HIGHLIGHTS OF THE SCIENTIFIC A N D TECHNICAL ARTICLES IN THIS ISSUE Time Resolution in Spark Source Mass Spectrometry
Analytical Applications of X-Ray Excited Optical Fluorescence Spectra: The Internal Standard Principle An internal standardization principle is described that compensates for interference effects caused by impurities present a t the ppm level in the host matrix.
The electronics necessary for pulse synchronization, instrumental requirements, a method of data reduction, and preliminary results of a study of the time variance of the ion beam emanating from an rf spark source are discussed.
E D W A R D L. DeKALB, VELMER A. FASSEL, TAKESHI T A N I G U -
C. A. EVANS, JR., and G. H. MORRISON, Department of Chemistry, Cornell University, Ithaca, N. Y. 14850
Department of Chemistry, Iowa State University, Arnes, Iowa 500 I O
Anal. Chem. 40, 2 106 (1968)
CHI,and T. R. S A R A N A T H A N , Institute for Atomic Research and
Anal. Chern. 40, 2082 (1968)
Determination of Sub-Microgram Quantities of Mercury by Atomic Absorption Spectrophotometry A reduction-aeration procedure is employed to produce and introduce mercury rapor into a closed system where the absorption of the 2537 A line is measured in a quartz w-indowed cell. W. R O N A L D H A T C H and W E L L A N D L. OTT, Falconbridge Nickel Mines Limited, Metallurgical Laboratories, Thornhill, Ontario, Canada
Studies on the Anion Exchange Behavior of Carboxylic Acids and Phenols Conclusions are drawn regarding the ion exchange behavior of carboxylic acids and phenols by a study of their sorption by a macroreticular anion exchange resin over a wide range of p H in aqueous-organic jolrent mixtures. JAMES S. FRITZ and A K I R A TATEDA, Institute f o r Atomic Research and Department of Chemistry, Iowa State University, Ames, Iowa 50010 Anal. Chern. 40, 21 I5 (1968)
Anal. Chem. 40, 2085 [ 1968)
Enhancement of Zirconium Atomic Absorption by Nitrogen.Containing Compounds and I t s Use in the Determination of Ammonia Nitrogen-containing compounds acting as Lewis bases enhance the absorption of zirconium in the nitrous oxideacetylene flame. A practical application is the determination of ammonia in biological material. A. M. BOND, Department of Inorganic Chemistry, University of Melbourne, Parkville, Victoria, Australia 3052, and J. B. WILLIS, Division of Chemical Physics, CSIRO Chemical Research Laboratories, P. 0. Box 160, Clayton, Victoria, Australia 3168 Anal. Chem. 40, 2087 (1968)
High Resolution Mass Spectral Photoplate Data Acquired and Reduced with a Real Time Remote Time4hared Digital Computer The procedure and the data presented illustrate the accuracy obtained by direct on-line communication between a microdensitometer-comparator system measuring photoplates and a remote digital computer which is involved in decision making during the data acquisition step.
D. M. DESlDERlO JR., and T. E. MEAD, American Cyanamid
Co.,
Stamford Research Laboratories, Stamford, Conn. 06904
Copper (I11 Oxidation of Thioureas in Acetonitrile The oxidation of a series of thoiureas by copper(I1) in acetonitrile and the nature of the intermediates formed in the oxidation process are reported. DAVID A. Z A T K O and BYRON KRATOCHVIL, Department of Chemistry, University of Wisconsin, Madison, Wis. 53706 Anal. Chem. 40, 2120 (1968)
Mixed-Metal Hydroxycarboxylic Acid Complexes. The Chromium (111) Inhibition of the Solvent Extraction of Indium(lll1 Hydroxycarboxylic acids both shoving and not showing the inhibitory effect of chromium on the extraction of indium are presented, as well as data indicating that complexes of several of these acids with more than one kind of metal can have high stability. T. W. GILBERT, Chemistry Department, University of Cincinnati, Cincinnati, Ohio, and LEONARD N E W M A N and PAUL KLOTZ, Brookhaven National Laboratory, Upton, N. Y. Anal. Chem. 40, 2 123 (1968)
Anal. Chem. 40, 2090 (1968)
Photometric Determination of Substances in Presence of Strongly Interfering Unknown Media
New Extraction Chromatographic Method for Rapid Separation of Americium from Other Transuranium Elements
The method of changing parameters. which yields results with an accuracy that is dependent upon the precision of the measuring device used, is introduced for the determination of substances in the presence of interfering media.
