摘要:

Proceedings of the Society for Analytical Chemistry CONTENTS Reports of Meetings . . . . 69 “Development of Chemical Crop Protection in Britain” 7 I Thermal Analysis . . . . 75 Report of the Analytical Meth- ods Committee 1965 .. . . 77 Membership changes . . . . 92 Publications Received . . . . 93 Notices .. .. .. .. 93 Proc. SOC. Analyt. Chem. Vol. 3 No. 5 Pages 69-94 Forthcoming Meetings . . . . 94 May 1966 Vol. 3 No. 5 May 1966 PROCEEDINGS THE SOCIETY FOR ANALYTICAL CHEMISTRY OF President of the Society A. A. Smales O.B.E. Hon. Secretary of the Society S. A. Price Hon. Treasurer of the Society D. T. Lewis C.B. Hon. Assistant Secretaries of the Society 8. S. Cooper; D. W. Wilson Secretary Miss P. E. Hutchinson 14 BELGRAVE SQUARE LONDON S.W.1 Telephone BELgravia 3258 Editor J.B. Attrill Proceedings is published by The Society for Analytical Chemistry and distributed t o members and all subscribers t o The Analyst without charge Single copies may be obtained direct from the Secretary The Society for Analytical Chemistry a t the above address (NOT through Trade Agents) price 2s. 6d. post free. Remittances payable t o “Society for Analytical Chemistry” MUST accompany orders Official Standardised and Recommended Methods of Analysis Compiled and Edited for THE ANALYTICAL METHODS COMMITTEE OF THE SOCIETY FOR ANALYTICAL CHEMISTRY by S. C. JOLLY B.Pharm. B.Sc. A.R.I.C. M.P.S. pp. xx+577 Price di6 6s. net Members of the Society for Analytical Chemistry are entitled to buy copies a t the special Members’ price of &4 4s. provided they order direct from The Editor The Analyst 14 Belgrave Square London S.W.I. Remittances made out to- “Society for Analytical Chemistry” must accompany Members’ orders. Published for the Society for Analytical Chemistry W. HEFFER & SONS LTD. PETTY CURY CAMBRIDGE by

ISSN:0037-9697    

DOI:10.1039/SA96603FX017

出版商:RSC    

年代:1966

数据来源: RSC

摘要:

May 1965 PROCEEDINGS OF THE SOCIETY FOR ANALYTICAL CHEMISTRY Vol. 3 No. 5 Reports of Meetings SPECIAL MEETING A SPECIAL Meeting of the Society was held at 6.30 p.m. on Tuesday April 26th 1966 in the Meeting Room of the Chemical Society Burlington House London W.l. The Chair was taken by the President Dr. A. A. Smales O.B.E. F.R.I.C. A lecture on “Automated Systems for Extra-terrestrial Nuclear Activation Analysis” was given by Professor R. E. Wainerdi Ph.D. (co-authors Dr. M. Y. Cuypers Dr. J. Hislop and Mr. W. E. Kuykendall) . ORDINARY MEETING AN Ordinary Meeting of the Society was held at 2.30 p.m. on Wednesday May 4th 1966 in the School of Chemistry The University Bristol. The Chair was taken by the President Dr. A. A. Smales O.B.E. F.R.I.C. The meeting was devoted to short papers on “Research Topics in Analytical Chemistry some current work in Universities and Colleges of Advanced Technology” and the following papers were presented and discussed “Some Aspects of Titrimetry on the Microgram Scale,” by C.L. Graham B.Sc. ; “Some Developments in the Use of Oximes as Analytical Reagents,” by C. Broughton M.Sc. A.R.I.C. A.R.T.C.S. ; “Continuous Substoicheiometric Analysis,” by B. Cooksey L.R.I.C. ; “Precise Coulometric Titration,” by M. Riley B.Sc. and E. Bishop B.Sc. A.R.C.S.T. F.R.I.C. ; “A New Fluorimetric Reagent for the Determination of Sub- microgram Amounts of Magnesium,” by R. Smith B.Sc. A.R.C.S. ; “Chromatography of Some First Row Transition Metals on Thin Layers of Substrates Impregnated with Tri-butyl Phosphate,” by G. Duncan B.Sc. A.R.C.T. L. S. Bark B.Sc.F.R.I.C. M.R.S.H. and R. J. T. Graham M.Sc. Ph.D. A.R.I.C. ; “Some New Inorganic Ion-exchangers,” by G. N. Stradling B.Sc. ; “Analytical Properties of Heterocyclic Azo Dyestuffs,” by R. G. Anderson B.Sc. and G. Nickless B.Sc. Ph.D. The meeting was preceded by a visit to the Analytical Chemistry Laboratories of Bristol University. MIDLANDS SECTION THE Eleventh Annual General Meeting of the Section was held at 5.30 p.m. on Tuesday March 8th 1966 at Boots Pure Drug Co. Ltd. Pennyfoot Street Nottingham. The Chair was taken by the Chairman of the Section Mr. W. T. Elwell F.R.I.C. The following appoint- ments were made for the ensuing year :-Chairman-Mr. W. T. Elwell. Vice-Chairma%- Mr. H. E. Brookes. Honorary Secretary-Mr. M. L. Richardson John & E. Sturge Ltd. Liff ord Chemical Works Liff ord Lane Kings Norton Birmingham 30.Ho.tzorary Treaswer- Mr. G. Ingram. Members of Committee- Dr. Alison M. G. Macdonald Professor R. Belcher Mr. K. A. Hyde Dr. V. J. Jennings Mr. W. M. Lewis Mr. N. Nix Mr. D. M. Peake and Dr. A. Townshend. Miss M. E. Tunnicliffe and Mr. P. G. W. Cobb were appointed as Honorary Auditors. The Annual General Meeting was held between two halves of a Joint Meeting of the Section with the Forensic Science Society and the East Midlands Section of the Royal Institute of Chemistry at which the Chair was taken by the Chairman of the Midlands Section Mr. W. T. Elwell F.R.I.C. The following papers were presented and discussed “New Methods and Applications for the Analysis of Raw Materials and Intermediate Products in the Drug Industry,” by J. Allen F.R.I.C.; “New Methods and Applications for the Analysis of Pharmaceutical Presentations,” by S. G. E. Stevens B.Sc. F.R.I.C.; “Drug Analysis with Special Reference to Forensic Analysis,” by E. G. C. Clarke M.A. Ph.D. D.Sc. F.R.I.C. 69 Honoyavy Assistant Secretary-Mr. R. Adkins. 70 REPORTS OF MEETINGS [PYOC. SOC. Analyt. Chew. A JOINT Meeting of the Section with the Birmingham and Midlands Sections of the Royal Institute of Chemistry and the Society of Chemical Industry was held at 7.30 p.m. on Thursday March 24th 1966 at the North Staffordshire College of Technology Stoke-on-Trent. The Chair was taken by the Chairman of the Midlands Section Mr. W. T. Elwell F.R.I.C. The following paper was presented and discussed “Automatic Analysis in Industry,” by A. G. Scobie B.Sc.A JOINT Meeting of the Section with the Lea-Valley Sub-section of the Royal Institute of Chemistry was held at 6.45 p.m. on Wednesday April 20th 1966 at the Bedfordshire College of Further Education Luton. The Chair was taken by the Chairman of the Midlands Section Mr. W. T. Elwell F.R.I.C. The following paper was presented and discussed “Recent Investigations at the Labora- tory of the Government Chemist,” by D. T. Lewis C.B. Ph.D. D.Sc. F.R.I.C. F.R.S.H. SPECIAL TECHNIQUES GROUP AN Ordinary Meeting of the Group was held at 7 p.m. on Tuesday March 22nd 1966 in Chemistry Lecture Theatre C Imperial College of Science and Technology London S.W.7. The Chair was taken by the Chairman of the Group Dr. G. F. Reynolds M.R.S.H. F.R.I.C. The subject of the meeting was “New Aspects of Infrared Spectrometry” and the following papers were presented and discussed “Far Infrared Spectroscopy and Some Applications,” by A.E. Martin Ph.D. D.Sc.; “Infrared Spectroscopy with the use of Multiple Internal Reflections,’’ by A. C. Gilby B.Sc. Ph.D. ATOMIC-ABSORPTION SPECTROSCOPY GROUP THE Twelfth Ordinary Meeting of the Group was held at 9.30 a.m. on Tuesday April 5th 1966 at the School of Chemistry The University of Newcastle upon Tyne 1. The Chair was taken by the Chairman of the Group Mr. W. T. Elwell F.R.I.C. The meeting took the form of demonstrations and discussions on “Commercial Atomic- absorption Apparatus.” Some delegates also visited the International Research & Development Co. Ltd. AUTOMATIC METHODS GROUP AN Ordinary Meeting of the Group was held at 6.30 p.m. on Tuesday April 5th 1966 in the Meeting Room of the Chemical Society Burlington House London W.1.The Chair was taken by the Chairman of the Group Dr. G. V. R. Mattock B.Sc. F.R.I.C. The subject of the meeting was “Sample Handling Techniques” and the following papers were presented and discussed “The Moisture Content Determination of Materials which May Vary in Density with their Moisture Content,” by R. G. Godding; “Sampling in the Fertiliser Industry,” by K. A. Sherwin ; “Sample-handling Techniques as Applied to Oil Blending and Mineral Processing,” by A. Hewett-Emmett. PARTICLE SIZE ANALYSIS GROUP AN Ordinary Meeting of the Group was held at 7 p.m. on Tuesday April 5th 1966 at the Bradford Institute of Technology Bradford 7. The Chair was taken by the Chairman of the Group Mr. T. Allen M.Sc. The following papers were presented and discussed “The I.C.I. Joyce Loebl Disc Centri- fuge for Particle-size Analysis,” by M. H. Jones; “Particle-size Analysis in the Sub-Sieve Range with an A.W.R.E. Centrifugal Photosedimentometer,” by M. W. G. Burt; “The Simcar Centrifugal Particle-size Analyser,” by C. Slater.

