by this method. A special sampling technique has proved very satisfactory for these alloys.
American Association of Spectrographers
Spectrographic Analysis of Titanium Alloys Using Flat Metallic Samples. T. E. GREEN,P. R. Mallory h Co., Inc., Indianapolis, Ind. Titanium alloys containing aluminum-chromium, iron-vanadium, and iron-aluminum in amounts from 1 to 5% of each constituent appear to be readily adaptable to spectrographic analysis. Such analyses, while not so accurate as wet methods, may be more informative, as an ingot's homogeneity can readily be studied and at a great saving of time. Individual titanium alloy samples from 0.5-inch diameter to 30-pound ingots are satisfactory samples if their surfaces are flat and smooth.
HE Chicago Chapter of the American Association of Spectrographers held a Symposium on Instrumental Methods of Analysis in the Nonferrous Industry in Chicago, Ill., on Map 13. Abstracts of the papers presented are given here. Correlation of Entrance Optics with Analytical Accuracy in the G. WRIQHT,AND S. Direct-Reading Spectrometer. J. H. JURMAIN, H. WALTER,Baird Associates, Inc., Cambridge, Mass.
Direct-Reading Spectrochemical Method for the Analysis of Aluminum and Its Alloys. R. RAISIQASD C. J. TLAPA, Apex Smelting Co., Chicago, Ill.
Several characteristics of optical components and samples have been investigated as t o their effect upon analytical accuracy. The results of the study have been applied successfully t o routine analysis of nonferrous alloys.
.I direct-reading spectrochemical method for the analysis of aluminum and its alloys utilizes controlled spark excitation of the sample in an atmosphere of nitrogen. Some of the effects and particular advantages obtained by the use of a nitrogen atmosphere were discussed and illustrated. The method is particularly adapted to the analysis of a wide variety of aluminum alloys. A dilution method was briefly discussed as a means of extending the ranges normally handled by spectrochemical methods.
Spectrographic Analysis of Lead and Lead Alloy Storage Battery Metal. I. S. BUBESAND M. B. SEILER,Goldsmith Bros. Smelting Bi Refining Co., Chicago, Ill. Rapid and accurate methods of analysis of all constituents in high antimonial and soft lead have been developed with reference to battery manufacturers and government specitidations. The accurate determination of 3 to 12% antimony in lead was discussed in particular, as well as the comparison of a series of spectrographic and chemical results.
Analysis of Aluminum and Bronze Alloys by Means of X-Ray Philadelphia Naval Shipyard, PhiladelFluorescence. J. SHERMAN, phia, Pa. Following a brief presentation of the physical basis of x-ray fluorescence methods, the problem of interpretation of measurements for analytical purposes was discussed. Factors considered are preparation of specimens, precision, range of elements, and concentration and interaction of elements in multicomponent alloys. These factors were illustrated by the analysis of nickel, copper, and zinc in the range of 1to SO% concentration.
Spectrochemical Analysis of Type Metal Alloys by the Pointto-Plane Spark Technique. E. J. DUNN,JR., National Lead Co., Xew York, N. Y. A spectrochemical method is based on a controlled spark between the basic type metal electrode and the carbon rod. Nine different elements can be determined, including the major alloying element of antimony and tin. The physical structure of these alloys is important and photomicrographs were included to illustrate their metallographic appearance.
Society of Public Analysts
New Developments in Equipment for Nonferrous Analysis. J. A. SCHUCFI, Jarrell-Ash Co., Boston, Mass. Recent developments in equipment for the analysis of metals have resulted in the Jaco Spec-Lab. A description of this equipment was given, with particular reference to adaptability to nonferrous work. Details of the equipment and construction were illustrated.
T THE
Quantometric Analysis of Zinc Die Casting Alloys. M. F. HASLER AND B. R . BOYD, Applied Research Laboratories, Glendale, Calif. A particular multisource discharge was found which would permit sufficient accuracy for all elements with a single arcing. In a total elapsed time of arcing and recording of less than 40 seconds a complete analysis is obtained. The precision of analysis under these highspeed operating conditions is as good as has been reported by any other methods to date. Duplicate direct-reading recordings may be obtained, if desired. Graphs illustrating the precision were shown, as well as the working curves for the elements concerned. Spectrographic Analysis of the Precious Metals. I. S. BGBES, Goldsmith Bros. Smelting and Refining Co., Chicago, Ill. d procedure for the assay of fine gold and fine silver by spectrographic methods was described, as well as the analysis of phosphorus and impurities in silver brazing alloys. Plans for platinum metals assay and sweeps assay were discussed.