Extraction chromatography with a Teflon-HDEHP column is used to separate Am(\-), obtained through an oxidation-reduction sequence, from C m ( I I I ) , other actinide (111, IV, VI) ions, lathanide (111. I\’) ions, and other metal ions.
A D A M SHATKAY, Isotope Department, The Weizmann Institute of Science, Rehovoth, Israel
FLETCHER L. MOORE, Analytical Chemistry Division, Oak Ridge National Laboratory, Oak Ridge, Tenn.
Anal. Chern. 40, 2097 (1968)
Anal. Chern. 40, 2130 (1968) VOL. 40, NO. 14, DECEMBER 1968
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Packard offers stimulating carder opportunifies for scientific and technkal personnel. Wa are an equal opportunity sntp1oyar.Circle No. 61 on Readers' Service Card
Vapor-Programmed Thin-Layer Chromatography, A New Technique for Improved Separations The apparatus described provides for more efficient control of the vapor processes during derelopment. Closely related substances which are inadequately separated by classical TLC techniques can now be identified through the use of vapor-programmed TLC. ROKUS A. de ZEEUW, Laboratory for Pharmaceutical and AnaChemistry, State University, Antonius Deusinglaan 2, Groningen, The Netherlands lytical
Anal. Chem. 40, 2134 (1968)
Rapid Separation by Carbon Number and Dete rmination of Na pht he ne and Paraffin Content of Saturate Petroleum Distillates up to 185 " C Type 13X molecular sieve is used for the separation. The influence of temperature and column length has been examined and the conditions necessary for analysis and collection of the separated naphthene and paraffin components have been established. J. V. BRUNNOCK and L. A. LUKE, The British Petroleum Company Limited, BP Research Centre, Chertsey Road, Sunbury-on-Thames, Middlesex, England Anal. Chem. 40, 2 158 (1968)
2,6-Dichloroquinone-4-Chloroimide as a Reagent for Amines and Aromatic Hydrocarbons on Thin-Layer Chromatograms 4 survey of the range of utility of 2.6-dichloroquinone 4chloroimide is reported. Amines, other nitrogen and oxygen compounds, and hydrocarbons were investigated as well as several chromatographic variables. JOSEPH H. ROSS, Indiana University, South Bend, Ind. 46615 Anal. Chem. 40, 2 138 (1968)
Pyrolysis-Gas Chromatography of Hydrocarbons This paper is an attempt to form standard methods for the reporting of PGC data analogous to that used in reporting mass spectra. The results of the vapor phase pyrolysis of 83 different hydrocarbons are reported. DALE L. FANTER, JOHN Q.WALKER, and CLARENCE J. WOLF, Research Division, McDonnell Douglas Corp., St. Louis, Mo. 63 I66 Anal. Chem. 40, 2168 (1968)
Resolution and Optimization in Gel Filtration and Permeation Chromatography Included among the factors discussed are plate height and optimum velocity, temperature, and solvent, optimum pore size and retention based on geometric similarity, and examples of resolution as related to molecular size differences.
Improved Techniques for Corrosive Fluoride Gas Chromatography A column based on fluorocarbon oil, techniques for more sensitive analysis of reactive fluoride compounds, and a stepped-up column mrangement which speeds up an analysis without storage of fractions are described.
J. C A L V I N GIDDINGS, Department of Chemistry, University of Utah, S a l t Lake C i t y , Utah 841 I2
W. S. PAPPAS and J. G. M I L L I O N , Laboratory Division, Oak Ridge Gaseous Diffusion Plant, Union Carbide Corp., Nuclear Division, Oak Ridge, Tenn.