ISSN:0037-9697    

DOI:10.1039/SA9660300069

出版商:RSC    

年代:1966

数据来源: RSC

摘要:

May 19661 DEVELOPMENT OF CHEMICAL CROP PROTECTION IN BRITAIN 71 Development of Chemical Crop Protection In Britain BY J. T. MARTIN (Long Ashton Reseavch Station Univevsity of Bvistol) AWARENESS of plant diseases and of the need to combat them was general in this country about 300 years ago. In 1657 R. A. Austin wrote “All trees or plants are afflicted with divers diseases as sensible creatures; and therefore we should apply ourselves to cure them not for pity to the trees but for our own profit.” Descriptions of pests and of their depradations came from the naturalists of the time. Special care was taken of fruit trees-orcharding had expanded since the time of Henry VIII when Harris the king’s gardener planted orchards in Kent to supply the royal kitchen. Caterpillars ants bark-worms earwigs snails and wasps were named as pests and moss and canker as diseases.The remedies used were primitive and of little value; straw fires some- times with added tobacco waste or sulphur were used to dislodge insects bark-worms were treated with a wash of cowdung and urine and wood ashes nettles and ferns were strewn beneath the trees. Insect infestations and fungus infections were known collectively as “blights,” and storms lightning and “noxious qualities” in the air were regarded as causative agents. The theory held since classical times that caterpillars and other blights arose from the vivification of rain-drops by sunshine still found support and was extended to other moist or slimy deposits on plants. Another view decreed that blights arose from the eggs of creatures that circulated within the plant the eggs being brought to life on mingling with the stagnating juices of bruised parts.The develop- ment of tree canker and the rotting of fruits were explained in this way. To kill eggs cir- culating within the tree an injection of metallic mercury into the trunk was recommended surely the first attempt to achieve systemic action. These ideas on the origin of plant diseases were overshadowed by the easterly wind theory held since biblical times. This postulated that plant diseases and many of the distempers of man including the plague arose from eggs or microscopic animals carried to this country by the easterly winds in spring. The theory which reflected the earlier idea of “noxious qualities” in the air gained support from the newly invented microscope which revealed the existence of minute organisms not visible to the naked eye.The apothecaries of the Bucklersbury quarter in London were believed to have possessed some immunity from the plague; strongly scented herbs and roots aromatic gums garlic cedar extract and black pepper therefore found favour as remedies against plant afflictions. Trees were washed with water in which onions had been steeped and bruised onions were strewn in the orchards a survival of the suggestion made at the time of the plague that boats containing onions should be moored on the Thames to combat the disease. Such practices are recalled by the traditional use in more recent times of herbs at the opening of the Old Bailey. The first doubts on the validity of the theory of windborne invasion arose about the middle of the eighteenth century from observations on the development of colonies of “smotherflies” (aphids).Those first seen on the plant were wingless the winged forms appearing later. They were believed to have arisen from the vivification of honey-dew then thought to be a product of the perspiration of leaves. The method of control recommended aimed at reducing the secretion of honey-dew; salt was spread on the ground beneath the plant and watered in. Another treatment consisted of swishing a brine wash into trees with coarse brushes; in 1755 the engines that had been devised for extinguishing fires were sug- gested as suitable instruments for the work. Corn seed was steeped in brine lime water or a solution of salt-petre alum or verdigris. To protect grain after harvesting it was placed in a pit and covered with lime.These seed dressings were used for about 100 years when they were replaced by steeps of copper sulphate or formaldehyde . The middle of the eighteenth century saw developments in the use of tobacco extract for controlling pests. As early as 1690 a tobacco wash was used in France for the control of an insect attacking pear trees. In 1734 Peter Collinson of London suggested that tobacco leaves be used to protect seeds and plants in transit and 12 years later he recommended the use of Progress was hampered by the popular beliefs held at the time. At about the same time interest was taken in treating seeds before sowing. * Presented a t a meeting of the Society on Wednesday March 9th 1966. 72 [Proc. SOC. Analyt. Chem. tobacco extract for the control of plum curculio on nectarine trees.The tobacco leaves were boiled in water with or without the addition of sulphur or black pepper or the extract could be purchased from the tobacco factory. By 1800 the tobacco - sulphur wash was established as the most efficient remedy against insects and mildew on fruit trees. By this time spraying machines known as “garden engines” were coming into general use. During the early years there was a marked increase in knowledge of the biological aspects of pest control. Insects and “parasitic plants” were differentiated as causative agents of blights many species of insects and fungi were described and the derivation of insect infestations from over-wintering eggs and the parthenogenetic reproduction of aphids were elucidated. Predation among insects was recognised; as early as 1740 Richard Bradley an ex-professor of botany at Cambridge had observed that “ichneumon flies feeding on caterpillars beetles and cankerworms may have their own foes and so to infinity.” Early in the century American “bug” or “blight” (woolly aphis) was inadvertently introduced into this country on trees imported from South America; confined a t first to an area around London it later spread to many parts and became one of the most serious pests of fruit trees.Other major pests such as raspberry moth were recorded. The invasion of stems of brassica plants by the larvae of a fly was described but as the larvae were smaller than those of the “flesh” or “blow” fly the damage was ascribed to the housefly! The severe potato famine of 1845 in Ireland brought salutory recognition that losses of crops due to disease were important factors in the life of the community.With the better understanding of the nature of pests and diseases came improved methods for their control. Soft soap found to affect aphids was added to the tobacco wash thereby increasing its efficacy. Fruit trees were treated with a suspension of sulphur in lime water the forerunner of the more efficient reacted product first prepared in 1851. Copper products became established as protectants of foliage against some diseases. Solutions of bluestone used earlier as steeps for corn seed were damaging but this difficulty was largely eliminated by the introduction between 1885 and 1887 of the insoluble Bordeaux and Burgundy mixtures. The original Bordeaux mixture consisted of 60 lb of copper sulphate and 115 lb of quicklime in 100 gallons of water but by 1890 the recommended strength had been reduced to 20 + 10 + 100 giving a material that could be applied as a spray; other copper products such as the oxychloride followed.Kerosene - soft soap emulsion and quassia extract prepared from wood chips of Quassia amaya L. and Picraena exelsa Lindl. from the West Indies became popular for use against aphids especially on hops and plums. Hellebore consisting of the powdered rhizomes of the white hellebore Ve‘evatvum album L. was recommended for a time for use on soft fruits. Nicotine fumigating papers were first manufactured about 1890 and 95 per cent. nicotine alkaloid was available to the grower in 1900. Tradition dies hard and older remedies persisted until the end of the century; one for the protection of valuable trees deserves to be recorded “Add 5 lb.of tobacco leaves to 8 pail of water and keep hot for 24 hours. Squeeze the water from the leaves add 8 pail of bullock’s blood 1 part of slaked lime and 16 partsof cowdung. Paint liberally on to the tree.” The early years of this century saw the rise of the arsenicals. Paris or Emerald Green (copper aceto-arsenite) was promoted by the Evesham Fruit Growers’ Experimental Com- mittee about 1890 for the control of caterpillars on fruit trees and bushes. London Purple an arsenical by-product from the dye-stuff industry and calcium salts were also used but damage to foliage led to the introduction of the insoluble lead arsenate first prepared by mixing lead acetate and sodium arsenate in the spray tank.Unless properly prepared unreacted soluble arsenate still caused damage but the position was improved by the marketing in 1906 of a factory-prepared lead arsenate paste. The risk of damage to foliage however focused attention on the possibility of controlling some insects by killing their eggs during the dormant period. Belief in the efficacy of lime was still strong and the lime-washed trunks of fruit trees became a feature of the countryside. At Long Ashton founded in 1903 many variants of lime and caustic washes were tried with little success. Aphids and many other insects abounded in orchards and little could be done against pests of vegetable and arable crops. A writer of the time plaintively observed that unfortunately there were still a few pests for which no certain cure had been found.The position was dramatically changed with the introduction in the early 1920’s of the tar oil winter wash first used for the control of aphids on plum trees. DEVELOPMENT OF CHEMICAL CROP PROTECTION IN BRITAIN The nineteenth century saw important advances. Keep in an open tub stirring daily and use after fermentation has set in. The modern era of chemical crop protection had begun. May 19661 DEVELOPMENT OF CHEMICAL CROP PROTECTION I N BRITAIN 73 The two decades before the Second World War were marked by the rapid development of commercial interest in crop protection and by the extension of work at the official research stations. Many factory-produced materials became available and industrial research centres were set up. Rothamsted’s interest in the effect of chemical structure upon biological activity led to the development of dinitro-o-cresol as an insecticide; this material had earlier been used under the name antinonnin to control forest pests in Bavaria.The potential risks to the consumers of soft fruits treated with arsenicals prompted collaborative work between Rothamsted and the Ministry of Agriculture’s Plant Pathology Laboratory on safe alternatives of botanical origin. Many fish-poison plants were examined but interest was centred on derris roots from the Far East and pyrethrum flowers from Albania. The active principles of derris root were isolated methods were devised for the chemical standardisation of extracts and field trials at Long Ashton and elsewhere confirmed the value of derris as a horticultural insecticide.Work on the chemistry insecticidal activity and commercial production of pyrethrum coincided with and assisted the establishment of the Kenya industry. The success of tar as a winter wash led to the development of other dormant sprays based on petroleum or mixed tar - petroleum oil fractions. Dinitro-o-cresol was damaging to foliage but found valuable use as a dormant spray with petroleum whereby the range of insects controlled by petroleum or tar alone could be extended. Despite the success of the winter washes summer sprays e.g. of nicotine or lead arsenate were still needed. Varying degrees of sucess were obtained against pests such as flea beetles but wireworms and other pests in the soil remained intractable. Attention during this period was directed towards the efficient use of mixed insecticide - fungicide washes to reduce the costs of separate applica- tions.Successes were limited but no serious side-effects arose. The lesson that too efficient an insect killer was not necessarily advantageous had yet to be learnt. During the pre-war period valuable work was done on the standardisation of spray materials in which analytical chemistry played a conspicuous part. In 1910 the Chamber of Horticulture drew attention to the need to standardise products and brief minimum specifi- cations for seven commonly used materials were published shortly afterwards. Later the Association of British Insecticide Manufacturers prepared agreed specifications with methods of analysis for fifteen summer spray materials and Hubert Martin formulated specifications and methods for winter washes.The specifications and methods were published by the Ministry of Agriculture finally in its Technical Bulletin No. 1. Each material was con- sidered by a committee of representatives from industry the Ministry of Agriculture the Laboratory of the Government Chemist and the research stations. Work on analytical methods for formulated products continues and has been extended on an international basis by the Collaborative Pesticides Analytical Committee of Europe. Co-operation between industry and official circles fostered throughout the years paved the way to the successful operation of the voluntary Approval and Pesticides Safety Precautions Schemes. Some materials were in short supply derris was cut off and alternatives were actively sought.DDT became available in 1942 and benzene hexachloride a little later. After the war parathion and other organo-phosphorus compounds were marketed; some such as schradan and demeton were taken up by plants and acted systemically. DDT and benzene hexachloride became the fore- runners of a new class of insecticides collectively called chlorinated hydrocarbons which included aldrin dieldrin and endrin. The new materials showed undreamed-of potencies against pests. Insects such as capsid bugs the apple blossom weevil and the cabbage butterfly that had earlier resisted suppression were virtually eliminated by DDT and the apple sawfly and others succumbed to benzene hexachloride. Aphids and spider mites were highly sus- ceptible to the phosphorus compounds and wireworms and other soil-inhabiting insects could be controlled by benzene hexachloride or other chlorinated hydrocarbons.The success of spring and summer sprays based on the new materials led to a decline in the use of the winter washes. Re-appraisal soon became necessary as side-eff ects began to appear. Parathion destroyed the natural predators of red spider and infestations of the mite built up from survivors of the treatment became devastating. DDT also eliminated predators of mites ; its use against codling moth was therefore discouraged by the Ministry of Agriculture until efficient acaricides such as chlorbenside became available. Unlike the medical field few instances of the acquired resistance of insects to poisons have been recorded in agriculture and horticulture although recently cabbage root fly in one area has developed a high degree of resistance to dieldrin.Some of the compounds showed high toxicities to man and under statutory regulations The coming of the Second World War brought profound changes. 74 DEVELOPMENT OF CHEMICAL CROP PROTECTION IN BRITAIN [Proc. SOC. Analyt. Chem. it is necessary to wear protective clothing and other safety measures must be taken by operators when certain scheduled materials are used. The potential risks that caused the greatest public concern however were those to the consumers of treated crops and to wildlife. DDT and dieldrin persist for long periods on crops and in soil accumulate in food chains and are known to occur in the body-fats of animals including man. Recently the restriction of certain uses of chlorinated hydrocarbons was voluntarily agreed and already there are indications that satisfactory alternatives are becoming available.The concern about residues in food has led to a vast amount of work making use of all the resources of modern analytical chemistry. The many papers in The Analyst on analytical methods for residues indicate the importance of the subject. The levels of contamination of many food commodities are known and discussions are actively taking place on an international basis on daily intakes of residues that are permissible for safety. In this country we limit residues on crops by ensuring proper treatment at the time of application and adequate periods for weathering between application and harvest. Other countries such as the United States of America concentrate on the harvested crops impose tolerances for residues and exercise analytical control.It must be remembered that conditions in this country and the United States differ radically. There more varied types of crops are grown and are harvested from one region or another throughout the year infestations of pests are more diversified severe and occur over much greater areas and greater use is made of the more potent chemicals such as parathion for pest control. Our much smaller scale of operations and comparatively simple pest problem permit a more logical and less costly approach that would be impracticable in America. With the impending decline of the chlorinated hydrocarbon insecticides greater interest is being taken in phosphorus compounds and new compounds are continually being added to the already swollen ranks of this group.The only other potential class in sight is that of the carbamates now being developed especially in the United States. Pests of foliage can be well controlled without serious side-effects by one material or another ; more attention will probably be given in the immediate future to the suppression of pests inhabiting the soil. Developments in fungicides have been less spectacular. Sulphur and copper compounds are still prominent dithiocarbamates captan dodine and dinocap have valuable uses and new compounds have recently appeared. Efforts to find a truly effective systemic fungicide have so far been unsuccessful. The most notable post-war advances have been made in herbicides and the ability to grow crops in weed-free environments has opened up new methods of crop husbandry.Hand in hand with the production of new chemicals have come improved methods for their application to crops. The rapid development of new products has considerably strained the limited resources of the official research and advisory services. Each new compound ideally should be inde- pendently assessed for its value in spray programmes. This means that much ad hoc testing has to be undertaken and the chief difficulty is to ensure that fundamental work at least keeps pace with commercial developments in the field. Our information on the inter-relationships between pest or disease organisms and their hosts is still scanty; some plants for example show a natural immunity to insects and others are singularly free from disease. A better understanding of such basic facts could be rewarding.The cost of developing a new crop protection chemical is already high. In addition to field evaluation against pests or diseases work has to be undertaken on the persistence of residues acute and chronic mammalian toxicities and risks to wildlife. To recoup the cost efficiency against a wide range of pests and the existence of a large market are needed. Selec- tivity in action permitting the control of a pest without destroying beneficial insects may well be a pipe-dream and prospects of limited use may react against the commercial develop- ment of compounds for the control of locally-important diseases. A wide spectrum of biological activity often includes high mammalian toxicity but risks to operators may be reduced by the use of new formulations such as protected granules. The difficulties that arise from the use of a toxic chemical of long persistence are now fully appreciated and it is unlikely that the experiences of the past few years will be repeated. The present reliance upon chemicals has prompted the examination of alternative methods of control. Interest is being taken in breeding plants for resistance to pests and diseases in the possibility of disseminating diseases of insects and in the use of insect sex attractants irradiation and chemo-sterilants. For the present however poisons of a conventional type must be the mainstay of crop protection.

