摘要:

Proceedings of the Society for Analytical Chemistry CONTENTS Editorial .. .. .. .. 77 Reports of Meetings . . .. 77 Pyrolysis - Gas Chromatography 79 Moisture Determination . . 82 Organic Reagents for Metals . . 85 Galvanic Analysis . . . . 87 Papers accepted for The Analyst 88 Obituary . . .. . . . . 89 Membership changes . . . . 89 Publications Received . . . . 90 Notices . . .. . . . . 91 Forthcoming Meeting . . Back cover h c . SOC. Anal. Chem. Vol. I No. 7 Pages 77-92 July 1964 Vol. I No. 7 PROCEEDINGS OF July 1964 THE SOCIETY FOR ANALYTICAL CHEMISTRY President of the Society D. C. Garratt Hon. Secretary of the Society S. A. Price Hon. Treasurer of the Society D. T. Lewis C.B. Hon. Assistant Secretaries of the Society 6. S . Cooper; D. W. Wilson Secretary Miss P. E. Hutchinson 14 BELGRAVE SQUARE LONDON S.W.1 Telephone BELgravia 3258 Editor 1.6. Attrill Proceedings is published by The Society for Analytical Chemistry and distributed to members and all subscribers to The Analyst without charge Single copies may be obtained direct from the Secretary The Society for Analytical Chemistry at the above address (NOT through Trade Agents) price 2s. 6d. post free. Remittances payable to “Society for Analytical Chemistry” MUST accompany orders Methods for the Analysis of Non-Soapy Detergent (NSD) Products by G. F. LONGMAN B.SC. F.R.I.C. & J. HILTON B.Sc. A.R.I.C. (Unilever Research Laboratory Port Sunlight) Society for Analytical Chemistry Monograph No. I -Q- This Monograph describes in detail the methods of analysis developed in Unilever’s Laboratories for the identification and assay of components of NSD Products. -0- Available ONLY from The Editor “The Analyst,” 14 Belgrave Square London S.W. I (Not through Trade Agents) Price 15s. or U.S. $2.00 Post free A remittance made out to “Society for Analytical Chemistry” should accompany every order Members of the Society may purchase copies at the special price of Ss. post free. I

ISSN:0037-9697    

DOI:10.1039/SA96401FX021

出版商:RSC    

年代:1964

数据来源: RSC

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SOCIETY FOR ANALYTICAL CHEMISTRY Reprints of Review Papers REPRIXTS of the following Review Papers published in The Analyst are available from the Secretary The Society for Analytical Chemistry 14 Belgrave Square London S.LV.1 (not through Trade Agents). Orders MUST be accompanied by a remittance for the correct amount made out to “Society for Analytical Chemistry.” “The Analysis of Synthetic Detergents,” by \T. B. Smith (February 1959). “The Infra-red Analysis of Solid Substances,” by G. Duyckaerts (April 1959). “X-ray Fluorescence Analysis,” by F. Brown (June 1959). “Ferrous Metallurgical Analysis,” by B. Bagshaw (Xugust 1959). “Zone Melting with Some Comments on its Analytical Potentialities,” by E. F. G. Herington “The Analytical Chemistry of Zirconium,” by G. W. C. Milner and J . IT.Edwards (February “Light-scattering Methods for the Chemical Characterisation of Polymers,” by F. TI’. Peaker “Analysis of Organo-silicon Compounds with Special Reference to Silanes and Siloxanes ” by “Flame-photometric Methods in Metallurgical Analysis,” by John A. Dean (September 1960). “The Oxygen Flask Method,” by A. M. G. Macdonald (January 1961). “.Analytical Chemistry of Beryllium,” by I,. E. Smythe and R. S. IVhitteni (February 1961). “lletermination of Residual Organo-phosphorous Insecticides in Foodstuffs,” by E. 11. Chilwell “Biological Standardisation and the Analyst,” by J . IT. Lightbown (April 1961). Price 5s. “The Toxicology of Nitrates and Nitrites with Particular Reference to the Potability of TT\’ater “Coulometric Methods in Analysis,” by D. T. Lewis (August 1961).“Emission Spectroscopy of Solutions,” by L. G. Young (January 1962). “-Analytical Applications of the Mercury Electrode,” by J . ,I. Page J . A . Maxwell and R. P. “The Determination of Tantalum and Niobum,” by M. H. Cockbill (,lugust 1962). Price 5s. “Classification of Methods for Determining Particle Size,” by the Particle Size A\nalysis Sub- “Xethods of Separation of Long-chain Unsaturated Fatty _Acids,” by A. 7’. James (Xugust “Beer’s Law and its Use in Analysis,” by G. F. Lothian (September 1963). ‘‘-1 Review of the Methods Available for the Detection and Iletermination of Small *\mounts Price 5s. “Circular Dichroism,” by R. I>. Gillard (November 1963). “Information Retrieval in the Analytical Laboratory,” by D. R. Curry (Kovember 1963). “Thermogravimetric Analysis,” by A.W. Coats and J . P. Redfern (December 1963). Price 5s. “Some Analytical Problems Involved in Determining the Structure of Proteins and I’eptides ” Reprints of Review Pafiers not on this list are no longer available from the Societjl. Many back numbers of The Analyst are still available and may be brought from Messrs. IFr. Heffer R- Sons Ltd. 3-4 Petty Cury Cambridge price 15s. plus 9d. postage. Price 2s. 6d. Price 2s. 6d. Price 2s. 6d. Price 5s. (December 1959). Price 5s. 1960). Price 5s. (April 1960). Price 5s. J . C . B. Smith (July 1960). Price 5s. Price 5s. Price 5s. Price 5s. and G. S. Hartley (March 1961). Price 5s. Supplies,” by E. H. W. J . Burden (July 1961). Price 2s. 6d. Price 5s. Price 5s. Graham (April 1962). Price 5s. Committee of the Analytical Methods committee (March 1963).1963). I’rice 5s. Price 5s. Price 5s. of Cyanide,” by L. S. Bark and H. G. Higson (October 1963). Price 2s. 6d. Price 2s. 6d. by Derek G. Smyth and D. F. Elliott (February 1964). I’rice 5s. SOCIETY FOR ANALYTICAL CHEMISTRY Forthcoming Meeting MIDLAKDS SECTION and THIN-LAYER CHROMATOGRAPHY PXXEL of the PHYSICAL METHODS GROUP THE Midlands Section of the Society for Analytical Chemistry the Thin-layer Chromato- graphy Discussion Panel of the Physical Methods Group of the Society for Analytical Chemistry and the Birmingham and Midlands Section of the Royal Institute of Chemistry will be holding a 1-day symposium on “Thin-layer Chromatography” at the Medical School The University Edgbaston Birmingham 15 on Wednesday October 14th 1964. The programme will be as follows- 1.30 p.m.in the Arthur Thompson Hall. “Thin-layer Chromatography in Clinical Biochemistry,” by J . G. Lines Ph.D. M.Sc. (Children’s Hospital Birmingham). “Exploitation of Thin-layer Chromatography in Plant Chemistry,” by E. J. Shellard Ph.D. F.P.S. F.L.S. F.R.I.C. (Chelsea College of Science and Technology). 2.45 p.m. Tea in the Chamberlain Museum. 3.15 p.m. in the Arthur Thompson Hall. PLENARY LECTURE “Some New Techniques and Apparatus in the Field of Thin-layer Chromatography,” by Professor Egon Stahl (University of Saarlandes Saarbrucken West Germany). 4.45 p.m. Tea in the Chamberlain Museum. 5.30 p.m. in the Large Anatomy Theatre. “The Use of Thin-layer Chromatography in Biosynthetic Studies,” by 13. H. Davies B.Sc. Ph.D. A.R.I.C. (University College of IVales Xberystwyth). 6.30 p.m.in the Large Anatomy Theatre. “Recent Developments in Thin-layer Chromatography Equipment ,” by R. P “Thin-layer Chromatography on Ion-exchange Media,” by C. S. Knight. There will be ample time allowed for discussion in each session. Hirsch (Camlab (Glass) Ltd. Cambridge). M.Sc. Ph.D. A.R.I.C. (W. & R. Balston Ltd. Maidstone Kent). Besides the refreshments listed above more substantial refreshments including lunch may be obtained in the University Refectory. A Trades Exhibition on Thin-layer Chromatographic Equipment and Materials has been arranged in the Chamberlain Museum (Medical School) and will be open from 11 a.m. until 8 p.m. All enquiries in connection with the Trades Exhibition should be made to Mr. D. M. Peake B.Sc. A.R.I.C. c/o Imperial Metal Industries (Kynoch) Ltd. P.O. Box 216 Kynoch Works l!itton Birmingham 6. Further details of the Symposium can be obtained from Mervyn L. Richardson A.R.I.C. A.C.T. (Birm.) Hon. Secretary Midlands Section The Society for Analytical Chemistry c/o John 4% E. Sturge Ltd. Lifford Lane Kings Norton Birmingham 30 England. PRINTED BY W. HEFFER & S O N S LTD. CAMBRIDGE. ENGLAND.

