of fluorine in the final solution has been examining the alizarin fluorine blue niethod in a succinate buffered solution and the results have been very promising. A method for improving the end-point in thorium nitrate titrations of up to 10 mg of fluoride was published by Selig (Analyst 1968 93 118) and has been investigated by the group dealing with milligram amounts of fluorine in the final solution. The members are in general subjectively satisfied that the author’s claim is justified and further work which it is hoped may lead to the recom- mendation of this method is in liand.Three of the Panels of the Joint Committee with the Pharmaceutical Society completed their programmes of work during the year. Panel 3 (Anthrayuinone Drugs) was set up in 1056 to recommend chemical methods of assaying the important antliraquinone drugs and their preparations. Work was begun first on senna both leaf and pod and methods were published in a Report in The ANalyst in 1965. The assay of aloes was considered next and the method recommended was published in 1967. An extension of this method to tlie assay of cascara bark and cascara preparations was then investigated and the Panel’s Report on “The Chemical Assay of Cascara Dry Extract Cascara Tablets and Cascara Bark’’ was published in the November issue of The Analyst.It is interesting to note that this method is recommended only for the bark and its dry preparations as for reasons not fully understood it proved to be unsuitable for liquid preparations. Panel 8 (Phenothiazine) completed its work on the development of a gas - liquid chroma- tographic method suitable for the assay of phenothiazine and some of its commercial prepara- tions. This Panel completed its work shortly before the gas-chromatographic method adopted by the A.O.A.C. was published. Subsequently the Panel has compared its own method with the A.O.A.C. method and has concluded that both methods give very similar results but it prefers its own method as the retention time of the dibutyl phthalate used as internal standard is considerably less than that of the promethazine hydrochloride used in the A.O.A.C.The An attempt to find support for such a project is in hand. 114 REPORT OF THE ANALYTICAL METHODS COMMITTEE [PYOC. S O C . Analyt. CheflZ. Panel's Keport is expected to be published in The Analyst by about the second half of 1969. Panel 9 (Thin-layer Chromatography of Corticosteroids) which had earlier devised an adsorption thin-layer system for limiting impurities in corticosteroids has continued with its efforts to improve on this system or to find a more satisfactory system. After a considerable amount of work exploring new approaches to the problems without any significant success the Panel has now concluded that in the absence of fundamental research there is little chance of any further progress being made.In consequence the work of the Panel has been terminated. The accuracy and precision of analytical procedures in the context of pharmaceutical analysis is the concern of Panel 10 which during the year carried out its first collaborative exercise. This work involved simple weighing dilution to volume measurement of volume with both burette and pipette and spectrophotometric measurement. Such has been the number of results submitted in this exercise that a fairly large computer processing project has had to be undertaken. I t is hoped however that the results will have been processed and a Report of the Panel's findings prepared before the end of 1969. The Joint Committee is currently considering other subjects on which Panel investigations could usefully be undertaken.Individual progress reports for all the Sub-Coimmittees and Panels together with their constitutions will be found on pp. 114 to 125. ANALYTICAL METHODS TRUST- Ihe number of organisations that gave donations to the Trust Fund during the year was 1 9 and the total amount received L1768 was approximately L700 more than in 1967. The Trustees have nevertheless had to face the fact that all the Deeds of Covenant entered into by various organisations as a result of the Appeal in 2960 had now terminated and in consequence income from direct donations would be considerably reduced in subseyuen t years. Inconie from the sale of publications was high in 1968 (L3580) but was not expected to continue at this level and revenue from this source together with interest on investments and bank deposits would not cover the annual expenditure.The Trustees therefore decided to appeal again to industry and this Appeal was launched in September. ISy the end of the year sufficient response had already been received to indicate that the Appeal would be successful. ,\ ANNUAL ACCOUNTS- The audited statement of accounts for the year ended October 31st 1968 is shown in Appendix I and a list of subscribers to the Trust Fund during the year is given in Appendix TI. REPORTS OF SUR-CONMITTEES 01; THE ANALYTICAL METHODS COMMITTEE ANALYTICAL STANDARDS SUR-COMMITTEE CONSTITUTION- E. Bishop D.Sc. A.R.C.S.T. F.R.I.C. (Chaavwan) I<. Archer B.Sc. P. R. W. Baker M.Sc. A.K.I.C. A. G. Hill F.R.I.C. E. J. McLauchlan M.Sc. A.R.T.C." K. G. Monk B.Sc. Ph.D. A.R.C.S. D.I.C.J. M. Skinner B.Sc. Ph.D. F.K.I.C. W. 1. Stephen E.Sc. Ph.D. F.R.I.C. J. T. Yardley B.Sc. F.R.I.C. P. W. Shallis (Secvetary) A.R.I.C.7 * Appointed December 1968 Uvlivevsity of Exetev (Depavtment of ChemzsZvy) Lapovte Titantum L t d . Wellcomc Reseavch I-abovatovies B. D. 13. Chemtcals Ltd. National Physical Labovatovy 7J. K.A .E.A . Atomac Weapons Rescavch Estah- Impevial Chemical Industvies Ltd. ( AgrtLdtuval linavevsaty of Hivvuzingham (DPpavtmed of Hopkin & Williams Ltd. lishment Davisaon) Chemastvy) t Appointed September 1968 TERMS OF REFERENCE-"TO examine existing analytical standards and to select suitable substances." July 19691 REPORT OF THE ANALYTICAL METHODS COMMITTEE 115 The year has been one of considerable activity for the Sub-committee and has been notable for the setting up of a separate Panel of members to allow more than one investigation to be carried out concurrently.As mentioned in the Report of the Analytical Methods Committee for 1967 a request has been received from I.U.P.A.C. for an investigation to be carried out on compleximetric standards. This request was referred to the Sub-committee and it was decided not to disrupt the planned programme of work by giving priority to the proposed investigation. It was however felt that considerable importance should be attached to the request from I.U.P.A.C. particularly as no authoritative recommendations of standards for use in conipleximetry existed. In consequence the Sub-Committee decided to set up a Panel including some of its members supplemented by other workers with a specialist interest in compleximetry.This Panel held its first meeting in December and full details are given below. Early in the year the Sub-corninittee learned to its satisfaction that the Report on “Sulphamic Acid as a Primary Standard in Acid - Base Titrimetry” had been