Spectrographic Analysis of Aluminum Alloys by Means of Low Inductance Alternating Current Spark Techniques. J. T. ROZSA ASD L. E. ZEEB, National Spectrographic Laboratories, Inc., Cleveland, Ohio. The practicability of using low inductance spark excitation for the analysis of aluminum alloys was discussed. Various parameters investigated to minimize the effect of alloying constituents include capacitanoe, inductance, size of sparked area, electrode form, number of discharges per half cycle, inert atmospheres, and peak voltages. Spectrographic Methods for the Analysis of Manganese Bronze Alloys. E. D. STAHL, H . Cramer Co. A spectrographic method has been developed for the analysis of the manganese-bronze alloys using a spark technique. All the impurity and alloying elements except copper and zinc are determined
meeting of the Society of Public Analysts and Other
A Analytical Chemists, held April 2 in London. the papers abstracted below were presented. Determination of Traces of Arsenic in Germanium Dioxide and Tetrachloride. S. T. PAYNE. The determination of arsenic by a direct Gutzeit test on materials rontaining germanium was shown to be unsatisfactory. Reproducible results have been obtained by extracting the arsenic with a chloroform solution of diethylammonium diethyldithiocarbamate after forming an oxalate complex with the germanium, and by completing the analysis by a modified Gutzeit test in which the hydrogen is generated electrolytically from a zinc-plated cathode. With a 5-gram sample of germanium dioxide or 5 ml. of germanium tetrachloride it is possible to determine as little as 0.10 p.p.m. of arsenic in the germanium material. Inorganic Chromatography on Cellulose. Determination of Thorium by Chromatography on Alumina and Cellulose Adsorbents and the Simultaneous Determination of Thorium and Uranium in Minerals and Ores. A. F. WILLIAMS. A method for the chromatographic separation of thorium from minerals and ores and its application to the quantitative determination of thorium in macro and micro amounts were described. The method can be applied to simple minerals, such as monazite, and to complex materials, such as samarskite and pyrochlor, which are very difficult to analyze by the classical analytical procedures. The method makes use of alumina as the principal adsorbent. Although thorium nitrate cannot be extracted from a cellulose adsorbent in the presence of phosphate ion by ether containing nitric acid, an extraction can be made from an alumina adsorbent. By the use of cellulose beneath the alumina, thorium nitrate can be extracted free from other ions. The method has been extended to the chromatographic determination of uranium and thorium in the same sample of material. Inorganic Chromatography on Cellulose. Spectrographic Determination of Micro Quantities of Thorium Separated by Chromatog-
1073
1074
ANALYTICAL CHEMISTRY
raphy from Minerals and Ores. G. IT. J. KINGSBCRY A N D R. B. F. TEMPLE. -I simple spectrochemical method was described for the determination of micro quantities of thorium separated by chromatographic methods from small samples of about 1 gram of minerals and ores. The extracted thoria is coprecipitated with lanthanum, which forms the matrix and acts as internal standard in the spectrographic analysis. The spectrochemical procedure alone has a standard deviation of *3% and has been operat'ed for ore concentrations betn-een 0.001 and 0.2% of thoria, only 1 gram of the original material being used. For concentrations above 0.2% of thoria, the amount of ore necessary is considerably reduced.
&ita meeting of the Physical llethods Group, April S, t,he following papers were presented: Measurement of Diffusion Current with Special Reference to the Tinsley Pen-Recording Polarograph. W. FVRNESS. The Tinsley polarograph (Model 1'3211) may be used with capacitance damping to record the average diffusion current during the life of successive mercury drops; alternatively it may be employed undamped to trace approximately the instantaneous values of diffusion current at maximum drop size. In the first case precision depends upon the time constant of the pen-recorder circuit, and accuracy is limited by the quality of the electrolytic condensers. In the second case, for a given drop rate, the peak values traced hy the pen-recorder depend mainly upon the viscosity of the dash-pot oil. Some limitations and advantages of the two methods in practical polarographic analysis were briefly discussed, and an oil of suitable viscosity was suggested. The relationship of the peak values, as recorded under various
conditions, to the corresponding values for the average diffusion current has been investigated with the aid of a silver voltameter. For several electroreducible substances in specified supporting electrolytes the ratio of the average diffusion current to the instantaneous current at maximum drop size differs significantly from the fraction 6/7 derived theoretically by Dekoviit; moreover, the observed values of the ratio vary from one electroreducible substance to another diminishing with increasing values of the diffusion coefficient. The extent of the variation is greater than would have been predicted from the recent equation of Lingane and Loveridge. but the change is in the expected direction. Hypochlorites and the Dropping Mercury Electrode.