ISSN:0037-9697    

DOI:10.1039/SA9660300071

出版商:RSC    

年代:1966

数据来源: RSC

摘要:

May 19661 THERMAL ANALYSIS 75 Thermal Analysis The following are summaries of papers presented at an Ordinary Meeting of the Thermal Analysis Group held on December 2nd 1965 and reported in the February issue of Pro- ceedings (p. 15). Coal Garbonisation Simple Thoughts on a Complex Matter BY D. FITZGERALD (Heating and Ventilating Research Association Bracknell Berks.) DR. FITZGERALD reported on the carbonisation of gram samples of coal macerals at linearly rising temperatures under vacuum. Gas samples had been regularly taken and analysed chromatographically up to C,. Results were examined kinetically on the initial assumption that each gas species was the result of a first-order decomposition of the solid material. The main conclusions were that the primary tar (known to be a brittle solid) was present in coal as such and that a reaction such as C + 2H = CH took place to a measurable extent at temperatures above the plastic zone.By making a number of assumptions on the nature of coal the observations had been used to derive a value for the number of aromatic rings in the basic coal lamella. These values agreed well with the results obtained by X-ray observations and other totally different techniques. It has also shown that the activation energy of the evolution of hydrogen in the later stages of carbonisation rose linearly with temperature. In addition Dr. Fitzgerald demonstrated that if in an Arrhenius diagram there was a reduction of slope at higher tem- perature this meant that the activation energy was increasing contrary to what was generally supposed. The analysis was as follows Suppose E = E for T 5 To and then k = k,,exp - (E,-bT + bT)/RT E = E + b(T - To) for T > To = k,exp - ((E - bT,)/RT + b/R) so that instead of E, E - bT was observed and the frequency factor was multiplied by ex-pb/R.An example was given in which E = 42,000 cal per mole up to about 820" K and after that E appeared to be 10,000 cal per mole. From this it could be readily shown that E = 42000 + 39(T-820) cal per mole. A more detailed study of this work has been reported (D. Fitzgerald and D. W. van Krevelen Fuel 1959,38 17). The Analysis of Volatile Materials by Mass-detection Gas Chromatography BY S. C. BEVAN AND S. THORBURN (Del3avlment of Chevnistvy Brunel College London W.3) THE paper was presented by Dr. Bevan who commented that the subjects of thermal analysis and gas chromatography touched at several points.One of the most interesting of these points of contact was between thermogravimetry and mass-detection gas chromato- graphy. In thermogravimetry a recording balance was used to follow the change in weight of a sample arising from loss of volatile materials during heating. In mass-detection gas chromatography a recording balance was used to follow the change in weight of an absorption vessel due to the absorption of volatile materials carried into the vessel by a stream of non- absorbed carrier gas. The volatile materials whose arrival in the absorption vessel were thus detected and quantitatively registered were the separated components of an analysis sample emerging from a gas-chromatographic column in the stream of inert carrier gas.The mass - time plots yielded by mass-detection gas chromatography consisted of a series of steps and resembled an inverted thermogravimetric curve. The location of each step on the time axis of such an integral chromatogram was characteristic of the component whilst the height of the step gave directly the absolute mass of the component. Mass detection offered some important advantages over most of the established methods of detection. Perhaps the most important in practice was that the chromatogram was integral and not differential as with other detectors with the notable exceptions of the titrimetric detector of James and Martin and the gas volumetric detector of JanBk. The James and Martin and the JanBk detectors suffered the disadvantage of being severely 76 THERMAL ANALYSIS [Proc.SOC. Analyt. Chem. restricted in application and were consequently little used. Differential chromatograms consisted of a series of peaks and generally necessitated for quantitative evaluation the integration of peak areas as well as prior calibration for every component in the sample and for different conditions of operation. Some detectors of high sensitivity such as the argon and flame-ionisation detectors assumed special importance in the analysis of scarce materials and in the determination of minor constituents. However with small samples errors independent of the detection system became critically important the introduction of a pre-determined amount of a representative sample became more difficult and the reactivity of the stationary phase might vitiate the quantitative interpretation of the chromatogram.In addition to this the inertness of the support material could no longer be presumed and the purity of the carrier gas might be more critical. High sensitivity of detection was not therefore the complete answer to the prayer of the quantitative analyst especially as the quantitative interpretation of a differential chromatogram was often far from straightforward. Dr. Bevan went on to say that the ideal differential chromatogram consisted of a constant base-line broken by a number of peaks and the area of each peak was proportional to the amount of component in the sample. Real chromatograms were not as simply evaluated as the ideal one. Most differential detectors were linear only over a limited range peaks were often unsymmetrical and even when they were symmetrical it was still a time-consuming and imprecise business to determine their areas.The most convenient methods of peak-area evaluation depended upon the recently developed automatic integrators that could be attached to recorders and that performed the integration simultaneously with the recording of the chromatogram either with digital print-out of peak areas or with the cumulative integrated area recorded as a separate trace on the chromatogram itself. Unfortunately integrators were not always perfectly reliable and were always expensive. The mass detector did away with all difficulties associated with peak-area integration and did not require calibration or prior knowledge of molecular response factors. Current work with the mass detector involved the use of activated charcoal as absorber.This material maintained at a suitable temperature made it possible to determine quantita- tively components of any chemical type and of a wide range of volatility. The detector had been used in conjunction with various columns and with column temperatures over a con- siderable range. The efficiency of absorption was high and was practically independent of flow-rate. With an electronic microbalance such as the Cahn R. G. Electrobalance or the E.M.B.l (made by Research and Industrial Instruments Company) of lo-' g sensitivity quantitative analysis could be achieved with samples of 1 plitre or less such as were commonly used in gas chroma- tography with the gas-density detector or katharometer. An interesting development resulting from the availability of the mass detector was the possibility of measuring molecular weights by gas chromatography.By combining the mass detector in series with a gas-density detector a dual chromatogram was obtained from a single gas-chromatographic analysis on a single sample. The mass integram consisted of steps whose heights corresponded to the masses of the components. The other chromato- gram that given by the gas-density detector yielded peaks whose areas were a function not only of the masses of the components but of their molecular weights as well. It was therefore possible in principle to work out the molecular weights of all the components provided the peak area and step height were known for one component of known molecular weight. The availability of a knowledge of molecular weight as well as the retention value went a long way towards identification of a component.Dr. Bevan concluded by saying that the successful application in the field of gas chro- matography of a recording microbalance to the quantitative assessment of absorbable vapours carried by a stream of inert carrier gas suggested the possibility of a modification of conventional thermogravimetry in which the balance was applied not to the task of following the change in weight of the sample itself but to the recording of the gain in weight of an absorption vessel in an adjacent constant-temperature compartment. This modification would make possible readier control of sample temperature more convenient measurement of sample temperature and would eliminate errors due to buoyancy and convection which had to be taken into account when the weight of the sample itself was being recorded. The lecture concluded with Mr. Thorburn discussing a selection of slides showing the results ob- tained by this interesting and elegant technique. As absorption was rapid the effective volume of the detector was small.