ISSN:0037-9697    

DOI:10.1039/SA96401BX023

出版商:RSC    

年代:1964

数据来源: RSC

摘要:

July 1964 Reports of Meetings Vol. I No. 7 NORTH OF EXGLAKD SECTIOS AXD MICROCHEMISTRY GROUP JOIXT Meeting of the North of England Section and the Microchemistry Group with the Manchester and District Section of the Royal Institute of Chemistry and the Chemical Society of the Royal College of Advanced Technology of Salford was held at 7 p.m. on Friday May 8th 1964 in the Department of Chemistry and Applied Chemistry Roval College of Advanced Technology Salford. The Chair was taken bv the Chairman of the Microchemistry Group Mr. D. \$’. Wilson M.Sc. F.R.1 .C. The subject of the Meeting was “Organic Reagents for Metals” and the following papers were presented and discussed “Organic Complexing Agents as Reagents for Metals,” F. Holmes B.Sc. F.R.I.C. ; “A Precipitant Designed for the Precipitation of Palladium by L.S. Bark B.Sc. F.R.I.C. and D. Brandon A.R.I.C. A.R.C.T.S. papers are given on p. 85.) Geigy Co. Ltd. Trafford Park Manchester. bx (Summaries of these The Meeting was preceded at 2.15 p.m. by a visit to the Ashburton Chemical Ii’orks NORTH O F ENGLAND SECTION THE twenty-seventh Summer Meeting of the Section was held at the Imperial Hotel Llandudno from Friday June 12th to Monday June 15th 1964. The Chairman of the Section Mr. C. J. House B.Sc. A.R.C.S. F.R.I.C. presided o\rer an Ordinary Meeting at 10.30 a.m. on Saturday June 13th at which Dr. D. W. G. Dicker gave a lecture entitled “The Biodegradability of Detergents.” On the Saturday evening the party visited the Arcadia Theatre and on the Sunday afternoon made a coach tour from Llandudno to Denbigh Denbigh Yloors to Pentrevoelas Rettws-y-Coed taking tea at the Voelas Hotel Pentrevoelas.MIDLANDS SECTIOX AND PHYSICAL METHODS GROL‘P .A JOIXT Meeting of the Midlands Section and the Physical Blethods Group with the East ,4nglia Section of the Royal Institute of Chemistry was held at 5.45 p.m. on Friday Xay lst 1964 at the Levington Research Station Fisons Fertilizers Ltd. Ipwich. The Chair was taken by the Chairman of the Midlands Section Mr. 117. H. Stephenson F.P.S. D.R.,4. F. R . I .c. 78 REPORTS OF MEETIKGS [Pvoc. SOC. Anal. Chew. The subject of the Meeting was “Some Physical Methods of Moisture Determination” and the following papers were presented and discussed “A Review of Methods of Determining Moisture in Paper,” by L. A. Kirk M.Sc.Tech. A.M.I.Chem.E. A.M.C.T.; “The Application of Nuclear Magnetic Resonance to the Measurement of the Moisture Content of Coals and Cokes,” by W.R. Ladner B.Sc. Ph.D. A.R.I.C. ; “An Introduction to Microwave Moisture Measurement,” by H. €3. Taylor. The Meeting was preceded at 2.30 p.m. by a visit to the Research Laboratories Levington Research Station Fisons Fertilizers Ltd. (Summaries of these papers are given on p. 82.) MIDLANDS SECTION A JOINT Meeting of the Midlands Section with the Birmingham and Midlands Section of the Royal Institute of Chemistry The Polarographic Society and the Guild of Associates of the College of Advanced Technology Birmingham was held at 6.30 p.m. on Tuesday June 9th 1964 in the Haworth Lecture Theatre Chemistry Department The University Edgbaston Birmingham 15. The Chair was taken by the Chairman of the Midlands Section Mr.W. H. Stephenson F.P.S. D.B.A. F.R.I.C. The following paper was presented and discussed “Galvanic Analysis,” by Dr. P. Hersch (see summary on p. 87). An exhibition of Instruments of the Lecturer’s company was shown. MICROCHEMISTRY GROUP THE forty-fifth London Discussion Meeting of the Group was held at 6.30 p.m. on Wednesday June loth 1964 at “The Feathers” Tudor Street London E.C.4. The Chair was taken by the Vice-chairman of the Group Mr. R. Goulden F.R.I.C. A discussion on “The Analysis of Organo-metallic Compounds” was opened by G. Ingram A.R.I.C. BIOLOGICAL METHODS GROUP THE Summer Meeting of the Group was held on Thursday May 28th 1964 and took the form of a visit to the Nicholas Research Laboratories and Nicholas Products Ltd. Slough Bucks.The morning was spent in touring the factory the research and development laboratories and the analytical-control laboratory and in the afternoon a visit was made to the biological research laboratories at Wexham Place. Analytical Methods Committee JOINT COMMITTEE ON METHODS OF ASSAY OF CRUDE DRUGS THE Joint Committee of the Pharmaceutical Society and the Societv for Analytical Chemistry has appointed a Panel to recommend a method of assay for phenothiazine. The constitution of the Panel is Mr. W. H. Stephenson (Chairman) Mr. J. K. Bailey Dr. P. Casapieri Mr. A. Holbrook and Mr. D. A. Walker with Mr. P. W. Shallis as Secretary and its terms of reference are :- “(a) To recommend a satisfactory method for determining phenothiazine and ( b ) to extend this method to cover most commercial phenothiazine dispersible powders.”