E. S.
JENKISS.
dlthough the dropping mercury electrode might nor appear proniising for use in oxidizing media. perfect,ly reproducible results are obtained with dilute commercial hypochlorite solutions-a fact of analytical value. -4free mercury surface is instantly attacked h y hypochlorites, but this net reaction may be interpreted electrochemically, and this explains the observed double anodic-cathodic polarographic waves. Polarographic Determination of Tellurium in Selenium. OSBORN A N D J. G. C. COBB.
G. H.
The presence of small quantitie.? of tellurium in the selenium used in rectifiers is very harmful and the determination by normal cheniical methods of the amounts pyesent .i difficult. -1 polarographic method mas suggested by Schv-aer and Suchy, bur has not been found satisfactory in practipe. -1method has now heen developed which will determine accurately tellurium content,^ between 100 p.p.m. and 5 % in selenium metal.
lnternational Congress on Analytical Chemistry PRCL1MIN;ARY program has been arranged for the Inter-
L4national CongreEs on Analytical Chemistry, t o be held at
Olford, England, September 4 to 9, 1952, under the patronage of the International Union of Pure and Applied Chemistry. Sir Robert Robinson is president of the congress and Sir Wallace rlhers is vice president. The board of Section V , the .inalytical Chemistry Section of the International Union, will meet September 3 and 10, as Rrell as the following commissions of the section: Physico-Chemical Data, Analytical Reactions, Microtechniques, Terminology, and Expression of Analytical Results. There will also be a meeting of the Commission on the Study of Fats, of Section VI, .4pplied Chemistry. The three main congress lectures will be:
micro Scale. R. BELCHER,E. F. CALDAS,A K D 3. J, CL.ARK Birmingham University, England. BIOLOGICAL
Use of Protozoa in Analysis. L. H. HAMILTON, S. H. HUTBER, L. PROVASOLI, Sloan Kettering Institute for Cancer Research, S e w Pork. Use of Fungi for Determining Trace Metals in Biological MaL-nirersity of Bristol, England. terials. D. J. D. NICHOLAS,
.4SD
Quantitative Assay of Pyrogens by the Febrile Response in Rabbits. D. M. TENNENT, l l e r c k Institute, Rahway, N. J. ELECTRICAL METHODS
A Fundamental Approach to the Establishment of pH Standards. R. C. BATES,Xational Bureau of Standards, Washington, Research in Analytical Instrumentation. R. H. NCLLER, D. C. Determination of the Equivalence Point in Potentiometric Los illamos Scientific Laboratory, Los Alamos, N. M. Titrations. G. GRAN,Svenska Traforskningsinstitutet, StockValue and Economic Importance of Chemical Analysis in holm, Sweden. Industry and Manufacture. L. H. LAMPITT,J. Lyons 8: Go., Replacement of Standard Cell and Salt Bridge by Indicator Ltd., England. Electrodes and the Use of Nonaqueous Solutions in PotentiContemporary Assessment of the Place of Classical Methods ometry. E. BISHOP, King's College, University of Durham, Technical in Chemical Analysis. C. J. v . 4 ~NIEUWENBURG, England. University of Delft, Holland. Square Wave Polarography. G. C. BARKER. .4t,omic Energy Research Establishment,, Harwell, England. The folloning papers have been promised for the scientific Polarography of Tetrathionates. ITr. CULE DAI-IES AND 1'. Eessions: F ~ R S E Brotherton ~S, & Co., Ltd., Leeds, EngIand. \IICROCHE1IIC 4 L A N 4 LYSIS
A Countercurrent Micro Rotary Extractor as an Analytical Tool. R. SPENCE. ~ N D R. J. IT'. STREETOX,Atomic Energy Research Establishment, Haraell, England. Direct Iodometric Microdetermination of Oxygen in Organic ~ U C H E R , Bayer Works, Germany. Compounds. J. UNTERZ Gravimetric Estimation of Lead, Silver, and Mercurous Mercury on the Microgram Scale. HAMEDM. EL-BADRY.4YD CECILL. ~T-ILSOX, Queen's Universitv of Belfast. Determination of Fluorine in Organic Compounds Containing Bromine, Iodine, Sulfur, Phosphorus, and Arsenic on the Semi-
OPTlCAL 3lETHODS
Ultraviolet Absorptiometric Determination of Arsenic as 12Molybdoarsenic Acid. 11. G. ~ I E L L O AN ND CCIE WADELIS, Purdue Universitv, Lafayette, Ind. Ultraviolet Absorption Spectra of F'yridoxine and Related Compounds. AGNESK. L r s s . ~ S D R. A. MORTOS,University of Lherpool, England. Recent Advances in Infrared Spectroscopy with Reference to SHEPPARD, University of Cambridge, Analytical Applications. 1. England.