ISSN:0037-9697    

DOI:10.1039/SA9660300075

出版商:RSC    

年代:1966

数据来源: RSC

摘要:

77 May 19661 REPORT OF THE ANALYTICAL METHODS COMMITTEE 1965 Report of the Analytical Methods Committee 1965 THIS tenth Report of the Analytical Methods Committee of the Society for Analytical Chemistry reviews the progress of work during 1965. ANALYTICAL METHODS COMMITTEE Chairman D. C. Garratt Ph.D. D.Sc. Hon.M.P.S. F.R.I.C. (Scientific A dviser Pharmaceutical Society of Great Britain) A. J. Amos O.B.E. B.Sc. Ph.D. F.R.I.C. E. Bishop BSc. A.R.C.S.T. F.R.I.C. W. A. Broom B.Sc. F.R.I.C. S. G. Burgess B.Sc. Ph.D. F.Inst.Pet. F.Inst.S.P. J . H. Hamence M.Sc. Ph.D. F.R.I.C. F.R.I.C. N. W. Hanson BSc. Ph.D. F.R.I.C. W. C. Johnson M.B.E. F.R.l.C. E. Q. Laws B.Sc. F.R.I.C. D. T. Lewis C.B. Ph.D. D.Sc. F.R.I.C. G. W. C. Milner D.Sc. A.Inst.P. F.R.I.C. R. F. Milton B.Sc. Ph.D. M.I.Biol. F.R.I.C.S. A. Price B.Sc. F.R.I.C. A. A. Smales C).B.E. D.Sc. F.R.I.C. S. G. E. Stevens B.Sc. F.R.I.C. C. Whalley BSc. F.R.I.C. K. A. Williams B.Sc. Ph.D. A.Inst.P. M.Inst.Pet. F.R.I.C. Analytical and Consulting Chemist Umivevsity of Exetev (Senior Lecturev Department Formerly Technical A dviser Nicholas Products Scienti3c Adviser Greatev London Council of Chemistvy) Ltd. Public Analyst OfJicial Agvicultuval Analyst and Consulting Chemist Industrial Chemist Reseavcla t- Development Department Impevial Chemical Industries Ltd. Technical Divector Hopkin and Williams Ltd. Pvincipal Scientific Oficev Ministry of Tech- nology Laboratory of the Government Chemist Govevnment Chemist Ministvy of Technology (Honovavy Tveasurer of the Society) Group Leader A .E.R.E. Harwell Analytical and Consulting Biochemist Head of Microbiological Section Vitamins Ltd.(Honovary Secvetavy of the Society) Deputy Chief Scientist Chemistvy Division and Head 0-f Analytical Chemistry Branch A.E.R.E. Harwell (Pvesident of the Society) Head of Analytical and Control Department Smith Kline and French Laboratories Ltd. Chief Analyst and Assistant Research Manager Laporte Chemicals Ltd. Analytical and Consulting Chemist Secretary P. W. Shallis GENERAL REVIEW Dr. D. W. Kent- Jones whose membership of the Committee began several years before the re-organisation in 1955 resigned during the year. It was during his term of office as President of the Society that the first moves towards setting up the permanent Secretariat of the Committee were made and he personally conducted the first appeal to industry for funds for this purpose.His link with the Committee will not however be entirely severed since he is to continue as a Trustee of the Trust Fund. The Committee extends its grateful thanks to Dr. Kent-Jones for his services and all he has achieved on its behalf and also wishes him well in his forthcoming retirement. Two other members-Mr. A. G. Jones and Mr. R. M. Pearson-resigned during the year and the Committee gratefully acknowledges their work on its behalf. PROGRESS OF WORK- The publication in The AvtaZyst in May of the Report on “Sodium Carbonate as a Primary Standard in Acid - Base Titrimetry” marked the successful completion of the first part of the Analytical Standards Sub-committee’s programme of work. This Sub-committee was set up in 1960 in response to a request from I.U.P.A.C.for an investigation to be carried out on existing and proposed titrimetric standards with a view to recommending a suitable substance for use as a primary standard in acid - base titrimetry. The Report of the Sub-committee embodying the recommendation of sodium carbonate as a primary titrimetric standard was sent to I.U.P.A.C. and was considered at its Paris Conference in July; details of any action to be taken by I.U.P.A.C. are awaited. The Sub-committee is currently investigating sul- phamic acid as a possible complementary standard to sodium carbonate. In March Dr. N. W. Hanson was appointed a member of the Committee. 78 REPORT OF THE ANALYTICAL METHODS COMMITTEE 1965 [PrOc. sot. Analyt. Chew. In its Report on “The Determination of Small Amounts of Mercury in Organic Matter’’ published in the September issue of The Analyst the Metallic Impurities in Organic Matter Sub-committee has made use in preparing the sample of the apparatus previously recom- mended for the controlled oxidation of organic matter with mixed nitric perchloric and sul- phuric acids (Analyst 1960 85 643).Although the recommended wet-oxidation procedure employs only nitric and sulphuric acids use of this apparatus removes the possibility of loss After destruction of the organic matter a two-stage dithizone extraction procedure is applied with subsequent spectrophotometric measurement. Details of the considerable number of collaborative investigations undertaken on all stages of the procedure are given in the Report. The Sub- Committee has become aware during the year of the possible advantages attending the use of 50 per cent.hydrogen peroxide in the destruction of organic matter but little has as yet been published on this subject. A request for information from analysts having experience with this reagent is to be published in PYoceedings and it is hoped that eventually the Sub-Commit- tee will be in a position to recommend its use in a supplement to its earlier Report on methods for the destruction of organic matter. When in 1962 the Additives in Animal Feeding Stuffs Sub-committee was disbanded on the completion of the work of most of its Panels the Prophylactics Panel still had work in hand. This Panel was reconstituted as a Sub-committee of the A.M.C. under the title of the Prophylactics in Animal Feeds Sub-committee and its latest Report on the determination of sulphaquinoxaline appeared in the September issue of The Analyst.There are still many drugs for which recommended methods of assay are required and the assistance of the Ministry of Agriculture Fisheries and Food a t whose request this work was undertaken in suggesting an order of priorities for the remaining drugs has been sought. Three short Reports from the Meat Products Sub-committee were published in The Analyst during the year. In one of these the Sub-committee has revised its previously recommended correction to be applied in the analysis of sausages and some other products for the nitrogen content of rusk filler. Changes in milling practice and certain other factors are known to affect the protein content of flour used in the manufacture of rusk fillers and for this reason the Sub-committee intends to keep the situation constantly in mind.The other two published Reports gave recommended nitrogen factors for veal and turkey and work is in hand on the collection of similar figures for mutton tongue kidney and pigs’ blood. When this current work is complete the Sub-committee will have established nitrogen factors for all the important types of meat used in the manufacture of food products. About a year ago the Committee’s attention was drawn to the lack of standardisedmethods for determining fluorine at all levels. A published request for information from analysts who even if only occasionally carried out fluorine determinations evoked a good response which established that there was a distinct need for standardised methods. Consequently the Fluorine Sub-committee has been set up and details of its constitution and terms of reference will be found on p.82. This new Sub-committee realised that its ultimate aims will not be easily or quickly achieved; however the first stage of its work-investigation of the available methods for the final determination of fluorine in solution-has been enthusiastically begun. Consideration was given during the year to the proposed publication of a Second Edition of “Official Standardised and Recommended methods of Analysis.” This book contains an edited collection of all the Committee’s recommended methods of analysis and a compre- hensive classified bibliography up to early 1963 when it was published. It has been decided that a Supplement containing all the Committee’s methods of analysis published since the appearance of the First Edition information to bring the bibliography up to date and an index covering the First Edition and the Supplement should be prepared for publication in early 1967; consideration would then be given to the publication of a Second Edition after a further suitable interval.The Committee is pleased to record that Mr. S. C. Jolly who collected and edited the First Edition of the book has undertaken to prepare the Supplement. The work of the other Sub-Committees is progressing satisfactorily. Notably a collection of critical appraisals of the first 30 methods of particle sizing listed in the Particle Size Analysis Sub-Committee’s published Classification (Analyst 1963 88 156) is now nearly complete and it is hoped that it will be published as a separate monograph in 1966.Other groups of methods will then be dealt with similarly. The Fish Products Sub-committee has completed its collection of values for the nitrogen content of cod flesh and a Report has been prepared ’ of mercury by volatilisation and this has been checked radiochemically. May 19661 REPORT OF THE ANALYTICAL METHODS COMMITTEE 1965 79 for publication. During its work this Sub-committee has confirmed the seasonal variations in nitrogen content of cod reported by other workers but members have been rather surprised to find that the over-all variation in nitrogen content has proved to be considerably less than they had expected. Considerable progress in the work of the Panels of the Joint Committee with the Pharma- ceutical Society was achieved during the year.The Joint Committee which was originally formed to recommend as required methods of assay for crude drugs has now realised that it has a useful function to perform in a broader field and has consequently widened its terms of reference to include all drugs. The Joint Committee has also changed its title to indicate its increased scope and is now known as the Joint Committee of the Pharmaceutical Society and the Society for Analytical Chemistry on Methods for the Evaluation of Drugs. One new Panel has been formed during the year and its aim is to recommend a thin-layer chromatographic procedure which it is hoped will prove suitable to replace the paper-chroma- tographic test currently specified in the British Pharmacopoeia for limiting the presence of foreign steroids in corticosteroids.This Panel began its work in October and details of its constitution and terms of reference will be found on p. 89. The Anthraquinone Panel’s work on senna was completed during the year and its Report on “The Chemical Assay of Senna Fruit and Senna Leaf’’ was published in the October issue of The Analyst. The recommended method assays the total anthraquinone glycosides content of the sample and comparison of the results with those obtained biologically on the same samples shows that both methods place the samples in the same order of potency. This Panel is now to carry out work aimed at recommending a chemical method for assaying cascara but as no suitable animal response to cascara has been found there is no immediate prospect of directly relating this work to the biological activity of the drug.A thin-layer chromatographic method that can be used for assessing the tri-iodothyronine content of a sample of thyroid has been developed by the Thyroid Panel based on the work of one of its members By using this procedure the Panel has successfully placed 10 samples of thyroid in the same order of potency as does the rat anti-thiouracil goitre method of bio- assay. Individual progress reports for all the Sub-Committees and Panels together with their constitution will be found on pp. 79 to 89. ANALYTICAL METHODS TRUST- The number of organisations that gave donations to the Trust Fund during the year was 27 and the total amount received was l2221 which is approximately E700 less than in 1964. ANNUAL ACCOUNTS- The audited statement of accounts for the year ended October 31st 1965 is shown in Appendix I and a list of subscribers to the Trust Fund during the year is given in Appendix 11.A Report for publication is at present being prepared. REPORTS OF SUB-COMMITTEES OF THE ANALYTICAL METHODS COMMITTEE ANALYTICAL STANDARDS SUB-COMMITTEE CONSTITUTION- E. Bishop B.Sc. A.R.C.S.T. F.R.I.C. (Chairman) University of Exeter (Department of Chemistry) S. Andrus F.R.I.C.