ISSN:0037-9697    

DOI:10.1039/SA964010077b

出版商:RSC    

年代:1964

数据来源: RSC

摘要:

July 19643 REPORTS OF MEETINGS 79 Pyrolysis - Gas Chromatography The following are summaries of papers presented at the Ordinary Meeting of the Society held on May 6th 1964 and reported in last month’s issue of the Proceedings (p. 67). The Identification of Polymers and Other High Molecular Weight Compounds by a Combined Pyrolysis - Gas Chromatographic Technique BY C. V. GIBSON (Imperial Chemical Industries Ltd. Dyestuffs Division Blackle?, Manchestev 9) and The Application of Pyrolysis - Gas Chromatography to the Analysis of Polymeric Materials RY P. E. ARNOLD (Impei&l Chemical Industries Ltd. Plastics Division Welzuyn Gardevz City Herts.) MR. GIBSON began by outlining some of the methods available for identifying polymeric materials. A preliminary purification or fractionation with solvents was often necessarj.before physical and chemical examination of the fractions or of their degradation products obtained for example by hydrolysis. In other instances e.g. vulcanisates the insolubilitj- and lack of chemical reactivity of the material made it necessary to depend largely on the interpretation of results obtained from dry heating differential swelling in organic solvents acid resistance and semi-specific colour tests. Examples were given of the difficulties that could arise; in order to avoid these difficulties a combined pyrolysis - gas chromatographic method had been developed in which pyrolysis was carried out in an electrically heated coil in the sample inlet of a gas chromatograph. Details were given of the sample-inlet system and the associated electrical circuit for controlling pyrolysis time and temperature; to carry out the tests samples were placed in the coil either as small discrete pieces or deposited from solutions or applied as pastes with gum tragacanth and then dried before pyrolysis.Pyrolysis patterns (“pyrograms”) had been obtained from 60 known polymers by using either a 6-foot column packed with 30 per cent. w/w silicone elastomer on 30- to 60-mesh G-CEL or a %foot column packed with 30- to 60-mesh silica gel and with temperature pro- gramming of the column heaters. The “pyrograms” were collected into atlases each with an index based upon relative retention times obtained by using suitable reference compounds. Unknown polymers were then identified by comparing their “pyrograms” with those in the atlases. The “pyrograms” of some known polymers were then discussed in relation to their structure and mechanism of degradation.Examples were then given of the identification of some typical samples of synthetic rubbers. The application of the method to materials other than polymers was illustrated by determining the length of the alkyl chain in a quaternarj- ammonium iodide. If polymers were encountered yielding “pyrograms” that did not match those in the atlases additional information was obtained by collecting the pyrolysis - gas chromatographic fractions and subjecting them to ultraviolet or infrared spectroscopy nuclear magnetic resonance or mass spectrometry. In order to isolate these fractions the effluent stream from the column was split and part was led through a heated capillary to a trap leaving only sufficient effluent flowing through the detector to maintain a satisfactory signal.Of these physical techniques the one showing most promise was gas - liquid chromatography used before mass spectrometry in which technique individual fractions could be identified by pass- ing them directly from the column into the inlet system of the spectrometer; hydrocarbons and styrene homologues had been identified in this way. MR. ARNOLD described the operation of a mechanical controller based on a synchronous motor. With this controller any of nine pre-set pyrolysis temperatures between 150” and 950” C could be obtained and the pyrolysis time varied between 5 and 30 seconds. The controller had been used in conjunction with a gas chromatograph fitted with a flame ionisa- tion detector to develop a rapid “fingerprint” method of identification for insoluble and filled polymers.The application of the method to the identification of various materials was 80 REPOKTS OF MEETIKGS _Proc. SOC. Agzal. Cheiiz. discussed. Fibres such as cotton rayons Terylene and nylons could be distinguished by the method where previously time-consuming chemical methods involving the use of larger samples were required. For polyolefins it was not only possible to distinguish between poly- ethylene and polypropylene but to differentiate between polyethylenes prepared by the high- and low-pressure processes. This had been found especiallj- useful Lvhen dealing with filled materials that were unsuitable for examination by infrared spectroscopy. The method had also been found useful in the characterisation of modifiers added to a polvmer.For example acrylic ester modifiers in poly(viny-1 chloride) compositions could be detected and identified by the presence and positions of extra peaks in the poly(viny1 chloride) “pyrogram.” In the examination of poly(viny1 chloride) compositions containing butadiene copolj-mers the buta- diene copolymer had been detected by the pyrolysis - gas chromatographic examination of the tetrahydrofuran-insoluble fraction obtained from these materials ; in this instance infrared spectroscopy could not be applied owing to the large amounts of inorganic salts present. The “pyrograms” obtained were sufficiently reproducible for the quantitati\-c determina- tion of copolymer compositions to be made bj- comparison with “pyrograms” of copolJ7mers of known composition.Results obtained with methyl methacrylate - ethJ.1 acrylate copolymers had been found to agree to within 1 per cent. with those obtained by infrared spectroscopy. The method had since been used for determining 2-ethylhexj.1 acrylate in methyl methacrylate copolymers for which no suitable infrared or chemical method could be found. ,\lso the method had been used to analyse polyethylene - propylene copolymers and but>-1 rubber - poly- propylene blends when these contained inorganic fillers. Finally the possibility of distinguishing between copolymers and blends of similar composition by a stepwise pyrolysis procedure was discussed and illustrated by reference to the “pyrograms” of a copolymer and blend of methyl methacrylate and styrene. This method had been used to distinguish between a fluoroethylene copolymer and polytetrafluoroethylene both of which produced identical “pvrograms” in the complete pyrolysis procedure.Both authors acknowledged the hc!p of Professor J. C. Robb of Birmingham University in the development of their techniques. DISCUSSION MR. C. E. R. JOKES commenting on 3Ir -Arnold’s statement that samples were pre-fired a t 250” C