AC BRIEFS Determination of Radiostrontium by Solvent Extraction A procedure for the separation of radiostrontium from a mixed fission product matrix containing Ce-Pr 144 , Cs137, Ru-Rli 1 "", ZrKb o:l , Pm" T , and Y"> can be performed in 45 minutes. Recoverv is 98.2% with a standard deviation of WALTER C. J O H N S O N , JR., Purex Analytical Control, Chemical Processing Division, Hanford Atomic Products Operation, Rich land, Wash. Anal. Chem. 38, 954 (1966)
Acidity of Aromatic Sulfonic Acids and Their Use as Titrants in Nonaqueous Solvents Twelve aromatic sulfonic acids were titrated potentiometrically with basic titrants in nonaqueous media and com pared with several inorganic acids. 2,4-Dinitrobenzenesulfonic acid was evaluated as a titrant for bases. DONALD J . PIETRZYK and J O N BELISLE, Department of Chem istry, University of Iowa, Iowa City, Iowa Anal. Chem. 38, 969 (1966)
Analytical Study of an Iodide-Sensitive Membrane Electrode
lsotopic Determination of Calcium-48 by Proton Activation The relative standard error over the concentration range from 0.18 (natural) to 4 atom % Ca 18 is 2.7%. T h e method involves activation with 4.75 m.e.v. protons of calcium samples containing enriched calcium-48 as tracer which leads to the formation of 44-hour scandium-48 and 4-hour scandium-43 and -44. M A X PEISACH and RENE PRETORIUS, Southern Nuclear Institute, Faure, C.P., South Africa
HIGHLIGHTS OF T H E SCIENTIFIC A N D T E C H N I C A L A R T I C L E S IN THIS ISSUE
Universities
T h e characteristics and analytical usefulness of the A g l impregnated silicone rubber membrane electrode were evaluated. Some areas of application to chemical meas urements in solution are suggested. G . A . RECHNITZ, M. Ft. KRESZ, and S. B. Z A M O C H N I C K , De partment of Chemistry and Analytical Chemistry Center, Uni versity of Pennsylvania, Philadelphia, Pa. 19104 Anal. Chem. 38, 973 (1966)
Anal. Chem. 38, 956 (1966)
Fluorometric Determination of Indoxole [2,3-Bis(p-Methoxypheny1)-Indole] in Biological Specimens Radiochemical Separations by lsotopic Ion Exchange Ion exchange and isotopic exchange operate simultane ously to effect rapid multitrace element separation from large amounts of a radioactive matrix element. T h e tech nique was applied to barium and sodium matrices. FOUAD TERA and G. H. MORRISON, Department of Chemistry, Cornell University, Ithaca, Ν Υ.
The method, based on an ethyl acetate extraction of the alkaline specimen and subsequent fluorometric analysis of an ethanolic solution of the extract residue, is sensitive to 0.07 itg./ml., 0.21 ,ug./ml., and 4.20 jug./gram of indoxole in serum, urine, and feces, respectively. DAVID G. KAISER, BARBARA J . B O W M A N , and ARLINGTON A . FORIST, Biochemical Research Division, The Upjohn Co., Kalamazoo, Mich. Anal. Chem. 38, 977 (1966)
Anal. Chem. 38, 959 (1966)
Fast Separation of Niobium-95 from Zirconium-95 in Commercial Radioisotope Solutions
Effects of Temperature upon the Barbital Buffers Used in Electrophoresis
A method based on the extraction of niobium-95 tracer with diisobutylcarbinol from aqueous solutions of dilute sulfuric acid-hydrofluoric acid results in radiochemical purities of 99.9% for niobium-95 and 99.8% for zirconium95.
D a t a are given for the effects of temperature on the solu bility and dissociation constant of 5,5-diethylbarbituric acid and on the p H and conductivity of barbitual buffers of various ionic strengths. These data permit the pre diction of the characteristics of the buffer at any temper ature in the useful range and the planning of buffer com position to meet the requirements of different electrophoretic conditions.