adopted by 1.U.P.A .C. and would be published in Pare and Applied Chemistry as an official recommendation together with the Report on “Sodium Carbonate as a Primary Standard in Acid-Rase Titri- metry,” tlie adoption of which had been notified earlier. The Sub-Committee has sub- sequently been informed that the two Reports are to be combined for re-publication. A t the request of I.U.P.A.C. the lines of communication between the Sub-Committee and Commission V3 of the Analytical Chemistry Division of I.U.P.A.C. have been strengthened by the appoint- ment of Dr.W. I. Stephen as the official representative of the Commission serving on the Sub-Committee ; a reciprocal arrangement has also been agreed to. Work has continued during the year in an attempt to classify other existing acid - base standards that are commercially available. Three acid salts have been under investigation- sodium hydrogen diglycollate potassium hydrogen phthalate and potassium bi-iodate. The procedure previously used for the assay of sulphamic acid was adapted for this purpose but so poor were the potentiometric titration curves for sodium hydrogen diglycollate and potas- sium hydrogen phthalate that it was concluded that they could not be assayed accurately and could therefore not be recommended nor classified within the Sub-committee’s published scheme.On the other hand tlie titration curve for potassium bi-iodate was particularly good but the stoiclieiometry of this substance is in doubt. It has been found that a single recry- stallisation of the analytical-reagent grade salt produces a material that can probably be classified as class E but further recrystallisation disturbs the balance of the salt which is produced by the half neutralisation of iodic acid. The presence of chloride in the inaterial from one conimercial supplier had been discovered and an investigation of the chloride content of the material from another source and manufactured by a different process is in hand in an attempt to discover whether or not the presence of chloride can have any effect on the stoicheiometry of the compound.Several other proposed acidimetric standards including hydrazine sulphate sodium tetraborate 4-aminopyridine and tris(hydroxymet’ny1)aiilino- methane have still to be considered. I’IIOGRESS OF WORK- COMPLEXIMETRIC STANDARDS PANEL CONSTITIJTION- E. Bishop B.Sc. A.R.C.S.T. F.R.I.C. (Chaivman) H. Bennett R.Sc. A.R.I.C. A. G. Hill F.R.I.C. R. G. Monk B.Sc. Ph.D. A.R.C.S. D.I.C. U.K.A.E.A. Atomic Weapons Research Esta- Univevsity of Exetev (Defiuvtmcnt of Chemistvy) British Cevamic Keseavch Association B.D.H. Chemicals L t d . A.R.I.C. blishment E. J. Newman R.Sc. Ph.D. F.R.I.C. W. I. Stephen ESc. Ph.D. F.K.I.C. W. J. Williams B.Sc. Ph.D. A.R.I.C. C. Woodward HSc. Ph.D. Hopkin G. Williams Ltd. Univevsity of Birmingham (Department of Bath Univevsity of Technology Imfievial Chemical Iwdustvies Ltd.(Agvicznltuval Chemistry) Division) P. W. Shallis (Secvetavy) 116 REPORT OF THE ANALYTICAL METHODS COMMITTEE [PYOC. S O C . AnaZyt. Cheuvt. PROGRESS OF WORK- The Panel held its first meeting in December and decided unanimously that work aimed at recommending standard substances for use in compleximetry should be carried out. As a preliminary step information relating to the more useful metals oxides and salts that have been recommended as standards is being collected. ESSENTIAL OILS SUB-COMMITTEE CONSTITUTION- G. W. Ferguson BSc. Ph.D. F.R.I.C. J. A. Bailey B.Sc. A.R.I.C. I<. Field M.Sc. Ph.D. J. H. Greaves B.Sc. F.R.I.C. A. M. Humphrey* B. n. Masters L.R.1.C.t W. S. A. Matthews A.R.I.C. Miss H. M. Perry M.Sc. M.Chem.A. F.R.1.C.t J . Ridlington B.Sc. A.R.I.C.J. H. Seager M.Sc. F.R.I.C. B. I). Sully B.Sc. Ph.D. A.R.C.S. F.R.I.C. G. Watson B.Sc. F.R.I.C. P. W. Shallis (Secretary) (C haivman) * Appointed May 1968. Resigned June 1968. Analytical and Coizsulting Chemist Rowntree & Co. Ltd. Ministry of Technology Laboratory of the Pyoprietary Per f umes Ltd. Rush Boake Allen Ltd. Bush Boake Allen Ltd. Ministry of Overseas Develo$ment Tropical Products Institute Bush Boake Allen Ltd. I.F.F. (Great Britain) Ltd. Yardley & Co. Ltd. Bush Boake Allen Ltd. Cocker Chemical Co. Ltd. Government Chemist t Resigned May 1968. TERMS OF REFEKENCE-(‘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- The gas - liquid chromatographic determination of constituents of essential oils has occupied the Sub-Committee’s attention for the whole year.Work on the determination of cineole in oils of cedrol in Cedarwood oil and of geraniol in Citronella oil have all been investigated. The Sub-committee has also acquired a considerable knowledge of the applica- tion of gas - liquid chromatography to the analysis of essential oils which it is hoped will be incorporated in a report for publication. The results for the determination of the cineole content of oils in which it is only a minor constituent have shown remarkably good inter-laboratory agreement considerably better than would be expected by the accepted o-cresol method. Some work is now to be undertaken to discover whether the method is equally suitable for oils having a high cineole content.FISH PRODUCTS SUB-COMMITTEE CONSTITUTION- S. M. Herschdoerfer Ph.D. F.R.I.C. F.I.F.S.T. M.R. S.H. (Chairman) G. H. 0. Burgess RSc. Ph.D. S.Z.S.* J. H.Bushill,D.Sc. F.R.I.C. F.R.S.H. C. B. Casson B.Sc. F.R.I.C. W. T. Little B.Sc. Ph.D. 1. A. Lovern Ph.D. D.Sc. F.R.S.E. F.R.I.C. T. McLachlan D.C.M. A.C.G.F.C. M.I.Biol. M.Chem.A. F.R.I.C. F.I.F.S.T. F.R.S.H. D. J. Ward F.R.I.C. F.I.F.S.T. R. E. Weston B.Sc. M.Chem.A. F.R.I.C. M. L. Windsor Ph.D. A.R.1.C.t P. W. Shallis (Secretary) * Resigned October 1968. T. Wall & Sons (Ice Cream) Ltd. Ministry of Technology Torry Research Station Formerly J . Lyons G. Co. Ltd. J . Lyons & Co. Ltd. Unzlever Research Laboratory (Colzvorth) Ministry of Technology Torry Hesearch Statio n Public Analyst Birds Eye Foods Ltd.Ministry of Technology Labovatory of the Ministry of Technology Humber Laboratory Government Chemist t Appointed April 1968. July 19691 REPORT OF THE ANALYTICAL METHODS COMMITTEE 117 TERMS OF REFERENCE-"(&) To establish the essential characteristics of fish and differences in those characteristics caused by decomposition or other changes. (b) 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- As attempts to find an alternative method for determining the fish content of food products by means of the separation and measurement of fish fibres proved to be unsuccessful the Sub-committee has had to continue with the determination of protein arrived at by means of a total nitrogen determination as a basis for the determination of fish content.In the Sub-Committee's earlier investigation of cod it was found necessary to collect figures for nitro- gen content for more than 12 months in order to establish whether or not there were seasonal variations. Coalfish has been chosen as the next species for investigation and figures for the nitrogen content of this fish have been collected throughout the year. Attempts to reduce to an acceptable level the blank values obtained in a method for determining milk protein added as milk powder in fish products by means of a determination of phosphoprotein have proved unsuccessful. A satisfactory method for determining milk protein is still being sought. The Sub-committee has been kept informed of the development at the Torry Research Station of an electrophoretic method for identifying fish species which is applicable to both raw and cooked fish provided that it has not been pressure cooked or canned.A member of the Sub-committee has collaborated in attempts to adapt this method to the quantitative determination of the fish but it is now considered that success is unlikely. FLUORINE SUB-COMMITTEE CONSTITUTION- T. K. F. W. Fennell H.A. (Chaivman) R. Belcher Ph.D. D.Sc. F.K.I.C. F.Inst.F.