* Laporte Chemicals Ltd. K. Archer B.Sc.T Fuller’s Earth Union Ltd. P. R. W. Baker M.Sc. A.R.I.C. Wellcome Research Laboratories A. G. Hill F.R.I.C. British Drug Houses Ltd. R. M. Pearson F.R.1.C.f Imperial Chemical Industries Ltd. (Agricultural J. M. Skinner BSc. Ph.D. F.R.I.C. Imperial Chemical Industries Ltd. (Agricultural W. I. Stephen B.Sc. Ph.D. F.R.I.C.University of Birmingham (Department of J. T. Yardley B.Sc. F.R.I.C. P. W. Shallis (Secretary) Division) Division) Chemistry ) Hopkin & Williams Ltd. * Resigned March 1965. t Appointed July 1965. Corresponding member 80 REPORT OF THE ANALYTICAL METHODS COMMITTEE 1965 [Proc. SOC. Analyt. Chem. TERMS OF REFERENCE-“TO examine existing analytical standards and to select suitable substances .” PROGRESS OF WORK- As a result of collaborative investigations extending over a period of 4 years the Sub- Committee has concluded that sodium carbonate is a suitable substance for use as a primary standard in acid - base titrimetry. During the investigations samples of sodium carbonate from several sources were assayed and although it was not practicable to examine samples from every known source of supply it was found that the analytical-reagent grade material marketed by one commercial organisation assayed within the limits prescribed by the Sub- Committee for a primary standard i.e.purity within the range 100 & 0.02 per cent. It was subsequently found that by applying a simple purification procedure on analytical-reagent grade sodium hydrogen carbonate as starting material sodium carbonate that also met the Sub-committee’s requirements could be prepared. Full details of this work are included in the Sub-committee’s Report on “Sodium Carbonate as a Primary Standard in Acid - Base Titrimetry,” which was published in the May issue of The Analyst. This Report was also submitted to I.U.P.A.C. at whose request the work was undertaken and details of any action to be taken by the International Union are awaited.Currently the Sub-committee is carrying out a parallel investigation on the suitability of sulphamic acid for use as a primary titrimetric standard. Some samples of sulphamic acid purified in the laboratory by a simple procedure have been examined and all of them met the Sub-committee’s requirements. To test the reproducibility of the purification procedure three further samples were prepared in different laboratories two of these have proved satisfactory but the third which had a different crystal size from the other two did not. The laboratory that prepared this faulty sample is now attempting to produce an acceptable one and possible reasons for the failure are being explored. ESSENTIAL OILS SUB-COMMITTEE CONSTITUTION- G. W. Ferguson B.Sc.Ph.D. F.R.I.C. (Chairman) H. E. Brookes B.Sc. F.R.I.C. K. Field M.Sc. Ph.D. J. H. Greaves B.Sc. F.R.I.C. H. T. Islip B.Sc. F.R.I.C.” B. D. Masters W. S. A. Matthews A.R.I.C. T. L. Parkinson B.Sc. Ph.D. F.R.I.C.1. Miss H. M. Perry M.Sc. F.R.I.C. J. H. Seager M.Sc. F.R.I.C. C. A. Slater B.Sc. Ph.D. A.R.C.S. F.R.I.C. S. G. E. Stevens B.Sc. F.R.I.C. B. D. Sully B.Sc. Ph.D. A.R.C.S. F.R.I.C. P. W. Shallis (Secretary) Analytical and Consulting Chemist Boots Pure Drug Co. Ltd. Ministry of Technology Laboratory of the Proprietary Perfumes Ltd. Formerly Tropical Products Institute W . J . Bush & Co. Ltd. Ministry of Overseas Developnzent Tropical Products Institute Formerly Beecham Foods Ltd. Stafford Allen & Sons Ltd. Yardley G. Co. Ltd. Schweppes (Home) Ltd. Smith Kline & French Laboratories Ltd.A . Boake Roberts & Co. Ltd. Government Chemist * Resigned November 1965. t Resigned April 1965. TERMS OF REFERENCE-“TO examine new methods of analysis applicable to the study of essential oils and to develop techniques for the determination of their more important con- stituents.” PROGRESS OF WORK- The Sub-committee has continued during the year with its collaborative investigation of the application of gas - liquid chromatography to the analysis of essential oils. Work has been carried out on oils of peppermint and lavandin and by rigorously standardising the conditions under which the chromatograms are run it has been possible in nine laboratories to record May 19661 81 remarkably similar chromatograms for these oils especially with regard to the major peaks.The possibility of devising idealised chromatograms that would be useful in the identification of genuine samples of these oils is now being considered. The quantitative application of gas chromatography is also currently under investigation and the Sub-committee hopes eventually to be able to recommend a gas-chromatographic method for determining cineole in essential oils. A preliminary investigation to discover conditions under which cineole can be separated from limonene on a gas-chromatographic column has been successfully completed and attempts are now being made to separate cineole quantitatively from a known four-component mixture. Other work being carried out is an investigation of the possible application of Dr. Sully's stearoylation method (Analyst 1962,87,940) to essential oils containing as major constituents primary and secondary alcohols or phenols.A Report of the Sub-committee's earlier investigation of the Demetrius and Sinsheimer method for determining eugenol has been accepted for publication and is expected to appear in The Analyst early in 1966. REPORT OF THE ANALYTICAL METHODS COMMITTEE 1965 FISH PRODUCTS SUB-COMMITTEE CONSTITUTION- S. M. Herschdoerfer Ph.D. F.R.I.C. F.I.F.S.T. T. Wall & Sons (Ice Cream) Ltd. M. R. S . H. (Chairman) J. H. Bushill D.Sc. F.R.I.C. F.R.S.H. (Deputy W. C. A. Wise B.Sc. A.R.I.C.) P. J. Cooper BSc. A.R.I.C." Ministry of Technology Laboratory of the C. L. Cutting B.Sc. Ph.D. F.R.I.C. British Food Manufactuving Industries Research J. R. Fraser B.Sc. A.C.G.F.C. F.R.1.C.t Ministry of Technology Laboratory of the B.J. Hasberry B.Sc. A.R.S.H. (Deputy D. J. Ward) Birds Eye Foods Ltd. W. T. Little B.Sc. Ph.D. Unilever Research Laboratory (Colwovth) J . A. Lovern Ph.D. D.Sc. F.R.S.E. F.R.I.C. Ministry of Technology Torry Research Station T. McLachlan D.C.M. A.C.G.F.C. M.I.Biol. Public Analyst P. W. Shallis (Secretary) J . Lyons & Co. Ltd. Government Chemist Association Government Chemist F.R.I.C. F.I.F.S.T. F.R.S.H. * Appointed August 1965. Resigned June 1965. TERMS OF REFERENCE-" (a) 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- The collection of analytical results for the nitrogen content of cod flesh was completed during the year and the Sub-committee thanks the interested organisations that have assisted in this task.A total period of some 21 months has been covered and this has enabled the Sub-committee to substantiate the seasonal variations in nitrogen content observed by some previous workers in this field. A Report of this work embodying the recommendation of an average nitrogen factor of 2.85 for use in the analysis of cod products has been prepared and publication is expected during the first half of 1966. Early during the programme of work on cod the possibility of using the non-protein nitro- gen content of the fish for calculating the amount of it present in a product was investigated.This value was however found to be particularly variable and it was concluded that no reliance could be placed on the non-protein nitrogen figure as a measure of fish content. Work is currently in hand on methods for determining milk protein in manufactured fish products such as fish cakes. Before further work on establishing nitrogen factors for fish species is undertaken the Sub-committee is awaiting information on a possible alternative method-not based on total nitrogen-for determining the fish content of a manufactured product. 82 CONSTITUTION- REPORT OF THE ANALYTICAL METHODS COMMITTEE 1965 [Proc. SOC. AnaZyt. Chem. FLUORINE SUB-COMMITTEE T. R. F. W. Fennell B.A. (Chaivman) E. J. Dixon B.Sc. Ph.D. A.R.I.C. H. A. Foner B.Sc. A.R.I.C. J. K. Foreman B.Sc. F.R.I.C.G. S. Goff Ministvy of Aviation Royal Aivcvaft Establish- ment Ministry of Technology Labovatory of the Government Chemist University of Leeds Houldswovth School of Applied Science U . K.A .E.A . Production Group Lincoln Electric Co. Ltd. H. Green L.R.I.C. R. J. Hall F.I.M.L.T. Ministry of Agriculture Fisheries & Food W. C. Hanson F.R.I.C. R. F. Milton B.Sc. Ph.D. M.I.Biol. F.R.I.C. E. J. Newman B.Sc. Ph.D. F.R.I.C. British Cast Iron Research Association National Agricultural A dvisory Service Fisons Fertilisers Ltd. Analytical and Consulting Biochemist Hopkin G. Williams Ltd. J . M. Skinner B.Sc. Ph.D. F.R.I.C. R. Waspe B.Sc. P. W. Shallis (Secretavy) Imperial Chemical Industries Ltd. (Agricultural Division) Laporte Acids Ltd. TERMS OF REFERENCE-"TO investigate methods for determining fluorine and to recommend standardised methods for its determination at all levels in both organic and inorganic materials." PROGRESS OF WORK- Replies received to a published request for information indicated a distinct need for standardised methods for determining fluorine in organic and inorganic materials at all levels.In consequence the Sub-committee was set up during the year and held its first meeting in October . As the first stage of its work the Sub-committee has decided to investigate methods for the determination of fluorine in solution and when this stage has been completed will consider methods for the preparation of the solution. Work in the first stage is to be undertaken by two groups one dealing with the determination of milligram amounts and the other with microgram amounts of fluorine in the final solution.MEAT PRODUCTS SUB-COMMITTEE CONSTITUTION- S. M. Herschdoerfer Ph.D. F.R.I.C. F.I.F.S.T. T . Wall & Sons (Ice Cream) Ltd. S . Back B.Sc. F.R.I.C. M. R.S. H . (Chaivman) Cvosse G. Blackwell Ltd. P. J . Cooper B.Sc. A.R.I.C.* Mivzistry of Technology Labovatory of the Government Chemist P. 0. Dennis B.Sc. F.R.I.C. J. R. Fraser B.Sc. A.C.G.F.C. F.R.I.C.I. Ministity of Technology Laboratovy of the H. C. Hornsey F.R.I.C. A. J. Kidney BSc. Ph.D. A.R.C.S. A.R.I.C. R. A. Lawrie B.Sc. Ph.D. F.R.I.C. T. McLachlan D.C.M. A.C.G.F.C. M.I.Biol. Public Analyst F.R.I.C. F.I.F.S.T. F.R.S.H. A. McM. Taylor B.Sc. Ph.D. F.R.I.C. E. F. Williams O.B.E. M.A. F.R.I.C. P. W. Shallis (Secretary) 0 x 0 Ltd. Government Chemist J . Sainsbuvy Ltd. T . Wall & Sons (Meat and Handy Foods) Ltd.University of Nottingham (Department of Agri- cultural Sciences) Bvitish Food Manufacturing Industvies Research J . Sainsbury Ltd. A ssociation * Appointed August 1965. 7 Resigned June 1965. May 19661 83 TERMS OF REFERENCE-“(a) The determination of the meat content of products containing meat; (b) the determination of the constituents of meat and meat products.” NoTE-“The term ‘meat products’ to include hydrolysed protein.” PROGRESS OF WORK- Three Reports from the Sub-committee were published in The Analyst during the year. These were “Nitrogen Factor for Veal,” “Nitrogen Factors for Turkey” and “Nitrogen Content of Rusk Filler,” the last named being the result of a re-assessment of the Sub-committee’s earlier recommended figure (Analyst 1961,86,560).As changes in milling practice and other factors tend to cause variations in the protein content of flour used for rusk making the Sub-committee will keep its latest recommended correction constantly under surveillance. The collection of analytical results for the nitrogen contents of mutton kidney tongue and pigs’ blood (used in the manufacture of black pudding) is well advanced and it is possible that Reports on all of them will be published in 1966. When this work is completed the Sub- committee will have recommended nitrogen factors for all the important meats and offals used in manufactured products. Attention is now to be directed towards investigating methods for determining non-meat protein in meat products. Some methods are currently being examined that may prove suitable for application to cooked products.REPORT OF THE ANALYTICAL METHODS COMMITTEE 1965 METALLIC IMPURITIES IN ORGANIC MATTER SUB-COMMITTEE CONSTITUTION- W. C. Johnson M.B.E. F.R.I.C. (Chairman) J. C. Gage B.Sc. Ph.D. F.R.I.C. Imperial Chemical Industries Ltd. (Industrial T. T. Gorsuch B.Sc. Ph.D. A.R.I.C. R. A. Hoodless B.Sc. Ph.D* Ministry of Technology Laboratory of the Government Chemist Miss E. M. Johnson M.Sc. A.R.I.C. British Food Manufacturing Industvies Research Association H. W. Liebmann Dr. Phil. F.R.1.C.t Metal Box Co. Ltd. R. F. Milton B.Sc. Ph.D. M.I.Biol. F.R.I.C. Analytical and Consulting Biochemist E. J. Newman B.Sc. Ph.D. F.R.I.C. Hopkin & Williams Ltd. W. L. Sheppard M.Sc. F.R.I.C.1 The Crookes Laboratories Ltd. G. B. Thackray B.Sc. F.R.I.C. Staffordshire County Council J.F. C. Tyler BSc. Ph.D. F.R.I.C.5 Ministry of Technology Labovatory of the Govern- P. W. Shallis (Secretary) Hopkin & Williams Ltd. Hygiene Laboratories) U.K.A.E.A . The Radiochemical Centre ment Chemist * Appointed November 1965. t Appointed September 1965. 1 Resigned August 1965. 