V O L U M E 2 5 , NO. 10, O C T O B E R 1 9 5 3 Structures. R. VIALLARD AND MLLE. MARCHETTI, University of Paris, Paris, France. The utilization of heavy water for the determination of water linked to solid substances was proposed by Viallard in 1950. The interest of the method of isotopic substitution resides in the possibility of studying the substances in conditions which are practically the normal conditions of hydration. The results obtained in the case of an artificial elastomer (Perbunan) and on organic glass (methyl methacrylate), resorting t o the densimetric technique of indirect analysis by means of a float, are explained. In view of an extension of the method to the study of macromolecular structures, a technique for the kinetic study of exchanges, brought about in view of the characterization of mobile hydrogens, has been perfected. Preliminary experiments on cellulose have made it possible t o separate neatly the exchange phase with water of hydration from the exchange phase with the mobile hydrogens of the polyose. These experiments will be pursued, utilizing the techniques of spectrographic determination in the infrared.
1575 particular case a preliminary study of the conditions of functioning of the counter is necessary, and this is one of the circumstances which limit the applications of tritium in this field. The technique described rests on the measurement of the activity of samples of hydrogen coming from the reduction of water furnished by the semimicrocombustion catalyzed by the tritiated substance. The effect is made once for all and the operations, in part automatic, are accomplished by means of a standardized apparatus. The ensemble, presented in the Salon de la Chimie, is made up of a row of burners for the oxidation of the substance and the condensation of the water of combustion, a furnace for the preparation of the hydrogen, a bank of special counters, and a totalizer of electronic impulses for the counting of the particles emitted.
Characterization of the E5ciencp of Distillation Column of Fixed Packing. H. BRUSSET A N D E. CHAHVEKILIAN, Laboratoire de Chimie Industrielle de 1’Ecole Centrale, Paris, France. We present a critical study of the notion of number of theoretical plates equivalent t o packed distillation columns, in the light of the “theory of interfacial films.” We mention factors capable of induencing the efficiency of such columns: nature and physical characterisAdaptation of Apparatus for Determining Carbon-Hydrogen, Oxygen, and Nitrogen to the Analysis of Certain Complex Substances. tics of the mixture, coefficient of relative volatility, flow of liquid and J. GARACH, Service des Recherches Chimique, AND G. VALDENEX, of vapor, titer of the mixture, distillation pressure, employment of Service des Goudrons et DQrivBs,Gaz de France. theoretical plate, etc. The equivalent height of a theoretical plate is more or less a function of all these factors. The height of a unit Micro and semimicroanalytical methods for the determination of of transfer depends equally on most of these same factors, and t o a the constituents of organic compounds cannot be applied to certain degree more important than is predicted by the theory. We concomplex molecules without special precautions. The authors have sider the problem of the practical determination of the efficiency of studied and adapted these methods to the dctermination of carbona column and the conditions that must be fulfilled by the standardhydrogen, oxygen, and nitrogen in the heavy products of the gas ized mixtures utilized either at atmospheric pressure or at pressures industry. At the same time they have tried to make the use of the from 1 mm. of mercury. apparatus easier and more rapid without sacrificing precision and accuracy given by operations in series. Laboratory Cycloconcentrator. G . DUCELLIER. The Ducellier cycloconcentrator is an apparatus composed of a Elementary Analysis of Organic Fluorine Compounds. l f . BELboiler for recovering condensed water and a concentrator with no C H E R , University of Birmingham, Birmingham. England. moving parts, permitting autorotation of the liquid t o be concenWhen fluorine is present in an orgnnic compound i t is ordinarily trated. A projection cylinder permits spreading the liquid in thin neceixiry to modify the conventional method of determining a parsheets on the sides of the concentrator. The volume of liquid can he ticul.ir clement. Ectimation of fluorine is complicated also by the reduced t o one tenth. difficulty of decompoaing its derivatives comiJetely, and by tile fact t h a t the methods of dctermination of the hydrofluoric ion leave someNew Methods of Organization for Quantitative Analysis. R . thing t o be desired. BELCHER, University of Birmingham, Birmingham, England. Cp to now thc following procedures have been pcrfectcd sufficiently for work i n series. Study of the Pneumatic Classification of Powders from 1 to 100 1)etermination of carbon and hydrogen. Microns on a Laboratory Scale. TH.REIS. Dererniination of fluorine (on a semimicro scale) in presence or ab-cmce of nitrogen, sulfur, other halogens, phosphorus, and arsenic. Determination of fluorine (on an entirely micro scale) in prcience Study of Chromatography. R. GRADE. or abvnce of nitrogen, sulfur, and all other halogens. Determination of chlorine. bromine, iodine. in