I015
V O L U M E 24, NO. 6, J U N K 1 9 5 2 Intensity Measurements with Time-Controlled Phototubes.
G. H. DIEKE, Johns Hopkins Cniversity, Baltimore, l l d . Colorimetry of Indicators. J. KISG, Government Laboratory, London, England. Identification by X-Ray Diffraction of Crystalline Inclusions in Glass. H . P. ROOKSBY, General Electric Co., Ltd., Wembley, England. Metals in Oils. Their Determination by Spectrographic Methods and the Errors Involved. A. J. HAM,J. NOAR,A N D J. G. REYNOLDS, Thornton Research Centre, Chester, England. RADIOCHEXZICAL
Activation Analysis of the Alkali Metals. M. T. KELLEY, Oak Ridge National Laboratory, Oak Ridge, Tenn. Analytical Chemistry of Astatine. A. H. W. ATEX, JR., Institute Voorkerphysisch, Onderzoek, Holland. Determination of Small Quantities of Uranium in Rocks and Minerals by Radioactivation. -4.A. SMALES,Atomic Energy Research Establishment, Harwell, England. Precision Alpha Counting with Special Reference to the Measurement of Standard Sources. R. HURST AND G. R. KILL,Stomic Energy Research Establishment, Harwell, England. Solvent Extraction of Group IIIB Metal Halides. H. h1. S. H. IRVING A N D F. ROSSOTTI, University of Oxford, England.
summary in English, French, and German. About 30 minutes will be allowed for each paper. Authors will not read papers, but give a brief introduction that will leave time for full discussion, The proceedings will be published in full after the congress, in the November and December issues of the Analyst. or in a special issue. *L large collection of exhibits has been arranged, illustrating new techniques or special applications of older techniques in analytical chemistry. A number of firms .n-ill exhibit modern apparatus and books. In addition t o scientific sessions, there will be social functions and excursions to places of intereet near Oxford, and a special program for ladies. Tours of the colleges will also be arranged. Accommodation for men has been reserved in Christ Church College, University College, bIagdalen College, Hertford College, and St. Peters Hall. Hotel reservations should be made direct. Oxford hotels include the Randolph, Mitre, Eastgate, Golden Cross, Kings’ Arms, Royal Oxford, and Isis. The final form of application for membership, together with the full program, will be available in a few weeks. Registration fee of $2 should be sent with application form.
ORGANIC COMPLEXES
Joint ACS-AAAS Meeting
Some Factors Controlling the Selectivity of Organic Reagents.
H. 11. K. H. IRVING, University of Oxford, England. Stability of Metal Chelates in Relation to Their Use in AnalF. FREISER, University of Pittsburgh, Pittsburgh, Pa. ysis.