* E. J. Dixon B.Sc. Ph.D. A.K.I.C.7 H. A. Foner B.Sc. A.K.I.C." J. I(. Foreman B.Sc. F.K.I.C. G. S. Goff H. Green L.K.I.C. R. J- Hall F.I.M.L.T. W. C. Hanson F.K.I.C. K. F.Milton B.Sc. Ph.D.,M.I.Biol. F.K.I.C. E. J. Newman B.Sc. Ph.D. F.R.I.C. J. M. Skinner B.Sc. Ph.I). F.R.I.C. R. Waspe B.Sc.* C.A. Watsonf J. E. Whitley B.Sc. Ph.L).* P. W. Shallis (Servetavy) * Corresponding member. 7 Resigned Novembcr 1968. Appointed May 1968. Miwistvy o/ Technology Hoyal Aivcvaft Esta- Univevsity qf Bivmingham (Professov of A n a l y - Ministvy of Technology Labovatovy of the Geological Suvvey of Isvael Ministry of Technology .Labovatovy of the Govevnment Chemist Lincoln Electric Co. Ltd. British Cast Ivon Research Association Ministry of Agvicultuve Fishevies and Food National Agvicultuval A dvisovy Sevvice Fisons Fevfilisevs Ltd. Analytical and Consulting Biochemist Hopkin & Williams Ltd. Imperial Chemical fndustvies L t d . (Agricultural Formerly Laporte Acids Ltd. Hopkin t ! Williams Ltd. Scottish Reseavch Reactov Centve blishment tical Chemistvy) Govevnment Chemist Division) 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." PROGKESS OF WORK- final determination of fluorine in solution.The work of the Sub-Committee has continued during the year to be concentrated on the Later when satisfactory methods have been 118 REPORT OF THE ANALYTICAL METHODS COMMITTEE [PYOC. SOC. AYzalyt. Chem. found the separation and recovery of fluorine for determination will be dealt with. The two groups of the Sub-committee one dealing with microgram amounts and the other with milligram amounts of fluorine in the final solution can both report some measure of success. The Group dealing with microgram amounts of fluorine in the final solution had earlier concluded that a method based on zirconium and solochrome cyanine R was too variable to be recommended immediately as a standardised method.Subsequently the use of alizarin fluorine blue with both acetate and succinate buffer has been investigated. The results with succinate buffer have been found to be more reproducible than those with acetate buffer and further collaborative work which it is hoped will prove the suitability of this method for recommendation is now in hand by the succinate buffer method. The thorium nitrate titration niethod has occupied the attention of the group dealing with milligram amounts of fluorine for most of the year. The conditions published by Selig (A~zalyst 1968 93 118) are under investigation. Sehg claims that by carrying out the titra- tion in a solution buffered with glycine - perchlorate at pH 3-35 and with methyltliymol blue as indicator the end-point is considerably sharper than those obtained with any other indicator previously recommended for this titration.From the work so far carried out several mem- bers of the group would support this contention. A potentiometric titration method is also being investigated. A critical review of radiometric methods for determining fluoride prepared by Mr. J. K. Foreman at the request of the Sub-committee has been accepted for publication in The Aiaalyst. Further work is in hand. MEAT PROIITJCTS SUF-COMMITTEE CONSTITUTION- S. M. Herschdocrfer Ph.D. F.R.I.C. F.T.€:.S.T. S. Back H.Sc. M.Chem.A. F.1I.I.C.” W. €3. Chapman B.Sc. M.Chem.h. F.K.1.C.t 1’. 0. Iknnis R.Sc.F.R.T.C. H. C. Hornsey F.R.I.C. A. J. Kidney R.Sc. Ph.D. A.R.C.S. A.K.I.C. K. A. Lawrie Ph.D. D.Sc. F.K.I.C. F.I.F.S.T. T. McLachlan D.C.M. A.C.G.F.C. M.T.Biol. M.Chem.A. F.K.I.C. F.T.F.S.T. F.K.S.H. A. McM. Taylor R.Sc. Ph.D. F.R.1.C. G. Wslley H.Sc. F.R.I.C. R. E. Weston R.Sc. M.Chem.A. F.R.I.C. F. K. S . H . ( Ch aivvna.l.2) E. I;. Williams O.B.E. M.A. F.R.I.C. P. W. Shallis (Secvetavy) * Resigned March 1968. T . WaM & Sons (Ice Cream) I<td. The Nestle‘ Co. L t d . Gveatev Lovzdon Council 0x0 Ltd. -1. Saiuzsbwy L t d . T . Wall & Sons (Meat and Handy Fuods) I l d . liuzivevsity of Nottingham (Food Science T,abova- tovzes) Public A nalyst C. Shicpavn Ltd. Unilevev Ltd. Ministvy of Technology Lahovatovy of the J . Sainsbury Ltd. Govevnment Chemist t Appointed October 1968.TERMS OF REFERENCE--"(^) The determination of the meat content of products containing meat; (b) the determination of the constituents of meat and meat products.” NoTE-“The term ‘meat products’ to include hydrolysed protein.” PROGRESS OF WORK- Collation of all the figures for the nitrogen content of mutton and lamb collected by the Sub-Committee as a preliminary step towards preparing a Report for publication brought to light the fact that virtually all the results available applied only to lamb. As from the point of view of manufactured food products niutton is the more important of the two preparation of the Report has been delayed until sufficient figures for mutton have been collected to permit an average factor to be recommended. Reports from the Sub-committee on “Nitrogen Factor for Barley” and “Nitrogen Factor for Blood’’ appeared in the July issue of The Analyst.The Sub-committee has considered some of the problems posed by the new Regulations affecting certain types of meat products that come into effect in 1969. The Regulations affecting sausages lay down a minimum lean meat content and define lean meat as meat July 19691 KEPORT OF THE ANALYTICAL METHODS COMMITTEE I19 trimmed free from visible fat. All manufacturing joints do however contain intramuscular fat and it appears that some measure of the average percentage of intramuscular fat likely to be present will be needed so that due allowance for this can be made in ascertainins whether or not a product meets the legal requirements. The Sub-committee is collecting the results of analytical determinations of the fat content of “lean” meat with a view to deciding whether or not it is practical to recommend an average figure.The Regulations also pose the problem of the determination of rind and other connective tissue in meat products. There are currently no satisfactory methods for this purpose and the Sub-committee is of the opinion that a full- time research project will probably be needed. Various means by which this project could be set up are being explored. The investigation in one laboratory of a haemagglutination method by which it is claimed specific proteins in raw or cooked meats can be deterinined is still in progress. Towards the end of the year the Sub-committee began a consideration of standardised methods for the determination of moisture ash nitrogen chloride nitrite nitrate fat and creatine and creatinine in meat products which it is intended shall be ready for inclusion in the second edition of “Official Standardised and Recommended Rilethods of Analysis.” METALLIC IMPURITIES IN ORGANIC MATTER SUB-COMMITTEE CONSTITUTION- T,. E. Coles B.Pharm. Ph.D. F.P.S. F.R.I.C. W. Cassidy B.Sc.Tech. M.Cbem.A. F.R.1.C.” J . C. Gage I<.