to remove solvent residues said that this practice must jeopardise quantitative recoveries as some polymers e.g. those containing methyl methacrylate had a finite de- gradation rate a t this temperature and would not give a discrete peak but a diffuse base- line or merely appear as a drift. He believed that much benefit accrued from working with samples of about 4 p g as opposed to a milligram.Much cleaner chromatograms resulted owing to the suppression of secondary reactions. He showed two slides illustrating the cleanliness of polystyrene degradation together with the reproducibility as shown by the pyrolysis chromatograms of four consecutive 4-pug samples pyrolysed a t 700” C. They also showed that 0.5 per cent. of styrene in a 99.5 per cent. methyl methacrylate - 0.5 per cent. styrene copolymer was ea5ily determined on this scale Degradation routes were influenced not only by environment but by the components and the relative amount of these components in a copolymer e g 80°0 - 20°& and SO0/ - 407L copolymers of vinyl acetate and dioctyl fumarate gave such strongly con- tr,tsting fingerprint chromatograms that on inspection one would infer the presence of di fferent species.Graft copolymers could be readily distinguished from polymer mixtures. For example vinyl acetate had frequently been emulsion-polymerised with poly(viny1 alcohol) a s the protective colloid. Under certain conditions the products contained a high pro- portion of graft copolymer which gave quite different pyrolysis chromatograms to those from poly(viny1 alcohol)-stabilised poly(viny1 acetate) emulsions that were not grafted. Mr. Ik-nold replied that the pre-heating a t 250” C was carried out for 15 seconds with the coil fitted in the column inlet and so far no evidence of polymer degradation had been observed. IYith regard to the sample size 1 nig had been found to be convenient a5 the method was developed primarily for insoluble materials and the only practical way to handle 4 p g was in solution.MR. J. V. MORTIMER said that both authors had described the pyrolysis of samples by using a heated nichrome-wire coil but recent papers had describecl the use of furnace July 19641 REPORTS OF XIEETIKGS chambers heated conventionally or by radio-frequency energy as pyrolysis units. He sought the speakers’ opinions on the relative merits of the heated-wire coil and the furnace- chamber pyrolysis units. Neither speaker had experience of furnace or radio-frequency heating but Mr. Arnold commented that with a furnace it would not be possible to carry out stepwise pyrolysis procedures. MR. E. L. BUSH asked if Mr. Gibson had a systematic method for finding solvents for his plastics and if either author considered it possible to gain information on the structure of cross-linked materials from pyrolysis chromatograms.hlr. Gibson used a range of solvents of increasing polarity based on previous experience. Mr. Arnold said that “pyrograms” of cross-linked polythenes normally showed no difference from ordinarp polythene. However a sample of very highly cross-linked polythene had been found to produce an extra series of peaks. Mr. Gibson added that structural differences could be detected but that it was first desirable to study a series of known polymers. Mr. A%rnold told MR. W. A. CREGEEN that no significant differences had been observed in the “pyrograms” of polythenes from different low-pressur e processes and he told DR. H. ~VARSOX that i t was not possible to detect by pyrolysis - gas chromatography the cross-linking agent in such polymers as polyacrylate or poly(methacry1ate) cross-linked in the emulsion form.MR. L. DAVIES said that it would appear that the technique described suffered from the drawback that the system had to be disrupted for the introduction of the sample but neither author found any disadvantage in the system since the sample was introduced nhile the column heater was being cooled for the next run; attention was drawn to the paper by J . H. Dhont (Analvst 1964 89 71) describing the identification of aliphatic alcohols by sweeping them through a pyrolysis tube with carrier gas. Mr. Gibson told MR. D. J . DIMMOCK that it wa5 possible to distinguish between phenol - iormaldehyde and cresol - formaldehyde resins but that resols and novolaks had not been compared. MR. R. \T. LEWIS asked what effect any residues remaining on the coil after pyrolysis had on the temperature during subsequent analyses.Both speakers said that residues could be burnt off the coil by raising the temperature of the coil to 1000” C in air; inorganic residues normally left as an ash that could be brushed off. There was no effect on subse- q uent analyses. MRS. S. M. I~YUICKA said that caution was needed in interpreting pyrolysis chromato- grams. In the Paint Research Laboratory they had found that pyrolysis of paint films in a gas-chromatographic column gave different patterns of peaks although the paints contained the same organic media and differed only slightly in the inorganic pigments. Presumably a catalytic effect caused a different pattern of decomposition. If this was realised pyrolysis patterns could give some information both on the organic material and also on small differences in the inorganic matter present.MR. R. M. ROWLEY drew attention to the work of Barlow Lehrle and Robb ( S . C . I . Jlovzogvaph 17 Society of Chemical Industry London 1963) on random and block or graft copolymers and asked Mr. Gibson if he had applied this work in the field of rubber analysis. Mr. Gibson said that for some acrylic resins differences had been found in the relative proportions of some of the peaks in the “pyrograms” from mixtures and random copolymers of the same components but these had not been studied in detail. MR. C. F. EVERETT asked how copolymers could be quantitatively analysed if they did not pyrolyse to give simple monomers but each gave a series of degradation products. Nr. Xrnold said that copolymers ethylene and propylene that did not pyrolyse to monomers had been analysed by measuring the relative peak heights of certain peaks in the “pyro- gram.” Mr. Gibson said that authentic polymers of known composition must first be studied and calibrations established for one or more characteristic peaks from each polymer component; the calibrations could then be used for the quantitative analysis of samples. DR. W. W. WRIGHT asked Mr. Gibson to enlarge on his technique involving pyrolysis - gas chromatography and mass spectrometry. Mr. Gibson replied that an A.E.I. MS 2 mass spectrometer had been used; about 5 per cent. of the effluent from the gas - liquid chromatographic column had been fed in a capillary tube into a tap system so that the required fraction could be fed into a reservoir and then into the mass spectrometer. 81