Anal. Chem. 40, 2 143 (1968)
Anal. Chem. 40, 2 I76 ( 1968)
Visual Titrimetric Determination of Total Reactivity and Differentiation of Trialkylaluminum and Dialkylaluminum Hydride in Mixtures Aluminum trialkyl and aluminum dialkyl hydride can be determined either in mixtures or separately by titration with pyridine using phenazine as the indicator. D O N A L D E. J O R D O N , Research and Development Department, Continental Oil Co., Ponca City, Okla. Anal. Chem. 40, 2150 (1968)
Resolution of C4to CI2 Petroleum Mixtures by Capillary Gas chromatography The present study determines the resolution of the hydrocarbons mhich occur in the C, to Clr portion of nonolefinic petroleum by using a mixture of squalane Kel-Flo as the substrate.
+
Electrochemical Reduction of Beta-Diketones in Dimethylsulfoxide Dibenzoj-lmethane (DBMH) and other p-diketones are electrochemically reduced with DMBO as the solvent. The acidity of the species formed, the neutral enol, results in complex electrochemical behavior because of the formation of radicals. R A Y M O N D C. BUCHTA and DENNIS H. EVANS, Department of Chemistry, University of Wisconsin, Madison, Wis. 53706 Anal. Chem. 40, 2181 (1968)
Effect of Static Magnetic Field on Direct Current Polarography The theory of magnetohydrodynamics is used to explain, in terms of the retardation of tangential motion of the mercury surface, the mechanism of the effect of magnetic field on the second kind of maxima.
PHILIP MERCHANT, JR., Dow Chemical Co., Pilot Plant Laboratory, Texas Division, Freeport, Texas
SHIZUO FUJIWARA, Y O S H I O U M E Z A W A , and TERUHIKO KUGO, Department of Chemistry, Faculty of Science, The University of l'okyo, Bunhyo-ku, Tokyo, Japan
Anal. Chem. 40,2 153 [ 1968)
Anal. Chem. 40, 2186 (1968) VOL. 40, NO. 14, DECEMBER 1968
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Notes Fluorescence of Prostaglandin El Reproducible fluorescence for prostaglandin El, in the range of 0.5 to 2.5 pg, is obtained in a 70% H,SOd-HnO solution heated a t 65 " C for 30 min and cooled to 15 "C for another 30 min. Samples are activated a t 365 mp and read at 420 mw. C. L. GANTT, L. R. KIZLAITIS, D. R. T H O M A S , and J. 6. GRESLIN, Clinical Research Center, Department o f Medicine, University of Illinois College of Medicine, Chicago, 111. 60612 Anal. Chem. 40, 2 190 (1968)
Separation of Paraffinic Classes in Petroleum Distillqtes on a Cross-Linked Dextran The Sephadex LEI-20 separation of branched paraffins from cycloparaffins is extended to wide-range petroleum fractions. Three other separations were also found to occur: condensed from noncondensed cycloparaffins, condensed cycloparaffins according to the number of rings, and separation of branched paraffins according to carbon number. P. C. TALARICO, E. W. A L B A U G H , and R. E. SNYDER, Gulf Research & Development Co., Pittsburgh, Pa. Anal. Chem. 40, 2 192 (1968)
quantitative Determination of Organic Halides in Dimethylsulfoxide Organic halides are determined quantitatively by making use of their rapid reaction with base in DhISO. The excess base is determined by the Volhard method or by titration with standard acid. J O E A. V I N S O N and JAMES S. FRITZ, Institute for Atomic Research and Department of Chemistry, Iowa State University, Ames,
Chemical Microscopy of 10-Methylacridiniumchloride. Reactions with Platinum Metals and Gold The addition of a 0.2.21 solution of 10-methylacridiniumchloride in 1M . HCl to acid solutions of the chlorides of several precious metals at low concentrations causes the separation of micro crystals of characteristic shapes and optical properties. H A R O L D F. SCHAEFFER, Department of Chemistry, Westminster College, Fulton, Mo. 65251 Anal. Chem. 40, 2202 [ 1968)