3 Resigned November 1965. TERMS OF REFERENCE-“TO investigate the determination of small quantities of metals in organic matter.” PROGRESS OF WORK- The Report of the Sub-committee on “The Determination of Small Amounts of Mercury in Organic Matter” was published in the September issue of The Analyst. In this Report details of the collaborative investigations of all stages of the recommended method are given together with full details of the method itself. A notable feature of the recommended method is that the wet oxidation of the organic matter with sulphuric and nitric acids is carried out in an apparatus that avoids loss of mercury by volatilisation.Collaborative work is now in hand on methods for determining tin and cadmium. For tin a dithiol method and an as yet unpublished method involving the use of catechol violet are being investigated and for cadmium a polarographic method and a dithizone method are under consideration. In view of the increasing popularity of the use of 50 per cent. hydrogen peroxide in conjunction with sulphuric acid for the wet oxidation of organic matter the Sub-committee is considering the possibility of issuing a supplement to its earlier Report on “Methods for the 84 REPORT OF THE ANALYTICAL METHODS COMMITTEE 1965 [Proc.SOC. AnaZyt. Chem. Destruction of Organic Matter” (Analyst 1960 85 643) giving details of the use of this sub- stance. Details of the substances to which it has been applied and of the method of use are currently being sought from analysts who have experience in the use of 50 per cent. hydrogen peroxide and some useful information has already been collected. PARTICLE SIZE ANALYSIS SUB-COMMITTEE CONSTITUTION- E. Q. Laws B.Sc. F.R.I.C. (Chairman) Ministry of Technology Laboratory of the T. Allen M.Sc. Bradford Institute of Technology R. de B. Ashworth M.Sc. Ph.D. F.R.I.C. Ministry of Agriculture Fisheries and Food Plant Pathology Laboratory D. G. Beech Ph.D. British Ceramic Research Associatioiz V. T. Crowl B.Sc. Ph.D. F.R.T.C. A.R.C.S. D.I.C. Paint Research Station I. C. Edmundson B.Pharm.Glaxo Laboratories Ltd. C. G. L. Furmidge B.Sc. Ph.D. F.R.I.C. “Shell” Research Ltd. H. Heywood Ph.D. Woolwich Polytechnic H. W. Hibbott M.Sc. Ph.D. F.R.I.C. D. R. Collins Ltd. J. F. Hinsley F.I.M. F.1nst.P. Edgar Allen & Co. Ltd. R. Howes B.Sc. Chesterford Park Reseavch Station B. Scarlett M.Sc. Loughborough College of Technology D. C. Soul M.Sc. F.R.I.C. A.R.C.S. Welwyn Hall Research Association P. W. Shallis (Secretary) Government Chemist TERMS OF REFERENCE-“TO study methods of particle size analysis to survey available instru- ments and to evaluate them with regard to their principles of operation and fields of application.” PROGRESS OF WORK- Work has continued during the year on the not inconsiderable task of preparing and editing critical appraisals of the individual methods of particle sizing.A small editorial panel of the Sub-committee is carrying out the initial collection and editing of these appraisals which have been prepared mainly by members of the Sub-committee although for those methods unfamiliar to members some outside help has been sought. The first group of appraisals covering the first 30 methods in the Sub-Committee’s “Classification of Methods for Determining Particle Size” (Analyst 1963,88 156) is now approaching completion and it is hoped that it will be published as a separate monograph in 1966. Comparison of the individual methods by means of collaborative investigations sponsored by the Sub-committee has continued during the year but progress in this phase of the work is steady rather than rapid. Nevertheless the Sub-committee extends its grateful thanks to the many organisations not represented among its members that are taking part in these investigations.Sufficient results on a standard silica powder have now been obtained by some methods to permit a statistical evaluation and this is currently being carried out. PROPHYLACTICS IN ANIMAL FEEDS SUB-COMMITTEE CONSTITUTION- S. G. E. Stevens B.Sc. F.R.I.C. (Chairman) N. C. Brown M.A. B.Sc. A.R.I.C. P. J . Cooper B.Sc. A.R.I.C. Ministry of Technology Laboratory of the G. Drewery B.Sc. F.R.I.C. A. W. Hartley F.R.I.C. D. H. Mitchell B.Sc. R. S. Hatfull F.R.I.C. M.R.S.H. J. A. Stubbles B.Sc. D. C. Thomas M.Sc. P. W. Shallis (Secretary) Smith Kline & French Laboratories Ltd. Coopev Technical Bureau Govevnment Chemist Merck Sharp & Dohme Ltd.Sflillers Ltd. Wellcome Chemical Works Kent County Council May & Baker Ltd. Unilever Ltd. May 19661 REPORT OF THE ANALYTICAL METHODS COMMITTEE 1965 85 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- Difficulties associated with the extraction of certain drugs from animal feeds have somewhat restricted the progress made by the Sub-committee during the year. Results obtained by the Sub-committee’s method for determining acinitrazole were not entirely satisfactory and an alternative method has been investigated and has been found to give marginally better results in certain circumstances; a Report of this work is being prepared.Collaborative investigations on dimetridazole Zoalene and ethopabate are still in hand. The Sub-committee’s Report on “The Determination of Sulphaquinoxaline” appeared in the September issue of The Analyst. PUBLICATIONS SUB-COMMITTEE CONSTITUTION- D. C. Garratt Ph.D. D.Sc. Hon.M.P.S. F.R.I.C. A. J . Amos O.B.E. B.Sc. Ph.D. F.R.I.C. J . B. Attrill M.A. F.R.I.C. J . H. Hamence M.Sc. Ph.D. F.R.I.C. S. G. E. Stevens B.Sc. F.R.I.C. S. C. Jolly B.Sc. B.Pharm. M.P.S. F.R.I.C. Assistant Director Department of Pharma- ceutical Sciences Pharmaceutical Society of Great Britain Chairman Analytical Methods Committee Member A nalytical Methods Committee Editor The Analyst Member Analytical Methods Committee Member Analytical Methods Committee (Chairman) (Secretary and Editor) PROGRESS OF WORK- In order to bring up to date the first edition of “Official Standardised and Recommended Methods of Analysis,” published in 1963 a Supplement is to be published in the first half of 1967 and work on this began during the year.The Supplement will contain all the Com- mittee’s recommended methods of analysis published since the appearance of the first edition information to bring the bibliography up to date and an index both to the first edition of the book and the Supplement. It is intended that a second edition of the book will then be prepared for publication after a further suitable time interval. REPORT OF THE P.S.-S.A.C. JOINT COMMITTEE ON METHODS FOR THE EVALUATION OF DRUGS MAIN COMMITTEE CONSTITUTION- K. R. Capper Ph.D. B.Pharm. F.P.S. D.I.C. Pharmaceutical Society of Great Britain F.R.1 .C.(Chairman) J . Allen F.R.I.C. T. C. Denston B.Pharm. J. W. Fairbairn B.Sc. Ph.D. F.P.S. F.L.S. F.RI.C. University of London (Professor of Phavma- A. J. Feuell B.Sc. Ph.D. A.R.I.C. Ministry of Overseas Development Tropical British Drug Houses Ltd. British Pharmacopoeia Commission cognosy ) Products Institute D. C. Garratt Ph.D. D.Sc. I-Ion.M.P.S. F.R.I.C. Chairman Analytical Methods Committee of the S.A.C. C. A. Johnson B.Sc. B.Pharm. F.P.S. F.R.I.C. W. Mitchell B.Sc. Ph.D. F.R.I.C. H0n.M.P.S. R. F. Phipers B.Sc. Ph.D. F.R.I.C. J . M. Rowson M.Sc. Ph.D. F.P.S. F.L.S. P. W. Shallis (Secretary) British Pharmacopoeia Commission StajScord Allen & Sons Ltd. Cooper Technical Bureau Bradford Institute of Technology (Professor of Pharmacy) TERMS OF REFERENCE-“TO prepare standard methods for the evaluation of drugs their preparations and of kindred materials.” 86 REPORT OF THE ANALYTICAL METHODS COMMITTEE 1965 [PYOc.SOC. AnaZyt. chem. PROGRESS OF WORK- The year under review has seen the setting up of one new Panel which will undertake a large programme of work aimed at eventually recommending a thin-layer chromatographic method for limiting the content of foreign steroids in corticosteroids. It is hoped that the test to be recommended by this Panel will prove suitable as a replacement for the paper-chromato- graphic test that is at present official in the British Pharmacopoeia. The Report of Panel 3 (Anthraquinone Drugs) on “The Chemical Assay of Senna Fruit and Senna Leaf’’ was published in the October issue of The Analyst.This marked the success- ful completion of several years of collaborative effort by the Panel to standardise the pro- cedural details of a chemical method for determining the total anthraquinone glycosides content of samples of senna pod and senna leaf. The results obtained by the Panel’s recom- mended method showed good correlation with bioassay results on the same samples carried out by the associated Panel 3A and details of the work of this Panel are included in the published Report. Progress was maintained in the work of the other Panels during the year and Panel 7 (Thyroid) which was set up to devise a chemical method for determining the pharmacologi- cally-active constituents of thyroid is within sight of its objective. The Joint Committee is currently considering some suggestions for the formation of further Panels.PANEL 3 ANTHRAQUINONE DRUGS CONSTITUTION- J . M. Rowson M.Sc. Ph.D. F.P.S. F.L.S. C. Daglish B.Pharm. Ph.D. M.C.I.C. F.P.S. J. W. Fairbairn B.Sc. Ph.D. F.P.S. F.L.S. Miss B. Gartside B.Pharm. M.P.S. C. A. Johnson BSc. B.Pharm. F.P.S. F.R.I.C. Miss H. M. Perry M.Sc. F.R.I.C. H. A. Ryan B.Sc. F.R.I.C. K. V. Swann B.Sc. F.R.I.C. P. W. Shallis (Secretary) (Chazrman) A.R.I.C.* F.R.I.C. Bradford Institute of Technology (Professor of Pharmacy) Reckitt G. Sons Ltd. University of London (Professor of Pharma- Pharmaceutical Society of Great Britain British Pharmacopoeia Commission Staflord Allen G. Sons Ltd. Westminster Laboratories Ltd. Allen G. Hanburys Ltd. cognosy ) * Appointed October 1965. 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- The Panel began its work in 1956 with a collaborative investigation of Kussmaul and Becker’s method as modified by Fairbairn and Michaels for determining sennosides in senna fruit.Early work was concentrated on the extended procedure for determining only the carboxylic (rhein) glycosides but experience later showed that the refinements of this pro- cedure were unnecessary for measurement of purgative activity of senna fruit or leaf and consequently attention was turned to the less complex assay of total anthraquinone glycosides. Standardisation of conditions at the various stages of this procedure enabled all members of the Panel to return concordant results for the assay of samples of Alexandrian and Tinnevelly pod and leaf.Good correlation of these results with bioassay results on the same samples provided by Panel 3A was also achieved. Reports of the work of both Panels together with full details of the recommended chemical method of assay were published under the title “The Chemical Assay of Senna Fruit and Senna Leaf” in the October 1965 issue of The Analyst. Work is now in hand aimed at eventually recommending a chemical method for assaying cascara and its preparations. Preliminary work to gain experience in the type of assay pro- cedure that will be required for cascara is being undertaken on purified barbaloin and on aloes by the method described by Fairbairn and Simic ( J .Pharm. Pharmacol. 1963 15 325). May 19661 87 When this work has been completed an investigation of a published method for determining separately the aloins and O-glycosides of cascara and of its dry extract (Fairbairn and Simic J . Pharm. Pharmacol. 1964 16 450) will be undertaken. REPORT OF THE ANALYTICAL METHODS COMMITTEE 1965 PANEL 3A ANTHRAQUINONE DRUGS (BIOLOGICAL ASSAY) CONSTITUTION- K. L. Smith M.P.S. (Chairman) 13. T. Brittain B.Pharm. Ph.D. M.P.S. M.I.Bio1. J . W. Fairbairn B.Sc. Ph.D. F.P.S. F.L.S. University of London (Professor of Pharnza- G. A. Stewart B.Sc. Ph.D. A.R.I.C. P. W. Shallis (Secretary) Boots Pure Drug Co. Ltd. Allen & Hanburys Ltd. F.R.I.C. c ogn osy ) Wellcome Biological Control Laboratories TERMS OF REFERENCE-“TO study biological methods for the assay of anthraquinone drugs.” PROGRESS OF WORK- During the year the Panel completed its collaborative bio-assays of the same samples of senna pods and senna leaf that had been examined by Panel 3 by its proposed chemical method.The bioassay results and brief details of the Panel’s work were included in the Report of Panel 3 on “The Chemical Assay of Senna Fruit and Senna Leaf,” which was published in the October issue of The Analyst. Panel 3 is now to investigate chemical methods of assaying cascara and its preparations and as no satisfactory animal response to cascara is known the Panel feels it cannot be of any direct assistance in this work. The Panel has therefore gone into abeyance but will again undertake work if a suitable animal response is discovered. PANEL 6 PYRETHRUM CONSTITUTION- W.Mitchell B.Sc. Ph.D. F.R.I.C. H0n.M.P.S. (Chairman) E. A. Baum D.Sc. I.C.N.