%. Ph.D. F.R.I.C. M.Ph. A. M.Chern.A. (Chairman) K. A. Hoodless R.Sc. Ph.D. Miss E. M. Johnson M.Sc. R.H.I.C. D. A. Lambie H.Sc. F.R.I.C. H. W. Liebmann Ur.Phil. F.R.I.C. K. F. Milton l’S.Sc. Ph.l>. M.I.Biol. F.1Z.I.C. E. J . Newman H.Sc. Ph.D. F.R.I.C. W. L. Shcppard M.Sc. F.K.1.C.t G. H. Thackray B.Sc. M.Chem.A. F.R.1.C. P. W. Shallis (Secretavy) * Appointed May 2968. Public AYzalyst and Oficzal Agvicznltizval Analyrt Deputy Public A.tzalyst Impevial Chemical Indutvies L t d .(I.izdustvin1 Hygiene Labovatovies) Ministvy of Technology Labovatovy oJ the Government Chemist Bvitish Food Manufactwing 1 vzdzzstvies I?eseavch A ssociation The RadioLhemical Centre Metal Box Co. Idd. Analytical and Consultzng Biochemist Hopkin & Wzlliams L t d . Unilevev L t d . Public Analyst 7 Appointed September 1968. TRIMS OF REFEIZENCE-“TO investigate the determination of small quantities of metals in organic matter.” PI~OGIESS OF WOKK- The Sub-committee has continued its work during the year on the determination of small amounts of cadmium in organic matter. A colorimetric method in which cadmium is determined as its red complex with dithizone a polarographic method and an atomic-absorp- tion method have all been investigated and found to be satisfactory.A Report for publication incorporating the recommendation of these three methods is to be prepared. A Report from the Sub-committee under the title “The Determination of Small Amounts of Tin in Organic Matter. Amounts of Tin from 30 to 150 pg” was published in the June issue of The Analyst and this completed the investigation of the determination of tin. It is an essential dietary element that in excess has been reported to cause abnormalities in sheep and cattle. A sensitive method is therefore required but unfortunately most of the established sensitive methods proposed involve the use of reagents that are considered to have carcino- genic properties and are no longer available. Some reagents proposed more recently- 2-mercapiobenzothiazole and 2-mercaptobenzoic acid-have however shown promise of providing adequately sensitive methods and work on these lines is being pursued.The publication by B.S.I. of ageneral procedure for the determination of arsenic with silver diethyl- dithiocarbamate is awaited before the Sub-committee decides upon the course of action it will follow to discover whether or not this method should replace the currently recommended molybdenum blue method. Part 11. Selenium is an element that has been under consideration during the year. 120 [E‘roc. SOC. Analyt. Chewz. Other methods previously published by the Sub-committee are also being reconsidered with a view to deciding on their continuing suitability. In particular the technique of atomic absorption is to be studied as it is felt that in several instances an alternative method to that already recommended could be proposed.REPORT OF THE ANALYTICAL METHODS COMMITTEE PARTICLE SIZE ANALYSIS SUB-COMMITTEE CONSTITUTION- E. Q. Laws BSc. F.R.I.C. (Chaivvnan) T. Allen M.Sc. Ph.D. R. de B. Ashworth M.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. H. Heywood Ph.D. D.Sc. A.C.G.I. M.I.Mech.E. J F. Hinsley F.I.M. F.1nst.P. R. Howes B.Sc. B. Scarlett M.Sc. Grad.1nst.P. J. P. Stuart B.Sc. Ph.D.* r). I. c . M.1.Chem.E. C. K. G. Treasure R.Sc. Grad.1nst.P. P. W. Shallis (Secretary) * Appointed October 1968. Formerly Ministvy of Technology Labovatory of University of Bradford Ministvy of Agvicultuve Fishevies and Food Plant PatJaology Laboratory British Ceramic Research A ssociation Paint Research Station the Government Chemist Glaxo Laboratories Ltd.“Shell” Reseavch Ltd. Loughborough University o j Tech nology Edgav Allen & Co. Ltd. Chestevfovd Pavk Reseavch Station Loughborough Univevsity of Technology Ministvy of Technology Wavven Spying Labora- Welwyn Hall Reseavch Association tory 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- It is with pleasure that the Sub-committee is able to report the publication in September of the first part of its projected critical review of techniques and apparatus used for particle size analysis.This booklet entitled “The Determination of Particle Size . I. A Critical Review of Sedimentation Methods” was compiled by the Sub-committee from the collective experience of its members and covers the first 30 methods contained in the “Classification of Methods for Determining Particle Size” published by the Sub-Committee in The AnaZyst in March 1963. For one or two methods however there was no member of the Sub-committee who had any first-hand knowledge and in consequence the assistance of experts was sought. The Sub-committee records its thanks to those persons who gave help in this way. Work is now in hand on the compilation of critical reviews covering other techniques and apparatus and in particular an appraisal of the Coulter Counter incorporating some 300 literature references is nearing completion.No collaborative tests of methods were arranged during the year owing to the thought- provoking nature of the results obtained in the first series of tests arranged. These tests involve the Andreasen pipette the Bostock sedimentation balance and the Coulter Counter. Wide variations in results were obtained and it has been concluded that procedural details were insufficiently defined and to some extent the silica powder sample used was unsuitable. A further exercise on a more limited scale is planned. The establishment of a bank of standard sized particles has been under consideration and has been discussed by the Sub-committee with other bodies. There is a considerable amount of enthusiasm for the idea in principle but the complexities of putting the idea into practice are realised to be enormous.The matter is however still being pursued. July 19691 REPORT OF THE ANALYTICAL METHODS COMMITTEE 121 PROPHYLACTICS IN ANIMAL CONSTITUTION- S. G. E. Stevens B.Sc. M.Chem.A. F.R.I.C. R. J. Anderson B.Sc. A.R.I.C. M. D. Beach B.Sc. F.R.LC.* A. G. Croft B.Sc. A.R.I.C. G. Drewery B.Sc. M.Chem.A. F.R.I.C. R. S. Hatfull F.R.I.C. M.Chem.A. F.R.S.H. S. Y. Hayes F.R.1.C.t J. S. Leahy M.A. A.R.I.C.; I. McLachlanS J. Markland B.Sc. M.Chem.A. F.R.I.C.7 D. H. Mitchell B.Sc. K. C. Spalding M.A. M.Chem.A. F.R.I.C.11 J. A. Stubbles KSc. C. B. Stuffins F.R.I.C. K. E. Weston B.Sc. M.Chem.A. F.R.I.C. (Chairman) D. R. Williams B.Sc. Ph.D. F.R.I.C. D. K. Wraige B.Sc. F.R.T.C. P. W. Shallis (Secretary) * Co-opted for work on organic arsenicals.t Representing t h e Compound Animal Feeding Stuffs Manufacturers National Association Ltd. $ Appointed October 1968. 