presence or absence Microelectrorheophoresis. Application to Proteins, Amino Acids, of 4 f u r and nitrogen. and Sugars. M. MACHEBOEUF (deceased), P. RIBEYROTTE, AW Determinarion of traces of hydrogen in fluorinared hydrocarbons. J. M. DUBERT,Institut Pasteur, Paris, France. The methods for the determination of sulfur and nitrogen are still under investigation. New Method Based on the Variation of a Capacity Permitting Multiple Records of Small Differences of Pressure in Chemistry Analytical Technique for the Determination of Tritium in Organic and Biology. TH. GAST. Compounds. MME. CORVALAND MESSRS. DREYFUS,GRENON. HERMANN, AXD VIALLARD, University of Paris, Paris, France. Dense Fluids and Their Industrial Applications. G. HULOT,Soci6t6 d’Etudes Chimiques pour 1’Industrie et l’Agriculture, France. A certain number of authors have utilized tritium as tracer for the study of reactions of organic chemistry. As tritium emits beta Application of the Thermobalance to the Determination of a particles of weak energy, most of these authors have measured this radioisotope by means of counters in which are introduced samples Mixture of Lime, Magnesia, Calcium Carbonate, and Dolomite. M. GIBAUDAND M. GELOSO,Faculty of Sciences, Paris, France. of one of the volatile compounds used in the experiments. I n each
Section of Analytical Chemistry, International Union meeting of the International Union of Pure and Applied A Chemistry, held in Stockholm, C. J. Van Nieuwenburg, T THE
Delft, Holland, president of the Section of Analytical Chemistry, presented a report of t h e activities of the section from September 1952 to August 1953. T h e Subcommission on Stability Constants of Complexes, Commission on Physicochemical D a t a of Analytical Interest, has collected stability constants of complexes of about one half of t h e inorganic cations. It is hoped t h a t this phase of the work m a y b e finished in 1954. T h e Subcommission on Absorption Spectrography will soon sub-
mit a partial list of extinction coefficients of organometallic compounds of analytical interest. T h e Subcommissions on Polarographic Data and Potentiometric Data are critically reviewing the literature on half-wave potentials and diffusion current constants. L. G. Sill& has been recommended as a liaison member of the Commission on Physicochemical Symbols and Terminology of t h e Section of Physical Chemistry. T h e subcommissions are also engaged in making recommendations in the field of p H standardization. A program is being planned on t h e compilation of dissociation constants of weak acids and bases.
ANALYTICAL CHEMISTRY
1576 The Subcommission on Osidation-Reductio11 1’otc:iiti:ils is making a critical survey of thermodj-namic and formal I)otcntials of various systems. The Commission on hlicrotechniques has collected extensive data on microchemical activity throughout the world and came to a preliminary under d i n g about the nomenclature of niicroweights and measures. The Commission on Terminology issued preliniinary reroiiimendations for format of methods. The secretary conipiled :L list of definitions of statistical concepts for discussion with the International Statistical Inntitutr’s committee 011 the same subject. The Commissioii 011 Analytical Reactions finished its work on the first report on colorimetry presented by ClCnient Duval, which has been handed to the General Secretary of the Virion for publication as the first monograph of the Union. Thc c,sperimental work for a second ci,itical report on colorimetry hws been divided among members of the commission. At the Stockholm Conference the section held two plenary meetings and came to the following oonrlusions. I t accepted the proposal of the Commksion on LIicrotechniques to hold (t Symposium on Microchemistry in Switzerland in 1955 and authorized P. E. Wenger t o open negotiations in Switzerland. I t accepted the task of compiling data on molecular spectroscopy, at the request of the Section of Physical Chemistry. Thr suggestion of Panta Tutundxik to employ the coulomb as the fundamental standard unit for measuring and expressing C O I I centration was referred to the president of the section for study. It was decided to t r y to convince ANALYTICAL CHE~IISTRY and The Analyst of the desirnhility of publishing summariep of papers in two other languages. The Cfiscllschaft Deutscher Chemiker undertook to take care of translation into German without chargr. German and French journals will be approached later. Five new members of the Section Committee %ere elected: president, 1953-57, I. M. Kolthoff (Cnited States); vice president, Ralph Chirnside (Great, Britain); G. Duyckaertr (Belgium); >I. K. Zacherl (Austria); I,. G. R i l l h (Sweden): aiitl C. J. Van Yieuwenburg (Holland). The Commission on Physicochemical Data held two meetings :Lt which it discussed the progress of reports in preparation. I t decided to spIit into three separate commissions t o cover electrochemical data, optical data, and equilibrium data. The Commission on New Reactions discussed the experimental work on the second report on colorimetry and, acting on a suggestion made by Professor Veibel to start a critical study of the malysis of organic functional groups, appointed Professors Duval and Veibel to investigate what should be done, starting with the aldehyde group.