ISSN:0037-9697    

DOI:10.1039/SA9640100079

出版商:RSC    

年代:1964

数据来源: RSC

摘要:

82 REPORTS OF MEETINGS L P ~ o c . SOC. ,47?al. Chcm. Some Physical Methods of Moisture Determination The following are summaries of papers presented at the Meeting of the Midlands Section and Physical Methods Group held on May lst 1964 and reported in this issue of the Proceedifqgs (P- 77). A Review of Methods for Determining Moisture in Paper BY L. A. KIRK (The Dlanchestev College of Science and Technology Dlaszchestev 1) MR. KIRK said that paper was a hygroscopic material that contained some 8 to 10 per cent. of moisture when in equilibrium with the typical English climatic conditions. Owing to the difficulties inherent in the absolute determination of moisture content of paper representative bodies such as the British Paper and Board Makers Association and the Technical Association of the Pulp and Paper Industry had essentially defined the moisture content of paper in terms of the direct oven-drying method as performed under closely specified conditions.Apart from the obvious handling difficulties arising from the rapidity with which the moisture content started to change on being introduced into new ambient conditions there were other difficulties in the oven-drying technique. ,4 major source of error was due to the relative humidity in a fresh-air oven which even at the recommended drying temperatures of 100" to 105" C. was some 1 to 2 per cent. the equilibrium moisture content of paper under these conditions might be as high as 1 per cent. This difficulty could be overcome by vacuum-oven drying but humidity cycling would be necessary to obtain a reproducible "zero per cent.relative humidity moisture content ." Moisture content by oven drying should be reproducible to ,toe2 per cent. Rapid drying techniques were not recom- mended if reliable moisture contents were to be obtained. If volatiles other than water were present moisture might be determined by the Dean and Stark technique of azeotropic distillation. Determinations of moisture by Karl Fischer reagent by reaction with calcium carbide or by room-temperature desiccation were not satisfactory for routine use. Moisture of paper on the paper-making machine could only be determined continuously by indirect methods. There were several methods by which the moisture content might be inferred from the operating conditions of the paper machine but of more general interest and application were continuous indirect methods based on the determination of moisture- dependent paper properties.Many such properties had been considered but most com- mercially available moisture meters depended on the variation of electrical resistance or capacitance with moisture content. For a wide range of papers the electrical resistance varied from about lo6 to 10l1 ohms as the moisture content varied from 22 to 4 per cent. Over this range a graph of log resistance against moisture content was essentially a straight line for a given paper; for different papers such a graph showed a series of roughly parallel lines whose displacement indicated that at the same moisture content papers might differ in resistance by a factor of 150. No completely satisfactory explanation of this difference in order of magnitude was available but it was probably connected with the mechanism of water sorption.The resistance might be measured either through or along the paper by using a.c. or d.c. methods. The dielectric constant of dry paper was 1 to 2 whereas that for water was about 80. For moist paper the dielectric constant was found to be a linear function of moisture content over the range 2 to 14 per cent.; for different papers the function differed by factors of up to 4. A capacitor having moist paper as a dielectric material hence had a capacitance that was directly related to moisture content. Moisture meters with. parallel-plate capacitors were not as a rule satisfactory and fringing-field capacitors operating at frequencies of 1 Mc/s upwards were almost invariably used. A new capacitance-type moisture meter extended the potential range up to some 400 per cent.of moisture as measured on an oven-dry basis. Both resistance and capacitance moisture meters were preferably calibrated under operating conditions. In practice this might be extremely difficult and many such meters July 19641 REPORTS OF MEETINGS 83 were satisfactorily used as “deviation meters,” with an arbitrary scale as part of a closed-loop system for control of the drying section of the paper machine. Indirect moisture meters were in general affected by paper-making variables other than moisture e.g. basis weight fillers and pH it was necessary to control these variables independently if satisfactory moisture measurement on the paper machine was to be achieved. The Application of Nuclear Magnetic Resonance to the Measurement of the Moisture Content of Coals and Cokes BY w.R. LADNER (British Coal Utilisation Research Association Leatherhead Surrey) DR. LADNER discussed the use of broadline nuclear magnetic resonance for moisture determination under three main headings (i) the principles involved in a nuclear magnetic resonance experiment (ii) the apparatus required for nuclear magnetic resonance moisture measurement and (iii) the results of some experiments mainly made on coals and cokes; but brief mention was included of those for fertilisers peat and iron ore. He said that nuclear magnetic resonance depended on the absorption of energy by a nucleus when it was subjected simultaneously to a strong homogeneous magnetic field and to radio-frequency radiation.I t was possible to make use of nuclear magnetic resonance to measure moisture since the nuclei of the hydrogen atoms in water exhibit pronounced resonance absorption. Moreover because the shape of the resonance signal (i.e. graph of energy absorbed veysus magnetic field for a given radio frequency or ueysus frequency for a given field) was critically dependent on the precise environment of the hydrogen atoms it was possible to distinguish between the hydrogen atoms in water sorbed on a solid and those chemically bound in the solid. The chemically bound hydrogen within the solid gave rise to a broad and weak resonance signal whereas the water produced a comparatively strong and narrow signal that could in favourable circumstances be used to measure the amount of moisture present.The much greater mobility of the hydrogen atoms in the water molecules compared with that of the hydrogen in the solid accounted for these important differences in beha\-iour . The nudear magnetic resonance apparatus that he described consisted basically of a large permanent magnet (1 ;-inch gap; 5-inch diameter poles) giving a highly homogeneous field of 3750 gauss a quartz-crystal oscillator (frequency 16 Mc/s) to provide the radiation and a parallel resonance circuit comprising the sample coil and a variable condenser for detecting the resonance. The effective sample volume was that of a cylinder 2 inch in diameter and 2 inches in length and corresponded to a coal sample of about 10 g. The nuclear magnetic resonance signal produced by this simple arrangement was relatively weak.To improve the strength of the final nuclear magnetic resonance signal the magnetic field had been modulated at a low audio frequency permitting phase-sensitive detection to be employed the final resonance signal appearing on the first derivative of the absorption signal. The peak-to-peak amplitude of the deril-ative signal was taken as the measure of the amount of water. Neasurement on both stationary and moving samples had shown that a narrow signal was obtained not only for the liquid water on the surface of the coal or coke particles but also for that adsorbed within their pore structure. Samples of three coals (81 85 93 per cent. carbon; dry mineral matter-free basis) ground to pass a &-inch R.S. mesh sieve had been tested. For batch samples the total moisture content could be determined with an accuracy of & 1 per cent.over the range 3 to 30 per cent. by using a single calibration curve. However the resonance signals for the two coke samples tested were weaker than those obtained for the coals. The strength of the signal also varied from one coke to the other and it was believed that this had been due to the presence of ferro-magnetic material. Measurements on a mo\-ing column of wet coal were also described; these were limited to the 81 per cent. carbon coal with moisture contents less than 15 per cent. because of the difficulties encountered in packing and moving the wet coals and cokes. I t was suggested that a form of horizontal worm feed might overcome these difficulties. 84 REPORTS OF MEETIKGS [Proc. SOC. Anal. Chena. An Introduction to Microwave Moisture Measurement BY H.B. TAYLOR (A ssoczated Electi/ical Industvzes L t d . Electiroii i c -1 ppai(atits Diz1isi o i l L e i cestrv) MR. TAYLOR said that the use of microwave techniques as a means of measuring the water content of materials was relatively new having been first investigated in this country bv the D.S.I.R. Building Research Station in 1956. The interest aroused bv this new approach to the problem of measuring water content had been great and as a result several materials had been measured to assess the value of these techniques for industrial purposes. The principle on which the technique was based was that of measuring microwave losses and he described the technique briefly. He also described equipment for making loss measurements at two different frequencies and the methods used for different types of material.These measurements combined with a knowledge of the water content permitted calibrations to be prepared so that the microwave equipment could then be used as a moisture meter. Several factors that could affect the performance in this r61e were discussed by the speaker. Some of these arose as the result of using microwaves others were inherent in the tvpe of material. Consideration of some of these factors had led to the proposal for a hypothetical curve representing the general relationship between losses and water content. The speaker illustrated graphically some results of measurements made at different frequencies. These indicated partly the range of interest and the kind of accuracy obtain- able. These results were compared with the estimated losses for pure water and an analysis made in terms of the nature of the materials.The possibility of using the techniques for continuous indication of water content was described with some ideas on the kind of sample control that would be necessary. Brief mention was made of the techniques required for low water-content measurement. 2 per cent. and & 6 per cent. of the total water content had been achieved and that each material would require individual stud\. and calibration. Broadly speaking the curve relating microlvave losses and \vater content could be accounted for in terms of the loss tangent for pure n-ater modified bj- the presence of binding forces and conducting salts. The conductility effects although smaller at high frequencies could not be ignored in some materials. The use of microwaves presented the possibility of continuous monitoring without the necessit!. for electrical contact with the material. I t also provided a possible means of exploring the interaction between water and material at molecular levels. In conclusion it was stated that accuracies of between

ISSN:0037-9697    

DOI:10.1039/SA9640100082

出版商:RSC    

年代:1964

数据来源: RSC

摘要:

REPORTS OF MEETISGS 85 Organic Reagents for Metals ? ? lhe follorving are summaries of papers presented at the Joint Meeting of the North of England Section and Microchemistry Group held on May Sth 1964 and reported in this issue of the Proceedifigs (p. 7 7 ) . Organic Cornplexing Agents as Reagents for Metals BY F. HOLMES (Chemistvjl Depavtment Univevsity College Barzgor Caevnnvzlonslzirej MR. HOLMES limited himself to a short discussion of organic reagents used directly in the determination of metal ions and omitted any reference to their use in masking reactions and their alteration of redox potentials. His chief concern was the extent to ~7hich theoretical considerations about complexes might be linked to practical aspects of designing new reagents. He began by outlining the derivation of formation constants and indicated their uses and limitations illustrating this with results for several aliphatic amines.The idea was developed of the importance of the shape of a polydentate ligand and the nature of the co-ordinating atoms in it. Jlr. Holmes then examined unselective reagents and considering EDTA4 as the most generally useful of these pointed out the way in which its properties could be altered by changing the bonding groups or by introducing new ones and b>- varj-ing the chain length. More specific reagents for transition metals were considered in the second half of the lecture. Polyamines oximes and similar compounds were discussed and their limitations enumerated. Consideration was given to the specific properties of dimethylglyosime and of substances similar to dipyridyl and to the chemical reasons for their selectivity discussed.n'ewer reagents of these two types were considered in some detail. Finally the lecturer speculated on the possibilities of obtaining new reagents that might ha\-e selective properties by reference to already used effects such as charge-transfer spectra metal - metal bonds or close-tailoring to fit a given metal ion. He concluded that the problems of designing completely different organic complexing molecules that could be specific for other metals of the periodic classification could not be solrred in this waj. if indeed it could be done at all. &4t present the best ways of achieving selectivity or specificity were by the standard analytical techniques such as masking and de-masking and it seemed as though this would continue to be true in general.A Precipitant Designed for the Precipitation of Palladium BY L. S. BARK AND D. BRAXDOK (DeFavtment of Chemistvy Royal College of Advaiiced Techizoiogji Salfoi/d) MR. BARK said that there were very few reagents that n.ere specific for one element although there were “selective reagents” containing functional groupings n.hich conferred reasonable specificity for a small number of elements. The vicinal dioxime grouping was reasonably specific for nickel and palladium ions. The analytical applications of vicinal diosimes had been recently reviewed by Banks. Dimethylglyoxime cyclohexane-1 J-dione diosime and 4-alkyl cyclohesane-1 ,2-dione dioximes had been recommended for nickel and palladium. Among the factors that influenced the choice of a reagent as a preciptant were- (i) The stabilitv of the metal chelate.(ii) The solubility of the metal chelate. The solubility was affected mainly by lattice energies the co-ordination state of the metal in the precipitate and in the solution and the steric factors that controlled the packaging 86 REPORTS OF MEETINGS [Yroc. SOC. ,4naL. Clzeiiz. of individual complex units together to form a polymer. The stability was influenced by the strength of the metal-ligand bonds which in turn were determined by the relative electronegativities of the two atoms and the amount of electronic overlap. I t was recognised that the palladium and nickel complexes of any vicinal dioxime did not have the same stability nor the same solubility and that the palladium complexes were the more stable and less soluble.Since for analogous complexes one had the same chelate and approximately the same relative electronegativities of the bonding atoms the increased stability and insolubility must have been substantial owing to the increase in the size of the metal species; this increase would result in- (a) greater palladium - nitrogen orbital overlap giving greater bond strength and ( b ) greater metal - metal orbital overlap resulting in a stronger bond holding the complex units together to form a polymer and giving a lower tendency to form hydrates and hence be solubilised by water. To make a vicinal dioxime more selective for palladium than for nickel it might only be This The only practical methods of varying the availability of nitrogen orbitals for overlap necessary to decrease the tendency for the oxime to form complexes with nickel.could be achieved by decreasing the probability of nickel - nitrogen orbital overlap. were- (i) To increase the metal - nitrogen separation. (ii) To introduce into the compound groups capable of withdra1ving electrons from the nitrogen atoms on to the carbon atoms. Although it was not always possible to separate these two effects it had been decided to concentrate on the former. This desired increase could only be achieved in the 5-membered chelate ring system containing the metal if the two angles subtended by the nitrogen atom and the 1,2-carbon atoms were increased. From a consideration of steric models of saturated alicyclic compounds with 5 to 10- membered rings containing the 1 ,%dioxime grouping and of aliphatic “straight-chain” compounds containing the vicinal dioxime grouping it could be seen that the angles subtended by the nitrogen atom and the 1,Z-carbon atoms were the same for all systems except the 5- membered rings.In a 5-membered ring the angles were increased and the nitrogen - nitrogen separation was increased. Such compounds were thus potentially less capable of forming analytically acceptable nickel complexes than was cyclohexane-l,2-dione dioxime. The parent compound cyclopentane-l,2-dione dioxime had been previouslv reported as being difficult to prepare and of no analytical significance for either palladium or nickel. The authors had considered that the compound indane-1,2-dione dioxime would be more useful since the “weighting effect” of the benzene nucleus would increase the sensitivity of the compound for precipitation.Classi- cal precipitation methods gave the expected quantitative yield of the palladium complex but even a few milligrams had been difficult to filter and prolonged washing had been necessary to ensure removal of excess of precipitant. Precipitation of the complex from homogeneous solution with in situ preparation of the dioxime from the corresponding monoxime had been considered. Two simultaneous reactions were possible- (1) Hydrolysis of dioxime to the monoxime in acid conditions to establish an equilibrium having only a small amount of dioxime present at any time in solution. (2) Immediate reaction of any dioxime with the palladium present to form a stable complex. If the metal complex had the expected high stability constant under the reaction condi- tions then reaction (2) predominated until all the metal was removed as a complex.Reaction (1) would prevent formation of any noticeable excess of the precipitant and hence gross contamination of the precipitate was avoided. Interference from other substances would be restricted to species forming insoluble complexes stable complexes that can be co-precipitated with the palladium chelate or to compounds formed by reaction with one of the reactants. This compound had been prepared and examined as a precipitant for palladium. July 19641 REPORTS OF MEETINGS 87 On precipitation of the palladium complex from homogeneous solution an easily filtered precipitate free from contamination was obtained. The effect of foreign ions or species on the precipitate had been investigated and the optimum analytical condition pH temperature duration of reaction had been determined by the usual methods. The overall time of determination compared favourably with that when niosime or substituted niosimes were used. Only gold and platinum gave noticeable interferences.