* H. E. Coomber B.Sc. L. Donegan M. Elliott Ph.D. A. D. Harford S. C. Jolly B.Sc. B.Pharm. M.P.S. F.R.I.C. W. S. Manson B.Sc. A.R.I.C. R. A. Rabnott F. H. Tresadern T. F. West Ph.D. D.Sc. A.M.I.Chem.E. F.R.I.C. P. W. Shallis (Secretary) Stafford Allen & Sons Ltd. Pyrethrum Bureau Mitchell Cotts & Co. Ltd. Ministry of Overseas Development Tropical Rothamsted Experimental Station British Petroleum Research Centre Pharmaceutical Society of Great Britain Cooper Technical Bureau Analytical & Consulting Chemist Stafford Allen & Sons Ltd. Society of Chemical Industry Products Institute - * Resigned June 1965. TERMS OF REFERENCE-“TO investigate methods of assay of pyrethrum flowers and pyrethrum extract with a view to recommending a standard chemical or physical method of assay.’ ’ PROGRESS OF WORK- Since the publication in 1964 of the Panel’s recommended mercury reduction method (a slightly modified version of the A.O.A.C. method) for determining pyrethrins attention has been directed to other methods. Two methods for determining “pyrethrin 11” were con- sidered-an infrared method and a method involving chromatographic separation. Although these methods and the comparable methods for determination of “pyrethrin I,” are less empirical than the mercury reduction method it was decided not to instigate collabora- tive work on them mainly because they require as much time for performance as does the mercury reduction method. 88 REPORT OF THE ANALYTICAL METHODS COMMITTEE 1965 [PrOC.SOC. Anabt. CheW. The Panel decided however to attempt to find a suitable and more rapid method that could be recommended for routine use. With this object in view a preliminary collaborative investigation of the as yet unpublished ethylenediamine method for determining “total pyrethrins” is being undertaken to assist the Panel in deciding whether or not this method is worth further consideration. PANEL 7 THYROID CONSTITUTION- C. A. Johnson B.Sc. B.Pharm. F.P.S. F.R.I.C. British Pharmacopoeia Commission R. E. A. Drey B.Sc. F.R.I.C. Miss S. J. Patterson B.Sc. A.R.I.C. Ministry of Technology Laboratory of the N. A. Terry B.Pharm. F.P.S. C. Vickers B.Sc. M.Pharm. A.R.I.C. Miss B. Gartside B.Pharin. M.P.S. (Assistant Pharmaceutical Society of Great Britain P.W. Shallis (Secretary) (Chairman) Wellcome Chemical Works Government Chemist British Drug Houses Ltd. Boots Pure Drug Co. Ltd. Secretary) TERMS OF REFERENCE-“TO investigate the possibility of devising a chemical method for determining the pharmacologically-active constituents of thyroid.’’ PROGRESS OF WORK- After several unsuccessful attempts at devising a method for determining the pharma- cologically-active constituents of thyroid the Panel agreed to limit its objective and to con- centrate on attempting to find a method that could be used to sort acceptable from unaccept- able samples of thyroid. For this purpose the Panel began in 1964 a collaborative investiga- tion of a thin-layer chromatographic method devised in the laboratory of one of its members that was capable of separating iodinated amino-acids (Clements and Patterson Nature 1965 207 1292).It was soon established that 3,5,3‘-tri-iodothyronine the principal active con- stituent could readily be separated from all other substances and by running on the same plate a graded series of standard liothyronine spots it was possible to obtain a measure of the tri-iodothyronine content. This method was applied to nine samples of thyroid and 5 batches of thyroid tablets and each member of the Panel was able to place all samples in the same order of biological potency as had previously been assessed by the rat anti-thiouracil goitre method. A report of the Panel’s work incarporating details of the recommended method is being prepared. PANEL 8 PHENOTHIAZINE CONSTITUTION- W. H. Stephenson F.P.S. D.B.A. F.R.I.C.Boots Pure Drug Co. Ltd. J. K. Bailey A.R.I.C. Boots Pure Drug Co. Ltd. P. Casapieri B.Sc. Ph.D. Cooper Technical Bureau A. Holbrook F.R.I.C. Imperial Chemical Industries Ltd. (Pharma- D. A. Walker B.Sc. A.R.I.C. P. W. Shallis (Secretavy) (Chairman) ceuticals Division) Nicholas Research Institute Ltd. TERMS OF REFERENCE-“ (a) 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- During the year the Panel completed its work on standardisation of conditions for the partition-chromatographic method for determining phenothiazine (Holbrook Barlow and Bailey J . Pharm. Pharmacol. l963,55,232T). By the inclusion of (a) purification procedures May 19661 REPORT OF THE ANALYTICAL METHODS COMMITTEE 1965 89 for some of the reagents and (b) a modification of technique whereby the sample was trans- ferred to the column as a solution all members obtained in a final collaborative investigation results the precision of which could probably not be improved upon by this method.Details of the standardised method have been made available for inclusion in the forthcoming Supple- ment to the British Veterinary Codex. Although this has proved to be the simplest method the Panel has considered its precision has been found to be slightly inferior to that of the partition-chromatographic method. Currently the Panel is investigating two further possible methods-a method based on the formation of a coloured complex with palladium chloride (Ratcliffe and Stevens J .Ass. Publ. Analysts 1965 3 93) and a gas-chromatographic method. Subsequently an investigation of an infrared method has been undertaken. PANEL 9 THIN-LAYER CHROMATOGRAPHY OF CORTICOSTEROIDS CONSTITUTION- C. A. Johnson B.Sc. B.Pharm. F.P.S. F.R.I.C. British Pharmacopoeia Commission R. A. Bastow B.Sc. F.R.I.C. Miss B. Gartside B.Pharm. M.P.S. A. Hall B.Sc. W. McMeekin B.Sc. Ph.D. J. S. Wragg B.Sc. F.R.I.C. P. W. Shallis (Secretary) (Chairman) Pjizer Ltd. Phawnaceutical Society of Great BYitain Glaxo Laboratories Ltd. Organon Laboratories 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 B.P. and the B.P.C." PROGRESS OF WORK- The Panel held its first meeting in October which was devoted to a discussion of the programme of work to be carried out.A collaborative investigation of several revealing agents has been put in hand aimed at establishing which of them offer adequate sensitivity within the context of the test the Panel hopes to devise. Solvent systems capable of separating impurities from corticosteroids on silica gel plates will then be investigated. 90 REPORT OF THE ANALYTICAL METHODS COMMITTEE 1965 [Proc. SOC. Analyt. Chew. APPENDIX I THE SOCIETY FOR ANALYTICAL CHEMISTRY ANALYTICAL METHODS TRUST ACCOUNTS FOR THE YEAR ENDED OCTOBER 31s~ 1965 Income and Exfienditwe Account f o v the Yeav ended October 31st 1965 1964 L L 364 3294 63 165 32 48 94 84 4144 - 1373 L5517 _- - 1964 k t Rent Light Heat and Telephone .. . . 401 Salaries . . .. . . 2504 Maintenance of Office Equipment . . . . 8 Printing and Stationery 276 Travelling Expenses . . 40 Expenses of Meetings . . 99 Postage and Petty Ex- penses . . . . . . 84 Audit Fee and Ac- countancy . . . . 37 - 3449 Excess of Income over Expenditure for the year ended October 31st 1965 transferred to Accumulated Fund 31 1964 k L Subscriptions and Donations from 2935 Industry . . Interest from 215 Investments L L Gross . . . . 7 Taxed (net) . . 199 From Bank 206 527 Deposits . . 746 __ -_ 742 __ 181 1659 Profit on sales of “Recom- mended Methods for the Analysis of Trade Effluents” received from the Society for Analytical Chemistry Income Tax refunded on Covenanted Subscrip- tions 1963-64 .. k5517 ___ - Accumulated Fund 1964 f f /d /d Decrease in value o n Realisa- A - tion of 500 United Molasses Co.20,329 Ltd. 10s. units Ordy Stock . . . . 52 462 200 Tate & Lyie Ltd. Balance a t October 31st 1965 Ordy Shares . . . . 47 - 99 1373 22,164 carried to Balance Sheet . . 22,096 L- - - @2,164 k22,195 &22,164 - Balance a t October 31st 1964 brought forward from previous Account . . . . .. . . Increase in Value on Realisation of Securities . . . . . . Excess of Income over Expendi- ture for the year ended October 31st 1965 . . .. .. L 2221 952 84 223 k3480 - - fI 22,164 - 31 k22,195 - May 19661 REPORT OF THE ANALYTICAL METHODS COMMITTEE 1965 91 1964 Balance Sheet at October 31st 1965 1964 L f l f l Accumulated Fund . . ‘ 2,2096 Sundry Creditors 6484 The Society for Ana- 174 lytical Chemistry.. 186 195 - - 243 L L 22,164 21 Accountancy . . . . 57 11,000 f l k Investments (at Cost) Cash at Banks As per Schedule . . 7385 (Market Value k6966) United Dominions Trust Ltd Account 11,000 Account .. 3954 On Deposit On Current Barclays Bank Ltd. 14,954 fl22,359 L22,339 Signed on behalf of the Analytical Methods Trust Fund G. H. LLOYD-JACOB Chairman D. J. LEWIS Honorary Treasurer. Auditors’ Repm! to the Trustees of the Society for Axalytical Clzevnistvy 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 1965 and it is in accordance with the Books kept by the Trustees. We have verified the Investments and Cash Balances and found them to be in order.65 Southampton Row London W.C.l. February 28th 1966. Nominal amount L l O O L l O O L375 250 500 83 1100 ,6300 660 300 ,5100 - - 400 300 (Signed) KIDLEY & CO. Chartered Accozmtants Auditors. Schedule of Investments held at October 31st 1965 34?( Conversion Stock . . .. . . 3;t:/ War Stock . . . . .. .. Debenhams Ltd. 10s. Ordy Shares . . Imperial Chemical Industries Ltd. Ordy Stock . . . . . . . . .. Philip Hill Investment Trust Ltd. 5s. Hill Samuel Ltd. 5s. Ordy Shares (issued as Bonus through Philip Hill Invest- Morris & David Jones Ltd. 5s. Ordy Shares . . . . . . . . . . Bonus Issue * . . . . . . . Ranks Hovis McDougall Ltd. 10s. units Ordy Stock (purchased May 1965) . . Royal Insurance Co. Ltd. 5s. units Ordy Stock . . . . . . . . . . issued in part satisfaction of 500 United Molasses Co.Ltd. 10s. units Ordy Stock (brought in at ,6389; sold June 1965 realising ,6341; decrease in value United Molasses Co. Ltd. 10s. units Ordy Stock . . . . . . . . . . acquired by Tate & Lyle Ltd. on issue of 200 Ordy Shares in that Company (valued a t ,6389 ; cash ,6581; decrease in value ,6192) Wharf Holdings Ltd. Ordy Shares . . Venesta Ltd. Ordy Shares (purchased Ordy Shares . . . . . . . . ment Trust Ltcl.) . . . . .. Renold Chains Ltd. Ordy Stock . . . . Tate & Lyle Ltd. Ordy Shares . . . . L48) June 1965) . . .. .. . . Held 3 1.10.64 a t cost 83 100 747 736 708 L - 1012 655 - - 735 - 973 706 - - itj6484 - Held 31.10.65 a t cost 83 100 747 736 708 It Unvalued 1012 685 Unvalued 1001 735 - - 706 872 fl7385 - - Market value at 31.10.65 63 54 456 853 400 fl 54 1141 800 990 517 - - 850 $88 fl6966 - __ - Income received during year ended 31.10.65 fl 3 Gross 4 Gross 16 29 12 1 3s 23 11 16 None due 22 31 None due - fl20s = 92 CHANGES IN THE REGISTER OF MEMBERS [Pvoc.SOC. Analyt. Chem. APPENDIX I1 SUBSCRIBERS TO THE TRUST FUND DURING 1965 A.B.M. Industrial Products Ltd. Albright & Wilson Ltd. Associated Portland Cement Manufacturers Boots Pure Drug Co. Ltd. The British Drug Houses Ltd. Cadbury-Fry Ltd. Central Electricity Generating Board Courtaulds Ltd. The Distillers Co. Ltd. Dunlop Rubber Co. Ltd. Fisons Ltd. Geigy (U.K.) Ltd. Hopkin & Williams Ltd. Ltd. Imperial Chemical Industries Ltd. Laporte Industries Ltd. J. Lyons & Co. Ltd. May & Baker Ltd. The Metal Box Co. Ltd. 0x0 Ltd. Procter & Gamble Ltd. Riker Laboratories Ltd.Rowntree & Co. Ltd. “Shell” Research Ltd. Smith Kline & French Laboratories Ltd. John & E. Sturge Ltd. Tate & Lyle Ltd. Unilever Ltd. Changes in the Register of Members NEW MEMBERS ORDINARY MEMBERS John Noel Armes A.R.I.C. ; Charles Norman Bell; George Brian Buckley B.Sc.(Lond.) ; Gordon Terry Chamberlain ; Thomas Malcolm Cotton ; Robert Anthony Cross B.Sc.(St. A.) ; John Herbert Futter M.Sc.(N.Z.) ; Godfrey James Hawltins B.Sc.(Wales) ; Geoffrey Hims- worth; Geoffrey Martin Holmes F.R.I.C. ; Peter Frederick Spencer Jackson B.Sc.(Manc.) ; Lawrence A. Keelan B.Sc. ; Harry Vincent Lowther B.Sc.(Lond.) F.R.I.C. ; Michael Derek Mayhew B.Sc.(Lond.) A.R.C.S. ; Ronald Sidney hlunday B.Sc.(Exeter) A.R.I.C. ; Kim-Chye Ong B.Sc. Ph.D. A.R.I.C. P.A.I.W.E. ; Mervyn Edward Pattinson A.N.Z.I.C. ; Sheila Jean Purdy B.Sc.(Lond.) Ph.D.(Leeds) A.K.C. ; Edward Braxton Reynolds B.Sc.(Lond.) ; John Stanley Charles Sceal B.Sc.(Lond.) ; Ian Leslie Stansfield A.R.I.C. ; Albert Stoner; John Victor Tidder L.R.I.C. ; Raphael Mbogo Wanguo M.S. ; Herbert Dale Warren B.A. (Rice) M.S. (Idaho) Ph.D. (Oregon) ; Robert Wood B.Sc. Ph.D.(St. A.) A.R.I.C. ; Trevor Owen Young A.C.T.(Birm.) F.R.I.C. JUNIOR MEMBERS Jeffrey Paul Arnold B.Sc.(Lond.) ; Andrea de Luca B.Sc.(Manc.) ; Alvan William Leonard Dudeney B.Sc.(Leic.) ; Andrew Dick Nicol B.Sc. ; William Bruce Painting; David Arthur Stevenson.