3 Appointcd May 1968. 7 Appointed March 1968. FEEDS SUB-COMMITTEE Consulting Chemist Cooper Techvtical Bureau Lenvtig Chemicals Ltd. Spillers Ltd. Merck Sharp & Dohme I-td. Public Analyst Silcock & Levev Feeds Ltd. HuntivtgdoN Research Centre n o w Chemical Co. (U.K.) Ltd. Public Analyst Bur~.oughs Wellcome & Co. Public Analyst May 6. Bakev Ltd. J . Bibby 6 SONS Ltd. Ministry of Technology Laboratovy of the UNilevev Ltd. Research and Advisory Services Ltd. Government Chemist 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- The Ferti- lisers and Feeding Stuffs Regulations 1968 contain the Sub-committee methods for acinitra- zole amprolium nitrofurazone and sulphaquinoxaline.To these will be added methods for ethopabate and furazolidone the Sub-Committee’s recommendation for the latter having been published in the June issue of The A.tzaZyst. Work on dimetridazole for which a polaro- graphic method is to be recommended] and on zoalene for which the A.O.A.C. method is accepted has been completed; Reports for publication are in the course of preparation. A short Report has also been prepared for publication dealing with the determinations of amprolium ethopabate and sulphaquinoxaline when present together in proprietary formulations. Other drugs under consideration by the Sub-committee are carbarsone clopidol (meti- clorpindol) I decoquinate methyl benzoquate and statyl.The hydroxyquinolate drugs used in medicated feeds appear to be relatively unreactive in an analytical sense and the only satisfactory method so far proposed for their determination is a spectrophotofluorimetric one. The Sub-committee is loathe to recommend the use of such expensive equipment without further study and possible alternative procedures are under investigation. The Sub-committee is able to report considerable progress during the year. I22 REPORT OF THE ANALYTICAL METHODS COMMITTEE LProc. SOC. Analyt. Chem. PUBLICATIONS SUR-COMMITTEE CONSTITUTION- J). C. Garratt €?h.l>. D.Sc. Hon.M.P.S. M.Chem.A. F.H.I.C. (Chairman) J. 13. httrill M.A. F.R.I.C. J . H. Hamence M.Sc.Ph.’L>. M.Chem.R. S. G. E. Stevens B.Sc. M.Chem.A. F.R.I.C. S. C. Jolly B.Sc. B.Pharm. M.P.S. F.R.I.C. Chairman Analytical Methods Conzmzttee Editov The Analyst Membev Amzlytical Methods Committee F. K. I. C. Member A nalytical Methods Committee I?. K. I. C. Assistant Director Department of Pharmaceutical (Secretary and Editor) Sciences Phavmaceutical Society of Great Britain PROGRESS OF WORK- The first Edition of “Official Standardised and Recommended Methods of Analysis,’’ published in 1963 is out of print. The A.M.C. on the advice of the Sub-Committee has decided to publish a second Edition in the autumn of 1972 which will contain all the Society’s recommended methods of analysis and an up to date version of the bibliography of official standardised and recornmended methods of analysis.As many of the methods contained in the first Edition of the book were recommended several years ago the Sub-Committee has appointed Assessors to advise on whether these methods are still satisfactory or whether modification or replacement by a more modern method is desirable. Reports from some of the Assessors are currently being considered. Arrangements have been made for the compilation of most of the sections of the bibliography. REPORT OF THE P.S./S.A.C. JOINT COMMITTEE ON METHODS FOR THE EVALUATION OF DRUGS MAIN COMMITTEE T i . Ii Capper Ph.D. B.Pharm. F.P.S. U.I.C. J . IV. Fairbairn B.Sc. Ph.D. F. P.S. F.L.S. I). 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.T’harm. F.P.S. F.R.1.C W. Mitchell B.Sc. f.‘h.D. F.R.I.C.Hon.3l.P.S. R. F. Phipers B.Sc. Ph.I>. F.R.I.C. J. M. Kowson M.Sc. Ph.l>. F.P.S. F.L.S. K. Sinar B.Pharm. B.Sc. F.P.S. F.R.I.C. K. I,. Smith F.P.S. W. H. Stephenson F.P.S. D.B.A. F.R.I.C. S. G. E. Stevens B.Sc. M.Chem.A. F.R.T.C. A. F . Stott B.Sc. A.K.T.C. P. W. Shallis (Secretary) F.K.I.C. (Chairman) F.R.I.C. M.Chem.A. F.R.1 .C. M.Ph. A. F.R.I.C. M.Chem.A. M.Ph. A. Pharmaceutical Society of Gveat Britain Univevsity of London (Professor of Pharma- Chaivman Analytical Methods Committee of the Univevsity of London (School of Pharmacy) Bvitish Phavmacopoeia Comvnission cognosy ) S.A .c. Bush Boake Allen Ltd. Cooper Technical Bureau University of Bvadford (Professov of Phavmacy) Analytical and Consulting Chemist Boots Pure Drug Co. Ltd. Roots Pure Dvug Co. Ltd. Consulting Chemist Geigy (U.K.) Ltd.July 1969J REPORT OF THE ANALYTICAL METHODS COMMITTEE 123 TERMS 01; KEFEKENCE-"TO prepare standard methods for the evaluation of drugs their Preparations and of kindred materials." PROGRESS OF WOKK- Since the Joint Committee was formed in 1956 ten Panels have been set up to investigate the chemical assay of drugs or to study analytical techniques used in pharmaceutical analysis. In addition a Panel was convened to investigate the biological assay of senna specifically to assist in the interpretation of results obtained by the Panel considering the chemical assay of senna. Of these ten Panels only one is still active and all except one of tlie remaining nine achieved success in their investigations. Panel 3 (Anthraquinone Drugs) had added recommended methods for the assay of cascara dry extract cascara tablets and cascara bark to its previous recommendations relating to senna leaf and fruit and aloes.Panel 8 (Phenothiazine) is to recommend a gas - liquid chromatographic method for the assay of phenothiazine and Panel 9 investigating thin-layer chromatography as applied to the measurement of related steroid impurities in corticosteroids has concluded that within the present state of knowledge it is not able to improve on its system for assessing corticosteroid impurities that is incorporated in the current British Pharmacopoeia. The findings of Panel 10 investigating accuracy and precision in pharmaceutical analysis are awaited with interest. So many results have been submitted in the first collaborative exercise organised by the Panel that computer processing has had to be undertaken.Fuller details of tlie work of these Panels is given in the individual sections of this report. Tlie Joint Committee has continued to consider other possible subjects for Panel work and it is hoped that some new Panels will be set up in 1969. Three Panels completed their work during the year. PANEL 3 ANTHRAQUINONE DRUGS COKSTITUTION- J. M. Kowson M.Sc. Ph.D. F.P.S. F.L.S. C. Daglish B.Pharm. Ph.lI. M.C.T.C. F.P.S. J. \ I T . Fairbairn B.Sc. Ph.D. F.P.S. F.L.S. University of London (Professor of Phavuna- Miss H. M. Ferry M.Sc. M.Chem.A. F.R.I.C. H. A. Ryan B.Sc. F.R.I.C. P. W. Shallis (Secretary) University of Bradford (Professor of Pharmacy) Ir'eckitt & Sows L t d . (Chazv7/nan) A.K.I.C. F. R . I. C. cognosy ) Rush Boake Allen Ltd.Westminster Laboratories Ltd. TERMS OF REFERENCE-"TO investigate methods for estimating the purgative activity of drugs and preparations of drugs containing anthraquinone derivatives with a view to recom- mending standard methods of assay." PROGRESS OF WORK- With the publication in the November issue of The Analyst of the Report on "The Chemical Assay of Cascara Dry Extract Cascara Tablets and Cascara Bark," the Panel completed its work. The Panel began its work in 1956 with an investigation of the chemical assay of senna (Analyst 1966 90 582) and this was followed by an investigation of the chemical assay of aloes (Aaalyst 1967 92 593). In the final stage of the Panel's work on the chemical assay of cascara a modified version of Fairbairn and Sirnic's method (-1. Yharm.Pharmac. 