ISSN:0037-9697    

DOI:10.1039/SA9640100085

出版商:RSC    

年代:1964

数据来源: RSC

摘要:

July 19641 REPORTS OF MEETINGS 87 Galvanic Analysis The following is a summary of a paper presented at the Joint Meeting of the Midlands Section held on June 9th 1964 and reported in this issue of the Proceedings (p. 78). Galvanic Analysis BY P. HERSCH (Beckman Instrumeiats I n c . Fullerton California U.S.A .) DR. HERSCH said that for half a century the currents from certain self-powered electro- chemical cells had been used on occasion to determine oxidising and reducing species. Several patents had been issued for these methods but little or no place had been given them in the reference literature. In 1951 he had been surprised to find how easily minute traces of oxygen in other gases lent themselves to quantitative determination. The first cells that lie had used combined an inert cathode partly bathed by a solution of caustic alkali partly exposed to the gas sample with a mildly corrodible metal anode.Later galvanic systems of this tjTpe had become the heart of various commercial monitors for trace oxygen in inert and process atmospheres. Laboratory-made simple cells had served such diverse purposes as determining thc oxygen dissolved in a few microlitres of blood and other biofluids the continuous determi- nation of parts of oxygen per thousand million parts of boiler feed-water the detection of oxygen in gas-chromatographic effluents down to 0.01 pl or oxygen from photosynthesis of algae after flash illumination. The indirect analysis of traces of organics had become possible in terms of oxygen remaining after combustion and hydrogen in small samples of steel wire could be determined similarly at the part per million level.In the earlier flow cells the number of oxygen molecules reduced was only a fraction of the number present. The fraction depended on the individuality of each sensor and on tem- perature. They required neither calibra- tion nor attention to temperature. Moreover with new accessories linearity was no longer confined to small traces and the application of diffusion barriers extended it to 100 per cent. of oxygen (OJ. Already in 1952 it was predictable (Chenz. Age 1952 565; Ind. Chew. 1952 28 488) that primary cells could be designed as analysers for many species besides oxygen. In the first place traces of hydrogen in a stream of nitrogen or helium (apart from being measurable in terms of oxygen decrement after combustion) could be made to operate a fuel cell j-ielding enough energy to drive a galvanometer.Carbon dioxide in the atmosphere lent itself to continuous measurement by an enhancement effect on the air - platinum - potassium hydroxide - mercury system promoting the galvanic atmospheric corrosion of mercury. Fractional parts per million of elemental halogen or of nitrogen dioxide (and indirectly after oxidation of nitric oxide) could be monitored in air with a platinum screen cathode a buffered solution of chloride and an anode of activated carbon. Chlorine and bromine in aqueous media slowly filtering through a cathode of graphite felt and an anode of silver screen gave galvanic responses with quantitative output in accordance with Faraday’s law. The reduction of the halogens was amongst the most readily achie\-ed quantitative electrode reactions.I t was natural to try to determine electromoti\.ely less active or inactive species indirectly by causing them to form or to consume halogen. Thus fractional parts per million of ozone in an air stream were monitored through reaction with a neutral buffered solution of bromide PLUS a trace of iodide for catalysis. The solution recirculated in a loop Cells that absorbed all oxygen were now available. 88 PXPEKS ACCEPTED FOR PUBLIC-ITION [Proc. SOC. Anal. Chew. over a platinum or graphite cathode. The net effect in this cell was the oxidation of some site on the carbon surface at the expense of one of gen atoms of the ozone molecule. Carbon monoxide and numerous other reducent in air or other gases could be determined down to parts per million ranges by reaction with iodine pentoxide at about 180” C.carrying the resulting iodine vapour into a cavity- shaped cathode of platinum graphite cloth or graphite felt with a chemistry as for ozone. Strongly acidic vapours (HC1 HNO, SiF, ClSO,H CF,CO,H RCOC1 R,SiCl) were determined in a loop or cavity with iodate and iodide in the electrolyte. The coulombic yield from ozone carbon monoxide and acid vapours was theoretical. The technique might therefore be called galvanic “coulo-halometry.” Oxygen-bearing organics were often pyrolvsed over carbon to con\Tert oxygen to carbon monoxide for analysis. Likewise carbon and hydrogen in organics were determined in terms of carbon monoxide by first passing the vaporised sample over hot copper oxide and the resulting carbon dioxide and water over hot carbon. The new simple and highly sensitive “coulo-halometric” cell for carbon monoxide invited wider uses of these methods both for elemental analysis and in gas-chromatographic detection. Moreover batchwise as well as continuous determination of organic halogenates by thermal cracking (j-ielding SiF, HC1 Rr and I,) should benefit from the new sensors. Dr. Hersch drew attention to a review on the present state of galvanic analysis in Volume 111 of “,idvances in Analytical Chemistrv and Instrumentation,” Tnterscience Publishers Inc. Xew I-ork 1964. Again active carbon was a suitable anode.

ISSN:0037-9697    

DOI:10.1039/SA9640100087

出版商:RSC    

年代:1964

数据来源: RSC

摘要:

88 PXPEKS ACCEPTED FOR PUBLICITION [Proc. SOC. Anal. Chew. Papers Accepted for Publication in The Analyst THE following papers have been accepted for publication in The Analjlst and are expected to appear in the near future. “The Determination of Ascorbic Acid in Blackcurrant and other Coloured Fruit-juice “The Determination of Sulphur Dioxide in Beers and IT‘ines,” by G. ‘1.. Jones. “The Determination of Radiocerium in Biological Matter and Seawater,” by B. L. Hampson. “The Spectrophotometric Determination of Silicic Acid in Dilute Solution,” by H. E. Garrett and A. J. Walker. “,4 Sensitive Method for Determining Nitrate in If’ater with 2,6-Xylenol,” by D. \Y. IT. -4ndrews. “The Determination of Chromium in Biological Material by Radioactivation,” by H. J. 31. Bowen. “The Effect of Glycerol Added to Tobacco on the Constituents of Cigarette Smoke,” by J. E. de Souza and M. Scherbak. “The Use of Sintered Polymeric Carriers in Partition Chromatography and Electro- phoresis,” by T. R. Pierce and P. F. Peck. “The i4bsorptiometric Determination of Silicon in Water. Part IV. Method for Determining ‘Reactive’ Silicon in Power-station 1TTaters Containing Phosphate,” by H. M. Webber and A. L. Wilson. “Separation of Some Isomeric Ionones and Methyl Ionones by Multiple Thin-layer Chromatography,” by J. H. Dhont and G. 1. C. Diikman. Syrups,” by Lee Kum-Tatt and P. C. Leong.

ISSN:0037-9697    

DOI:10.1039/SA9640100088

出版商:RSC    

年代:1964

数据来源: RSC

摘要:

Jul!~ 19641 Changes in the Register of Members NEW MEMBERS 0 RD I NARY ME PVI BE RS .Abdel Kader Sayed Ahmad B.Pharm. & Pharm.Chem. M.Pharm. Dr. Pharm. (Cairo) ; S. J. Lennart Bgveryd M.Chem.Eng. ; Albert Emile Delvaux I>.%. (Louvain) ; Dalrid IT’illiam Ihclter B.Sc. (Manc.) D.Phi1. (Oxon.) ; Edward John Dixon B.Sc. Ph.D. (Shefield) ; Emparo 21. Escarrilla Ph.D. (Iowa) ; Keith Fisher A.K.I.C. M.R.S.H. ; Ole Garbers; Frazer Keith Elliott Imrie B.Sc. (Lond.) M.I.Bio1. ; William Frederick Jones R.Sc. F.R.I.C. ; Peter Knight A.R.I.C. A.M.C.T. ; Vernon Charles Kyte A.I.S.T. ; Morris ]Ir. Lerner R.S. (Mass.) 1I.S. (Tufts) Ph.I). (Rutgers) ; Bengt Aron Ingemar Sandberg Dr. Tech. (Stockholm) ; Ales- ander Sinclair A.R.I.C. ; Brian Arthur Sewell L.R.I.C. ; Pearson Lawrence Stott L.R.I.C. ; .John Alan Tetlow A.R.I.C. A.K.T.C.(S). JUKIOR MEMBERS Rajnish Kumar; Andrew Warwick Powell B.Sc. (Sydney) ; Ram Swaroop Sadana R.Sc. (*\gra).