ISSN:0037-9697    

DOI:10.1039/SA9660300077

出版商:RSC    

年代:1966

数据来源: RSC

摘要:

May 19661 PUBLICATIONS RECEIVED 93 Notices CANADIAN ASSOCIATION FOR APPLIED SPECTROSCOPY 1966 CANADIAN SYMPOSIUM ON APPLIED SPECTROSCOPY THE 1966 Canadian Symposium (formerly called Ottawa Symposium) sponsored by the Canadian Association for Applied Spectroscopy will be held in Montreal Quebec at the Holiday Inn Hotel from October 24th to 26th 1966. An Exposition of the latest developments in spectroscopic equipment and accessories will be held in conjunction with this Symposium taking place for the first time in Montreal which is the site of the 1967 World Exhibition. Arrangements have been entrusted to the Montreal Section of the Canadian Association of Applied Spectroscopy. Titles and brief abstracts of papers should be submitted as soon as possible for review by the Programme Committee to Dr. S. Barabsa Programme Chairman Noranda Research Centre 240 Hymus Blvd. Pointe Claire Que. Canada. Papers are solicited dealing with all fields of spectroscopy. The final date for acceptance will be June 15th 1966. THE POLAROGRAPHIC SOCIETY A Meeting of the Polarographic Society will be held at the City University Designate (North- ampton College) St. John’s Road London E.C.l on June 15th 1966 at 2.45 p.m. The subject of the Meeting will be “Electro-analysis in Molten Salts,” and the speakers will include Professor G. J. Hills and Dr. D. Inman.

ISSN:0037-9697    

DOI:10.1039/SA966030093b

出版商:RSC    

年代:1966

数据来源: RSC

摘要:

THE SOCIETY FOR ANALYTICAL CHEMISTRY May Tuesday 17th STOCKTON-ON- TEES Wednesday 18th LONDON Thursday 19th HUNTINGDON Friday 20th to Monday 23rd LLANDUDNO Tuesday 31st PAISLEY June Wednesday 8th BIRMINGHAM Forthcoming Meetings SOCIETY Special Meeting to mark the Inauguration of the North East Section. Presentation of the Society’s Gold Medal to Mr. H. N. Wilson F.R.I.C. “Analytical Chemistry-A Nonconformist View,” by R. C. Chirnside F.R.I.C. Stockton-on-Tees Co. Durham. MICROCHEMICAL METHODS GROUP London Discussion Meeting on “The “The Feathers,” Tudor Street London E.C.4; 6.30 p.m. BIOLOGICAL METHODS GROUP Summer Meeting. Visit to Huntingdon Research Centre Huntingdon. NORTH OF ENGLAND SECTION Summer Meeting. The County Hotel The Promenade Llandudno. Ordinary Meeting Saturday morning R.J. Taylor B.Sc. will give an introductory talk to two films entitled “The Social programme. SCOTTISH SECTION One-day Symposium on “Thin-layer Chromatography.” “The Principles of Thin-layer Chromatography,” by E. V. Truter Ph.D. “The Application of Thin-layer Chromatography to Anthraquinone Dyestuff “The Thin-layer Chromatography of Carbohydrates,” by K. C. 13. Wilkie “The Thin-layer Chromatography of Lipids,” by W. R. Morrison Ph.D. “The Application of Thin-layer Chromatography to the Analysis of Pesticide College of Technology High Street Paisley; 10.30 a.m. Determination of Fluorine.” Physics and Chemistry of Water” and “Water in Biology.” B.Sc. A.R.C.S. D.I.C. Chemistry,” by C. G. Haynes Ph.D. B.Sc. Ph.D. B.Sc. F.R.I.C. A.R.C.S.T. Residues,’’ by J. Thomson Ph.D. A.H.-W.C. A.R.I.C. MIDLANDS SECTION and PARTICLE SIZE ANALYSIS GROUP on “Commercial Apparatus for Surface Area Measurement.” “The Perkin-Elmer-Shell Sorptometer,” by G. A. Lombard. “The Strohlein Areameter,” by D. P. Bryant. “The Numinco-Orr Surface Area - Pore Volume Analyser,” by A. G. Cottrell. Haworth Lecture Theatre Chemistry Department The University Edgbaston Birmingham 15; 6 p.m. Particle Size Analysis Conference Loughborough 1966 THE number of registration forms sent out in response to tentative enquiries about the Conference already exceeds the number of places expected to be available. Intending participants are advised in their own interests to return their completed application forms at the earliest opportunity. PRINTED BY CV. HEFFER & SONS LTD. CAMBRIDGE ENGLAND

ISSN:0037-9697    

DOI:10.1039/SA9660300094

出版商:RSC    

年代:1966

数据来源: RSC