1,lO-Phenanthroline and Mono-, Di-, Tri-, and Tetramethyll,l0-phenanthrolines as Chelated Copper Complex Cations. V. H. MCCURDYA N D G. FREDERICKSMITH, University of Illinois, Urbana, 111. Complexes Formed by Thorium and Uranyl Ions with Complexones. M. J. CABELL,Atomic Energy Research Establishrnent, Harwell, England. REPORTING OF RESULTS
Statistical Aspects of Analytical Determinations. W. J. National Bureau of Standards, Washington, D. C. Statistical Design in the Study of ,Analytical Methods. G. E. P. Box, Imperial Chemical Industries, Manchester, England. Statistical Methods in Radiochemistry. L. MARTIN, State Institute of Agronomics, Belgium. \-OUDEN,
ADSORPTION AIID PARTITION METHODS
Chromatography s. G. Gas Chromatography. J. GRIFFITHS, D. JAMES, AND PHILLIPS, Inorganic Chemistry Laboratory, Oxford, England. Gradient Elution Analvsis. R. J. P. WILLIAMS.Inorganic Chemistry Laboratory, Oiford, England. Gas-Liquid Partition Chromatography. A. J. P. MARTINAND A. T. JAMES, Sational Institute for hIedical Research, London, England. Chromatography of Larger Molecules. R. L. 11. SUNGE, Rowett Research Institute, Scotland. Instrumental Approaches to Paper Chromatography. DORIS L. CLEGG,Los Slamos Scientific Laboratory, Los Alamos, K. 11. Quantitative Inorganic Paper Chromatography. RIniE. A. IACOURT, G. SOMPIEREYNS, ASD G. WANTIEZ, Universite Libre de Bruxelles, Belgium.
c.
Ion Exchange Displacement Chromatography of Amino Acids and Organic Low Bases Using Ion Exchange Resins. S. W. PARTRIDGE, Temperature Station for Biochemistry and Biophysics. Applications of Ion Exchange to Analytical Chemistry. E. R. TOMPKIS’~. 1-niversity of California, Berkeley, Calif.
At the Xorthwest Regional 1Ieeting of the ERICAX AX CHEWSOCIETY with the American Association for the Advancement of Science, to be held in Corvallis, Ore., June 20 and 21, the following papers are scheduled for the Analytical Session on June 20. CAL
Determination of Free Acidity in Hydrolyzable Salt Solutions: G. J. ALKIRE,General Electric c o . Effect of High Beta Backgrounds on Proportional Alpha CountGeneral Electric Co. ing. D. G. MILLERA N D 31.B. LEBOEUF, Energy Dependence of End-Window Geiger-Muller Tube Efficiencies. U. L. UPSOS, General Electric Co. Construction and Calibration of a Simple Semiautomatic Microburet. U. L. UPSON,General Electric Co. Improved Spectrographic Analysis of Uranium-Base Materials by the Pyroelectric Concentration Method. J. L. DANIEL,General Electric Co. Further .4nalytical Procedures for Organic Mercury ComA N D V. L. MILLER.West Washinzton Exuounds. D. PELLEY periment Station. Colorimetric Determination of Glycerol. i\I. B. WILLIAMS A N D H. D. REESE,Oregon State College. Forms of Silicate ilvailable for Colorimetric Determination. D. TUSG-KHEICHOW.4ND R. J. ROBINSON, University of \\-ashington. Use of Dithizone in Acetonic Solution for Determination of Heavy Metals, Especially Copper. R . E. DELAVAULT, University of British Columbia. Determination of Bluminum in Zirconium Utilizing Ion E s change Separation. H. FREUND A N D F. J. LfINER, Oregon State College. Colorimetric Determination of Calcium with Ammonium PurOregon State Colpurate. J. H. MOSERAND 31. B. KILLIAMS, lege. A t the Chemical Education Session, two papers of especial interest to analytical chemists will be presented:
-
.Inalytical Chemistry a t the University of Oregon.
Iiuriz, University of Oregon.
A. H.
Analytical Chemistry a t Oregon State College. H. r a m s n , Oregon State College.
GENERAL
Solubilization Titration. A Rapid Method for the Analysis of Binary Mixtures of Organic Liquids. E. C. LUMBAND P. A. WINSOR,Thornton Research Centre, England. Quantitative Determination of Organic Halides. G. SamXON, Rubber Foundation, Holland. Aging of Precipitates. I 11. KOLTHOFF, University of lIinnesota, Minneapolis, Minn. Papers will be issued to registered members in preprint form before the congress meets. They will be in English, with a
Fifth Annual Summer Symposium. Michigan State College, East Lansing, ,Mich.. June 20 and 21 American Society for Testing Materials. Annual Meeting. Hotel Statler, New York, N. Y., June 23 t o 27 International Congress on Analytical Chemistry. Oxford, England, September 4 to 9 Sixth Annual Symposium on Modern Methods of Analytical Chemistry. Louisiana State University, Baton Rouge, La., February 2 to 6, 1953