ISSN:0037-9697    

DOI:10.1039/SA964010089b

出版商:RSC    

年代:1964

数据来源: RSC

摘要:

90 [Proc. SOC. Anal. Chem. Publications Received The publications listed below have been received by the Editor of The A m Z ~ ~ s t in which journal Book Reviews will continue to appear. CHIMICA GENERALE E INORGANICA. By the late GIUSEPPE BRUNI. Twelfth Edition. Revised and edited by GIORGIO RENATO LEVI and MARIO ALBERTO ROLLIER. Pp. xxiv + 724. Milan Tamburini Editore. 1964. Price L. 7,000. SOLUBILITIES OF INORGANIC AND ORGANIC COMPOUNDS. Volume 2. TERNARY SYSTEMS. Part 1. Edited by Prof. H. STEPHEN O.B.E. D.Sc. F.R.I.C. and DR. T. STEPHEN M.Sc. Ph.11. Pp. ii + 944. 1964. Price L12 10s. Edited by I. M. KOLTHOFF and PHILIP J . ELVIKG with the assistance of ERNEST B. SANDELL. Part I. THEORY AND PRACTICE. Volume 5. Pp. xx + 2707-3346. New York London and Sydney Interscience Publishers a division of John \Viley & Sons.1964. Price 120s. Od. Edited by H. A. BOEKENOOGEK. Pp. xiv + 421. New York London and Sydney Interscience Publishers a division of John Wiley & Sons Ltd. DETERMINATION OF pH THEORY AND PRACTICE. By ROGER G. BATES. Pp. xvi + 435. Kew York London and Sydney John Wiley & Sons Inc. CHEMICAL THERMODYNAMICS BASIC THEORY AND METHODS. By IRVING M. KLOTZ with advice and suggestions from THOMAS FRASER YOUNG. Revised Edition. Pp. xvi + 468. New York and Amsterdam W. A. Benjamin Inc. 1964. Price $9.75. INORGANIC REACTION MECHANISMS AN INTRODUCTION. Pp. xiv + 190. Sew York and Amsterdam W. A. Benjamin Inc. COORDINATION COMPOUNDS. By DEAN F. MARTIK and BARBARA B. MARTIS. Pp. x + 99. Sew York San Francisco Toronto and London McGraw-Hill Book Company. 1964.Price (paper) 15s.; (cloth) $4.95; 38s. 6d. ORGANOLEAD CHEMISTRY. By L. C. WILLEMSENS. Pp. 111. New York International Lead Zinc Research Organization. Free on request from the Lead Development Association 34 Berkeley Square London W.l. By IRVING M. KLOTZ with advice and sugges- tions from THOMAS FRASER YOUNG. New York and Amsterdam W. A. Benjamin Inc. 1964. Price $3.95. Pp. xiv + 375. h-ew York Plenum Press. 1964. Price $15.00. 1964. Price 15s. Oxford London New York and Paris Pergamon Press. TREATISE oh’ ANALYTICAL CHEMISTRY. ANALYSIS AND CHARACTERIZATION OF OILS FATS AND F A T PRODUCTS. Volume 1. 1964. Price 84s. Od. 1964. Price 100s. Od. By JOHN 0. EDWARDS. 1964. Price $7.00. 1964. hrrRoDuCTIoN TO CHEMICAL THERMODYNAMICS. Pp. xviii + 244. I R THEORY AND PRACTICE OF INFRARED SPECTROSCOPY.By HERMAN A. SZYMANSKI Ph.D. BRITISH STANDARDS YEARBOOK 1964. Pp. iv $. 759. London British Standards Institution. TABLES FOR IDENTIFICATION OF ORGANIC COMPOUNDS. Compiled by Prof. MAX FRANKEL Ph.D. and Prof. SAUL PATAI Ph.D. Second Edition. Pp. x + 301. Ohio U.S.A. The Chemical Rubber Co. 1964. Price 67s. 6d. Fifth Report of the Com- mission on Analytical Reactions of the Analytical Chemistry Division of the International Union of Pure and Applied Chemistry. London Butterworth & Co. (Publishers) Ltd. 1964. Price 32s. 6d. The contents ofthis book appear in Pure and AppliedChemistry VoZ. 8 No. 1. (1964) COMPREHENSIVE ANALYTICAL CHEMISTRY. Volume IIA. ELECTRICAL METHODS. Edited by CECIL L. WILSON Ph.D. D.Sc. F.R.I.C. F.I.C.I. and DAVID XV. \I7~~sopi M.Sc. F.R.I.C.in association with C. R. N. STROUTS M.A. F.R.I.C. Pp. xvi + 268. -Amsterdam London and New York Elsevier Publishing Company. 1964. Price 60s. (to subscribers to all volumes 50s.) REAGENTS AND REACTIONS FOR QUALITATIVE INORGANIC ANALYSIS. Pp. x + 88. July 19641 NOTICES 91 RADIOLYSIS OF HYDKOCARBONS. Edited by A. V. TOPCHIEV. English Edition Edited by 13. -4. HOLROYD. Pp. xii -+ 232. Amsterdam London and New York Elsevier Publishing Company. 1964. Price 65s. KIRK-OTHMER ENCYCLOPEDIA OF CHEMICAL TECHNOLOGY. Volume 3. B TO CALCIUM. Edited by HERMAN F. MARK JOHN J. MCKETTA jun. DONALD F. OTHMER and ANTHONY STANDEX. Second Edition. New York London and Sydney Interscience Publishers a division of John Wiley & Sons Inc. Price k l 6 18s. ; price per volume for subscribers to the complete set of 18 volumes L13. Pp. xii + 211. London John Murray. 1964. Price 30s. By ALBERT L. LEHNIN- GER. Pp. xxii + 263. New York and Amsterdam W. A. Benjamin Inc. 1964. Price 59.00. ORGAXIC CHEMISTRY. Volume 2. STEREOCHEMISTRY AND THE CHEMISTRY OF NATURAL PRODUCTS. By I. L. Finar B.Sc. Ph.D. A.R.I.C. Third Edition. Pp. xii + 690. London Longmans Green & Co. Ltd. 1964. Pp. xvi + 927. 1964. Foou SCIEXCE AND TECHNOLOGY. THE I V ~ ~ ~ ~ ~ MOLECULAR BASIS OF STRUCTURE AND FUNCTION. By MAGNUS PYKE B.Sc. Ph.D. F.R.I.C. F.R.S.E. Price 50s.

ISSN:0037-9697    

DOI:10.1039/SA9640100090

出版商:RSC    

年代:1964

数据来源: RSC