1964 16 450) was investigated. This method was found to be suitable for the assay of cascara bark dry extract and tablets but for reasons not fully understood was not satisfactory for liquid preparations of cascara. In the absence of a suitable alternative method for liquid preparations the Panel has recommended a method applicable only to the bark and dry preparations. The Panel has now been disbanded. 124 REPORT OF THE ANALYTICAL METHODS COMMITTEE [Proc. Soc. Anzalyt. Chem. PANEL 8 PHENOTHIAZINE CONSTITUTION- W. H. Stephenson F.P.S. D.B.A. F.R.I.C. K. J. Anderson BSc. A.R.I.C. J. K. Bailey A.R.I.C. A. Holbrook F. R.I.C. 3CChem.A. D. A. Walker B.Sc. A.R.I.C. P. W. Shallis (Secretary) Boots Pure Drug Co. Ltd. Cooper Techvzical Bureau Boots Pure Drug Co. Ltd. Imperial Chemical Industries Ltd.(Phavmaceu- ticals Division) Nicholas Research Institute Ltd. M. Ph. A. (Chairman) TERMS OF REFERENCE-"(^) To recommend a satisfactory method for determining pheno- thiazine and (b) to extend this method to cover most commercial phenothiazine dispersible powders. ” PROGRESS OF WORK- A comparison of the Panel’s gas - liquid chromatographic method with the somewhat different procedure adopted by the A.O.A.C. ( J . Ass. 08. Agric. Chewz. 1967 50 682) was carried out during the year on a collaborative basis. All laboratories taking part found that both methods gave almost identical results. The Panel has however concluded that it prefers 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 duplicate injections.The A.O.A.C. method also makes use of chloroform as solvent and the Panel had earlier experienced some difficulty in dispersing liquid phenothiazine preparations in this solvent. The Panel’s Report including details of the collaborative comparison of the two methods has now been accepted for publication in The Analyst. PANEL 9 THEN-LAYER CHROMATOGRAPHY OF CORTICOSTEROIDS CONSTITUTION- C. A. Johnson B.Sc. B.Pharm. F.P.S. F.R.I.C. M.Ph.A. (Chairwzun) K. A. Rastow B.Sc. F.R.I.C. A. Hall B.Sc. W. McMeekin B.Sc. Ph.D. J . S. Wragg R.Sc. P.R.I.C. P. W. Shallis (Secvetavy) Bvitish Pharmacopoeia Commission PfLzer Ltd. Glaxo I-abovatories Ltd. Organon Labovatovies Ltd. Boots Pure Drug Co.Ltd. TERMS OF REFERENCE:-“TO devise a thin-layer chromatographic procedure to limit foreign steroids in corticosteroids which it is hoped will prove suitable for use in Monographs of the R.P. and the R.P.C.” PROGRESS OF WORK- In the 2 years since the completion of the phase of the Panel’s work that led to the recom- mendation of a thin-layer adsorption system for separating and assessing related steroid impurities in corticosteroids which has been adopted by the British Pharmacopoeia a con- siderable amount of work aimed at finding an improved method has been carried out. The thin-layer partition system under consideration by the European pharmacopoeia has been investigated but although excellent for identification purposes was found not to offer any particular advantages over the Panel’s system €or quantitative work.Other techniques such as continuous evaporation of the solvent front in an attempt to improve separations of close running impurities and quantitative elution of impurity bands and the main band from the plate with subsequent spectrophotometric mezsurement to improve the precision of assessment have been tried but have not proved sufficiently repeatable from laboratory to laboratory to warrant publication as a standard method. The Panel has concluded that there is little chance of further progress unless some fundamental advance in technique is made. In consequence the Panel is carrying out no further work and is to be disbanded. July 19691 REPORT OF THE ANALYTICAL METHODS COMMITTEE PANEL 10 ACCURACY AND PRECISION I N PHARMACEUTICAL ANALYSIS CONSTITUTION- A.L. Glenn B.Sc. B.Pharm. Ph.D. F.P.S. A. F. Adamson B.Sc. Ph.D. F.R.I.C. F. Bailey L.R.I.C. R. A. Bastow B.Sc. F.R.I.C. P. F. G. Boon B.Sc. A.K.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. M.C.I.C. F.P.S. A.R.I.C. J. C. Deavin D. H. Dorken R.Pharm. M.P.S. F.R.I.C. M. J. K. Healy E. F. Hersant B.Pharm. Ph.D. F.R.I.C. F.P.S. D. W. Houghton l3.S~. J,. P. Jefferies B.Sc. F.K.I.C. C. A. Johnson B.Sc. B.Pharm. F.P.S. F.R.I.C. W. 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.Pharm. M.P.S. A.R.I.C. D. 14 i\l tchell B.Sc. A\. R. Moss B.Sc. Ph.D. A. W. C. I cacock B.Pharm. F.P.S. G. F. Phillips M.Sc. F.R.I.C. C. Radford L. R. Rowe B.Sc. Ph.D. A.R.C.S.D.I.C. M. 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. (Chairman) M.Ph.A. F. R. I .C. C. H. Thorpe B.Sc. A. J. Woodgate B.Sc. A.R.I.C. J. Wragg B.Sc. F.R.I.C. P. W. Shallis (Secretary) 125 University of London (School of Pharmacy) Wixthrop Lahoratories Imperial Chemzzcal 1 ndustvies Ltd. (Phavma- ceutiral Division) Pfizer Ltd. Ciba Laboratories LLd. Monsanto Chemicals Ltd. E. R. Squibb G. Sons L f d . Nacholas Products Ltd. Reckitt & Sons Ltd. Pharmace%ttical Socie fy of Great Britain Smith Kline 655 French Laboratories Ltd. M . R. C . Clinical Research Centre May & Baker Ltd. G. D. Searle & Co. Ltd. Glaxo Laboratories Ltd. British Pharmacopoeia Comfnission Cyunamid of Great Britain Ltd.Abbott Laboratories Ltd. Evans Medical Research Laboratories Parke Davis & Co. Burroughs Wellcome G. Co. Roche Products Ltd. Riker Laboratories ,Winistry of Technology Laboratory of the E1.i Lilly & Co. Ltd. Allen & Hanburys Ltd. Koussel Laboratories Ltd. Upjohn Ltd. Merck Sharp & Dohme Ltd. Geigy (U.K.) Ltd. (Pharmaceuticals Division) Chelsea College of Science and Technology (Pharmacy Department) B.D.H. Pharmaceuticals Ltd. Bush Boake Allen Ltd. Boots Pure Drug Co. Ltd. Government Chemist TERMS OF REFERENCE-“(i) To evaluate the accuracy and precision obtainable from esta- blished methods of pharmaceutical analysis under normal conditions of quality control. (ii) To investigate ways of improving accuracy and precision in pharmaceutical analysis.’’ PROGRESS OF WORK- Although the Panel has not held a meeting during the year a programme of collaborative work has been undertaken.Two tests have been carried out by a large number of analysts and the results are currently being processed by computer. The first test designed to measure the error in weighing and transferring a sample involved the weighing of a sample of potassium dichromate on a macrobalance transferring it to a 100- ml calibrated flask diluting it to volume and measurement of the extinction of the solution at 350 nm. The second test was designed to measure the errors in volumetric measurement. Calibration of 50 and 100-ml volumetric flasks 1 5 and 25-ml bulb pipettes and a 50-ml burette at various pre-arranged graduations was carried out by weighing the amount of water at known temperature contained in the flasks or delivered from the pipettes or burette.It is intended that when processing of the many results submitted is complete a report on this work will be published. 126 REPORT OF THE ANAT~YTICAL METHODS COMMITTEE [Proc. SOC. AflaZyt. Chew. APPENDIX I THE SOCIETY FOR ANALYTICAL CHEMISTRY ANALYTICAL METHODS TRUST ACCOUNTS FOR THE YEAR ENDED OCTOBER 31s~ 1968 Income and ExpevlditurP Account f o v the Yeav Evlded Octobev 31st 1968 Subscriptions and Donations from Industry . . Interest Received From Investments . . . . . . . . From Bank Deposits . . . . . . Books (Heffers) . . . . . . . . Rook Department . . . . . . . . Sales Income Tax Refunds Covenanted subscriptions 1966-67 . . Investments 1966-67 . . . . . . DEDUCT Rent Light Heat and Telephone... . Salaries . . .. . . . . .. Alterations and Maintenance of Premises Maintenance of Office Equipment. . Printing and Stationery . . . . Expenses of Meetings . . .. Postage . . .. . . .. Legal Charges . . . . .. Audit Fee . . .. . . .. Sundries . . .. . . . - Depreciation .. . . . . Stock a t 31.10.67 .. Printing of A.M.C. Publications . . Book Department Salaries . . Postage . . LESS Stock at 31.10.68 . . . . . . . . . . . . .. .. . . . . . . . . . . .. .. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. . . . . .. .. . . . . . . . . . . .. . . .. . . .. .. .. . . .. . . .. .. .. .. .. .. * . .. . . . . . . .. . . . . . . . . . . . . .. . . . . .. . . . . . . . . 1840 242 260 90 .. Excess of Income over Expenditure for the year ended October 31st 1968 transferred to Accumulated Fund .. .. . . .. L 356 479 234 3346 452 142 ~ 1056 3145 2 277 280 63 37 23 - - - - 2432 1200 L 1768 835 3580 594 1967 1082 L 230 818 455 1135 424 164 6777 4308 4883 1232 6115 594 3056 353 215 163 140 48 - - 52 2 5 2447 607 1840 - 5253 k945 (loss) July 10691 REPORT OF THE ANALYTICAL METHODS COMMITTEE Balance Sheet at October 31st 1968 Current Assets Stock of Rooks IJnsold . . . . . . . . . . . . Sundry Debtor The Society for Analytical Chemistry . . Cash a t Banks Old Broad Street Securities Ltd. . . . . . . . . . . Barclays Bank Ltd On Current Account . . . . . . . . . . . . On Deposit Account . . . . . . . . . . . . J)EUUCT CURRENT I J I m I L i n i ~ s Thc Socicty for Analytical Chemistry . . . . . . . . NET CURRENT Assms . . . . . . . . . .. . . . Investments (at cost) as per Schedule (Market Value k20731) . . I:inanced by Accumulated Fund Balance November lst 1967 . . . . . . . . Less Loss on sale of Shares during year Add Excess o f Income over Expenditure for year ended October 31st 1968 . . . . . . .. . . .. Signed on behalf of the Analytical Methods Trust Fund 24055 90 - G. 2967 jtr L 1200 1840 - 75 - 11000 358 763 5073 3686 6706 17289 - - 619 6706 16670 17921 7385 ~ _ _ _ _ ~- 24627 24055 =- 127 25000 23965 662 945 (loss) ~~ 24627 24055 - H. LLOYD- JACOB (Chairman) G. W. C. MILNER (Honorary Treasurer) A udztors’ Report to the Trustees of the Society for Analytical Chemistry Analytical Methods Trust 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 Fund a t October 31st 1968 and i t is in accordance with the Rooks 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. January 3rd 1969. (Signed) RIDLEY & CO. Chartered Accountants Auditors. 128 Nominal amount &loo L l O O 700 1900 250 2300 600 500 83 375 1000 1100 660 400 64 300 1200 400 REPORT OF THE ANALYTICAL METHODS COMMITTEE Schedule of Investments held at Octohev 31st 196'8 34% Conversion Stock (Sold 26.7.68 for 3+% War Stock (Sold 26.7.68 for Burmah Oil Co. Ltd. L1 Ordy Stock Courtaulds Ltd. 5s. Ordy Shares (Rt. Debenhams Ltd. 10s. Ordy Shares . . Distillers Co. Ltd. 10s. Shares (Bt. Eagle Star Insurance Co. Ltd. 10s. Ordy Shares (Bt. 16.2.68 for L2546. 10. 6) Philip Hill Investment Trust Ltd.5s. Hill Samuel & Co. Ltd. 5s. Ordy Shares Imperial Chemical Industries Ltd. k1 M. & G. Fund of Investment Trust Income Units (Bt. 29.7.68 for Morris 62 David Jones Ltd. Ordy Shares Ranks Hovis McDougall Ltd. Ordy Stock Units . . . . . . . . Renold Ltd. ;tT1 Ordy Stock Units . . Rights Issue 4 L1 Ordy for 25 at 53s. Royal Insurance Co. Ltd. 5s. Stock Units . . . . . . . . L46. 11. 6) . . . . . . . . L45. 16. 6) . . . . . . . . Units (Bt. 16.2.68 for L2550. 6. 6) 16.2.68) . . . . . . . . 16.2.68 for L2411. 7. 5) . . . . Ordy Shares . . . . . . Ordy Stock Units . . . . . . L575. 0. 1) . . . . . . . . each (Q69. 12. 0) . . . . . . Venesta Ltd. 5s. Ordy Shares . . .. Wharf Holdings Ltd. Ordy Shares . . Held 31.10.67 at cost 83 100 - - 747 - - 607 101 736 - 1012 1001 685 - 735 872 706 7385 Loss on H Proc.Soc. Amalyt. Chew. Id Sale 31.10.68 during year at cost - 36 - 54 2550 2466 747 241 1 2547 607 101 736 575 101 2 1001 685 170 735 872 706 90 17921 ___ .~ _-_ - = Market value 3 1.10.68 - - 3447 3182 475 2361 2550 675 123 1204 550 1210 1361 1070 171 645 435 670 Income received during year ended 31.10.68 1 3 24 49 20 43 24 13 1 23 - 40 35 26 - 18 9 22 20731 356 ~- July 19691 PAPERS ACCEPTED FOR THE ANALYST APPENDIX I1 SURSCRIBEKS TO THE TRUST FUND IN 1968 AND 1969 129 DURING 1968 Albright & Wilson Ltd. Associated Portland Cement Manufacturers Cadbury-Fry Ltd. Central Electricity Generating Board Courtaulds Ltd. Dunlop Rubber Co. Ltd. Geigy (U.K.) Ltd. Hopkin & Willianis Ltd. Imperial Chemical Industries Ltd. Laporte Industries Ltd.J. Lyons & Co. Ltd. May & Raker Ltd. The Metal Box Co. Ltd. 0x0 Ltd. The Pharmaceutical Society of Great Britain Riker Laboratories Ltd. Roche Products Ltd. Sandoz Products Ltd. Smith Nine & French Laboratories Ltd. John & E. Sturge Ltd. Ltd. SUBSCRIBERS EXPECTED DURING 1969 Abbott Laboratories Ltd. Albright & Wilson Ltd. Associated Portland Cement Manufacturers Beecham Group Ltd. Roots Pure Drug Co. Ltd. Rovril Ltd. British Aluminium Co. Ltd. British Arkady Co. Ltd. British Glues & Chemicals Ltd. British Petroleum Co. Ltd. British Titan Products Co. Ltd. Courtaulds Ltd. Ltd. Distillers Co. Ltd. Geigy (U.K.) Ltd. Glaxo Group A. Guinness Son & 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 & Co. Ltd. J . Mackintosh & Sons Ltd. Marks & Spencer Ltd. May & Baker Ltd. hlerck Sharp Sr Dohme Ltd. Nicholas Products Ltd. Organon Laboratories Ltd. 0x0 Ltd. Parke Davis & Co. Pfizer Ltd. The Pharmaceutical Society of Great Britain Procea Products Ltd. Quaker Oats Ltd. Ranks Hovis McDougall Ltd. Keckitt & Colman Holdings Ltd. Riker Laboratories Ltd. J. Sainsbury Ltd. Sandoz Products Ltd. Smith Kline & French Laboratories Ltd. Smith & Nephew Ltd. Spillers Ltd. J. & E. Sturge Ltd. Unilever Ltd. Wallace & Tiernan Ltd. The Wellcome Foundation Weston Research Laboratories Ltd. J. Wyeth & Brother.