Submicro Sampling and Solvent Extraction System for Rapid Gas Chromatographic Determination of Blood Alcohol The sampling procedure used in this study is based upon the Cnopette sampling system. Many of the cumbersome manipulative steps associated with sample preparation for gas chromatographic analysis are eliminated by using this procedure. R O N A L D H. LAESSIG, Department of Preventive Medicine, State Laboratory of Hygiene, University of Wisconsin, Madison, Wis. Anal. Chem. 40, 2205 [ 1968)
Determination of Amphetamine by Ultraviolet Spectropholometry Cerium oxidation of amphetamine in aqueous HC1 results in.%hexane soluble product which absorbs ultraviolet radiations. The procedure is epwific for the p-phenylethylamine group. J A C K E. W A L L A C E , JOHN D. BIGGS, and SHELDON L. LADD, Forensic Toxicology Branch, USAF Epidemiological Laboratory, Lackland Air Force Base, Tex. 78236 Anal. Chem. 40, 2207 [ 1968)
Iowa 50010
Anal. Chem. 40, 2 194 [ 1968)
Determination of Trace Copper in Petroleum Middle Distillates with Cuprizone Copper is determined colorimetrically after complexing and extracting it with biscyclohexanone oxaldihydrazone. Methanol or another polar solvent is used for the extraction. C. E. L A M B D I N and W. V. TAYLOR, Research and Technical Development, Texaco, Inc., P. 0. Box 1608, Port Arthur, Texas 77640 Anal. Chem. 40, 2 I96 ( 1968)
Volumetric Determination of Alcohols in Aqueous Solution with Bromine Chloride Micro amounts of either a primary or secondary alcohol in an aqueous solution can be determined quantitatively by oxidizing the alcohol with bromine chloride and titrating the excess bromine chloride iodometrically. K A Z U O KONISHI, Y O S H l H l R O MORI, H I R O H INOUE, and M A C H I K O NOZOE, Industrial Research Laboratories, Kao Soap Co., Ltd., 1334 Minatoyakushubata, Wakayama-rhi, Japan Anal. Chem. 40, 2198 ( 1968)
Quantitative Analysis of Amines via Amine Boranes The method involves treatment of an amine with an excess, but measured volume, of a standardized solution of diborane in tetrahydrofuran. Excess diborane is decomposed by the addition of water or alcohol, and the liberated hydrogen is measured. ROBERT E. LYLE arid EVERETT W. SOUTHWICK, Department of Chemistry, University of New Hampshire, Durham, N. H. 03824 Anal. Chem. 40, 2201 [ 1968) +Circle
No. 67
Spectrophotometric Determination of Microgram Amounts of Tantalum with Victoria Blue B Tantalum forms a ternary ion-associated complex with Victoria Blue B and fluoride in hydrofluoric acid-sulfuric acid medium. The complex is extracted into benzene and the tantalum determined spectrophotometrically. G. F. KIRKBRIGHT, M. D. M A Y H E W , and T. S. WEST, Chemistry Department, Imperial College, London, S.W. 7, England Anal. Chem. 40, 22 I O (1968)
Determination of Bisphenol A and Impurities by Gas Chromatography of Their Trimethylsilyl Ether Derivatives Bisphenol A and the major, high-boiling impurities in bisphenol A are reacted with bis(triniethy1silyl)acetamide to form the corresponding trimethyldyl ether derivatives which are analyzed gas chromatographically by using a flame ionization detector. L. E. BRYDIA, Chemicals and Plastics, Union Carbide Corp., Bound Brook, N. J. 08805 Anal. Chem. 40, 2212 (1968)
Indirect Spectrophotometric and Atomic Absorption Spectrometric Methods for Determination of Thiocyanate These methods, for the determination of 0.1 to 15 ppm of thiocyanate. are based on the formation of the dithiocyanatodipyridine copper(I1) complex which is extractable with chloroform. R I C H A R D S. D A N C H I K and D. F. BOLTZ, Department of Chemistry, Wayne State Universily, Detroit, Mich. 48202 Anal. Chem. 40, 22 I 5 [ 1968)