Society of Public Analysts E
meeting of the Korth of England Section of the Society of Public Analysts and Other Analytical Chemistq, held May 2 n t Liverpool, W. Gordon Carey and J. G. Sherratt introduced a c+oniprehensivediscussion on the nnalysis of waters, sewages, and rmuents. The 16th Summer Meeting of the section was held a t Llandudno from June 12 to 15. A paper on.“Random Reflections on Food T,cy$slation” was presented by C. A. Adams. THE
The new food and drug bill now being drafted for piesentation to Parliament is a matter of outstanding importance to public analysts and chemists engaged in food manufacture, and also to the general public as buyers and consumers of food. On the interest shown by the public much of the success of the bill will depend. The outstanding interest in the bill is in the powers sought to transfer temporary wartime legislation into permanent form and in additional powers that might be necessary to deal with the addition of chemicals to food, whether intentional in the course of manufacture, or adventitious in
the forni of pesticide residues or in any other way. These matters have recently been the subject of official inquiry in the Cnited States, and were dealt with a t length by J. R. Nicholls in his recent presidential address, and were summed up from the official angle by the lord president of the council in the annual report of the ddvisory Council on Scientific Policy a year ago. The main value of a change in the law would be in relation to the use of chemicals newly introduced into the food industry. If the orders under the Defence (Sale of Food) Regulations, 1943, were included in the new bill, it would make them unalterable without appeal to Parliament. Instead, fuller powers t o make such orders would be sought in the bill and the orders could then be re-enacted. Pride of place was allotted to the labeling of food orders and the food standards orders, all of which had been enforced by the food and drugs authorities a8 though they were part of the Food and Drugs Act. Welcome progress has been made in the “cooperative administration of food legislation.” If the range of the Food and Drugs Act is to be extended to cover problems arising from the use of cheniicals, pesticide residues, and the sale of substandard products, now is the time to make recommendations; once the bill becomes law further changes may belongdelayed. The Summer Sleeting of the Biological >lethods Group consisted of n. visit t o the Ministry of Agriculture and Fisheries’ Veterinary Laboratory, New Haw, Weybridge, Surrey, where members were shown work in progress in biochemistry, manufacture of vaccines, tuberculin production, poultry disrases, and manufacture of S.19 Brucella abortus vaccine. The Xorth of England Sect’ion and the Microchemistry Group met with the Liverpool and S o r t h Western Sections of the Royal Institute of Chemistry in Southport on September 25 and 26. Simpson’s Gold Thread Korks and the Victoria Colliery were visited and a Symposium on the Training and Education of Microchemists was held. C. L. Wilson spoke on “The Academic Approach,” Gerald Ingram on “Technical Aspects,” and Rudolph Rothwell on “Industrial Requirements.”
Infrared Spectroscopy The Department of Physics, Tennessee Agricultural and Industrial State University, Sashville 8, Tenn., wishes to a m o u n c e the availability of the facilities of its infrared spectroscopy laboratory to the chemical research laboratories of universitirs and industrial concerns in the Poutheastern region.
Society for Applied Spectroscopy The Society for Applied Spectroscopy nil1 meet November 10 a t the Hotel S e w Yorker, Sexy York, N. Y., for an informal dinner a t 6 P.M. At 8 P.Y. G. E. Peterson and E. IT. Currier, Federal Telecommunication Laboratories, Inc., will discuss the quantitative analysis of selenium. Secretary of the society is C. A. Jedlicak, U. S. Testing Co., Inc.. 1415 Park Ave., Hoboken, S . J.
Conference on Applied Mass Spectrometry. Institute of Petroleum. Hydrocarbon Research Group. London, England, October 29 and 30 Eleventh Annual Pittsburgh Diffraction Conference. Mellon Institute, Pittsburgh, Pa., November 5 and 6 Louisiana State University Analytical Symposium. Baton Rouge, February 1 to 4, 1954 Fifth Pittsburgh Conference on Analytical Chemistry and Applied Spectroscopy. William Penn Hotel, Pittsburgh, Pa., March 1 to 5, 1954 1
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