ISSN:0037-9697    

DOI:10.1039/SA9690600111

出版商:RSC    

年代:1969

数据来源: RSC

摘要:

July 19691 PAPERS ACCEPTED FOR THE ANALYST 129 Papers Accepted for Publication in The Anatyst THE following payers have been accepted for publication in The Afizalyst and are expected to appear in the near future. “The Direct Determination of Boron in Copper Alloys and Nickel After Dissolution in “The Determination of Anionic Detergents with Iron(I1) Chelates Application to Sewage “Interferences in the Determination of Iron by Atomic-absorption Spectrophotometry “Ammonium Dioxalato-oxotitanate(1v)-A New Primary Standard,” by V. Zatka. “Limit of Determination in Photometric Titrations with Self-indicating Systems,’ ’ by E. R. Groencveld and G. den Roef. “Improvement of Detection Limits of Flame-spectrophotometric Determination of Chlorinated Organic Pesticide Residues,’ ’ by Roland Herrmann and Brigitte Gut sche. Nitric A4cid,” by P. Pakalns. and Sewage Effluents,” by C. Taylor and R. Fryer. in an Air - Acetylene Flame,” by K. E. Curtis.

ISSN:0037-9697    

DOI:10.1039/SA9690600129

出版商:RSC    

年代:1969

数据来源: RSC

摘要:

130 THE SOCIETY FOR ANALYTICAL CHEMISTRY Announcements For the analyst. . . The new EEL 227 lntegrating Flame Photo- meter offers high precision for the simultaneous determination of sodium and potassium particu- larly in clinical tests. The EEL 227 is a twin- channel double-beam flame photometer with a lithium internal standard. In the double-beam system of measurement the lithium standard is introduced into the samples and signals from it are balanced against the sodium and potassium signals to nullify long-term instabilities from variation of air and fuel pressure change of sample temperature and viscosity and minor chemical interferences. Integration of the photomultiplier currents from the two channels offsets short-term instabilities in the flame and rate of nebulisation. The time of integration (about 10 seconds) is determined by a pre-set output level on the lithium channel and results in steady and reproducible meter readings.Details from Evans Electroselenium Limited Church Lane Braintree Essex. l’ye tJnicam Ltd. of Cambridge have introduced a Philips automatic sample changer for use with the standard Philips YW 1050 X-ray diffracto- meter. ’The Philips PW 1 170 provides fully automatic diffraction analysis of up to 35 powder samples over a pre-set angular range allowing unattended operation and shutdo~m. This feature improves the efficiency of an X-ray diffractometer by making possible the operation of the instrument overnight. Typical applications include the routine production of diffraction patterns or intensity measurements on a selected diffraction peak in which case the results can be printed out. Normally the sample number is indicated in analogue form on a recorder or digitally on a printer. The PW 1170 consists of a mechanical changing unit with an exchangeable magazine for up to 35 samples holders and a control unit mounted in a standard 19-inch rack. Printed by W Heffer & Sons Ltd Cambridge England

ISSN:0037-9697    

DOI:10.1039/SA969060130b

出版商:RSC    

年代:1969

数据来源: RSC