on Readers' Service Card VOL. 40, NO. 14, DECEMBER 1968
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Electroanalytical Determination of Molecular Fluorine in the Atmosphere An instrument is described for measuring the concentration of atmospheric fluorine. The measurement is accomplished coulometically when air is bubbled into a lithium chloride solution containing a silver anode and platinum cathode. SAMUEL KAYE and M I C H A E L GRIGGS, General Dynamics Convair, San Diego, Calif. Anal. Chem. 40, 2217 (1968)
Correspondence An Alternative Combustion Technique for Tritium Scintillation Counting T. H. VICKERS, Krebsforschungsinstitut der Univerrit'dt, 1090 Wien, Austria Anal. Chem. 40, 22 19 (1968)
Automafed Structure Elucidation of Several Kinds of Aliphatic and Alicyclic Compounds SHIN-ICHI SASAKI, M i y a g i University of Education, Aoba, Sendai, Japan, HIDETSUGU ABE, Department of Chemistry, Tohoku University, Katahira, Senadi, Japan, TATSUMI OUKI, M A S A Y O S H I S A K A M O T O , and S H U K l C H l O C H I A I , Japan Electron Optics Laboratory, Akishima, Tokyo, Japan Anal. Chem. 40, 2220 (1968)
Aids for Analytical Chemists Simple Tuning Device for Microwave Tapered Matching Cavity C A R L A. BACHE and D O N A L D J. LISK, Pesticide Residue Laboratory, Cornell University, Ithaca, N. Y. 14850 Anal. Chem. 40, 2224 (1968)
Simplified Method of Preparing Column Materials for Gas-liquid Chromatographic Separation of Some Pesficides C. E. M E N D O Z A , K. A. McCULLY, and P. J. WALES, Research Laboratories, Food and Drug Directorate, Department of National Health and Welfare, Ottawa 3, Ontario, Canada Anal. Chem. 40, 2225 (1968)
Calibration of the Methanol and Glycol Nuclear Magnetic Resonance Thermometers with a Static Thermistor Probe A N T H O N Y L. V A N GEET, Department of Chemistry, State University o f New York, Buffalo, N. Y. 14214 Anal. Chem. 40, 2227 (1968)
Dr. G. Sch'ifer, Ass't Professor at the Hannover Medical School, Institute for Clinical Biochemistry and Physiological Chemistry, Hannover, Germany, performing an enzyme kinetic study.
Because only the Phoenix Dual Wavelength Scanning Spectrophotometer brings you a new method of spectrophotometric analysis using First Derivative Spectra Techniques, I t can measure absorption changes of less than 3 x i o + O.D, units in turbid media. It is also a single instrument capable of operation both as a single beam instrument in a dual wavelength mode and as a high sensitivity scanning double beam spectrophotometer, Conventional spectrophotometers are not completely satisfactory so w e have provided the scientist with an unconventional instrument. Although it was primarily intended for studies in enzyme kinetics, oxidative phosphorylation and photosynthesis, it has also found applications in other areas where small O.D. differences have to b e measured i n optically dense media. This is why more a n d m o r e scientists are specifying Phoenix Scanning Dual Wavelength Spectrophotometers. For complete technical details write for Bulletin PMD-1010
Use of a Primary Beam Filter in X-Ray Fluorescence Spectrometric Determination of Trace Arsenic JOHN T. GILMORE, Chevron Research Company, Richmond, Calif. Anal. Chem. 40, 2230 (1968)
Determination of Trace Contaminants in Air by Concentrating on Porous Polymer Beads FREDERICK W. WILLIAMS and MERLE E. UMSTEAD, Fuels Branch, Chemistry Division, Naval Research Laboratory, Washington, D. C. 20390 Anal. Chem. 40, 2232 (1968) +Circle
No. 69 on Readers' Service Card
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VOL. 40, NO. 14, DECEMBER 1968
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