AART JURRIAANSE and FLETCHER L MOORE, Analytical Chemistry Division, Oak Ridge National Laboratory, Oak Ridge, Tenn. Anal. Chem. 38, 964 (1966)
R. D. STRICKLAND and M. M. ANDERSON, Chemistry Depart ment, Research Division, Veterans Administration Hospital, A l buquerque, Ν. Μ. Anal. Chem. 38, 980 (1966)
Voltammetric Applications of Rotating and Stationary Carbon-Epoxy Electrodes The carbon-epoxy material was fabricated into both a rotating carbon disk electrode for current-voltage investi gations and a linear diffusion cell for chronopotentiometrie work. These electrodes were tested on the Fe(CN)e" 4 Fe(CN)e-* couple. HAROLD S. SWOFFORD, JR., and ROY L. C A R M A N I I I , De partment of Chemistry, University of Minnesota, Minneapolis, Minn. 55455 Anal. Chem. 38, 966 (1966)
Comparison of Four Methods of Determining Urinary Pregnanediol Enzymatic hydrolysis of pregnanediol glucosiduronate, preliminary purification using silica gel column chroma tography, and quantitation by means of gas chromatog raphy was selected as the preferred method. R. D. BARRY, MICHAEL GUARNIERI, P. K. BESCH, W I L L I A M RING, and N. F. BESCH, Department of Obstetrics and Gyne cology, The Ohio State University College of Medicine, Colum bus, Ohio 43210 and Medical Research Consultants, Inc., Colum bus, Ohio Anal. Chem. 38, 983 (1966) VOL. 38, NO. 8, JULY 1966
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AC BRIEFS Micro and Trace Analysis by a Combination of Ion Exchange Resin-Loaded Papers and X-Ray Spectrography An evaluation of the chemical and x-ray spectrographs characteristics of ion exchange resin-loaded disks is reported. T h e results show that the combination of ion exchange and x-ray spectrography provides a general method for micro and trace analysis. W I L L I A M J . CAMPBELL, ERNEST F. SPANO, and THOMAS E. GREEN, U. S. Department of the Interior, Bureau of Mines, College Park Metallurgy Research Center, College Park, M d . Anal. Chem. 38, 987 (1966)
Theory of Gel Filtration (Permeation) Chromatography Starting with a general plate height equation, a theory of zone broadening is formulated. J . CALVIN GIDDINGS and KANAI L. MALLIK, Department of Chemistry, University of Utah, Salt Lake City, Utah Anal. Chem. 38, 997 (1966)
Rapid Analysis of Binary Amine Mixtures by Differential Reaction Rates. Detailed Study of Synergistic Effects and Other Sources of Error
Accuracy of Three Methods for Determination of Oxygen in Potassium a t Concentrations Less Than 20 p.p.m. Comparative determinations were made with the vacuum amalgamation, vacuum distillation, and neutron activa tion methods using a replicate sampling technique. T h e oxygen values obtained show good agreement when ad justed for systematic errors and the presence of alkaline impurities other than K»0. RANDALL F. G A H N and LOUIS ROSENBLUM, Lewis Research Center, National Aeronautics and Space Administration, Cleve land, Ohio Anal. Chem. 38, 1014 (1966)
2-Chloro-5-Cyano-3,6-Dihydroxybenzoquinone, a New Analytical Reagent for the Spectrophotometric Determination of Calcium ( I I ) The synthesis of 2-chloro-5-cyano-3,6-dihydroxybenzoquinone, which has a structure similar to that of the ehloranilic acid, is described. Micro amounts of Ca +2 were de termined spectrophotometrically by complexing with this reagent. The method m a y be used in the presence of Ba +2 . R. E. REHWOLDT, B. L. CHASEN, and J . B. LI, Vassar College, Poughlceepsie, Ν. Υ. Anal. Chem. 38, 1018 (1966)
Optimum Resolution and Minimum Time Operation in Gas Chromatography: Effect of Various Parameters on Resolution Under Normalized Time Conditions
The single point modification of the differential kinetic method of Roberts and Regan permits the analysis of mixtures containing almost any combination of aliphatic or aromatic primary, secondary, and tertiary amines. Solution conductance is recorded as a function of time.
Normalized time conditions arc used to calculate optimum column length, column temperature and capacity factor, carrier gas velocity, and particle or column diameter for maximum resolution by means of the general, well known equations for elution time, resolution, and flow rate through porous materials or open tubes.
RONALD A . GREINKE and HARRY B. MARK, JR., Department of Chemistry, University of Michigan, Ann Arlaor, Mich. 48104
GEORGES G U I O C H O N , Ecole Polytechnique Laboratoire du Professeur L. Jacqué, 17 rue Descartes, Paris (5eme), France
Anal. Chem. 38, 1001 (1966)
Anal. Chem. 38, 1020 (1966)
A Study of the Feasibility of the Iron Hollow Cathode as a Multi-Element Atomic Absorption Unit Magnesium, manganese, nickel, and copper produced sufficient absorption to have analytical value. T h e sensitivities determined for these elements were 10.0, 0.04, 0.10, and 0.80 p.p.m., respectively. C. W . FRANK, W . G . SCHRENK, and C. E. MELOAN, Kansas Agricultural Experiment Station, Department of Chemistry, Kansas State University, Manhattan, Kan. Anal. Chem. 38, 1005 (1966)
Separation and Infrared Analysis of Products from the Nitration of a/pha-Olefins Infrared techniques using base-point and inverted matrix methods were devised for the direct analysis of complex mixtures of nitro alcohol, nitro olefin, dinitro paraffin, and nitro nitrates. An additional near infrared technique was devised for the determination of nitro alcohol and nitro olefin in complex mixtures. HARRY M O R G A N , R. M. SHERWOOD, and T. A . WASHALL, Research Center, The Atlantic Refining Co., Glenolden, Pa. Anal. Chem. 38, 1009 (1966) "See Laboratory Guide for all Products/Sales Offices" Circle No. 59 on Readers' Service Card
Experimental and Theoretical Study of Specific Retention Volumes in Mixtures of Polar and Nonpolar Stationary Liquids Specific retention volumes of monofunctional organic solutes were measured in 1-dodecanol, lauronitrile, ranges of mixtures of each of these with squalane, and squalane. The results are correlated with a theory in which it is assumed that solutes and solvents interact in solution to form complexes in a manner obeying the Law of Mass Action. A N T H O N Y B. LITTLEWOOD and FREDERICK W . WILLMOTT, School of Chemistry, The University, Newcastle upon Tyne I, England Anal. Chem. 38, 1031 (1966)
Apparatus for Reaction Gas Chromatography. Instantaneous Hydrogénation of Unsaturated Esters, Alcohols, Ethers, Ketones, and Other Compound Types, and Determination of Their Separation Factors The apparatus and procedure eliminate the need for a separate hydrogénation step. Two apparatus and hydrogénation procedures for fatty acid esters and also alcohols, ethers, ketones, aldehydes, amines, epoxides, nitriles, halides, and sulfides are presented. MORTON BEROZA and RAFAEL SARMIENTO, Entomology Research Division, Agricultural Research Service, U. S. Department of Agriculture, Beltsville, M d . Anal. Chem. 38, 1042 (1966) VOL. 38, NO. 8, JULY 1966
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AC BRIEFS Automobile Exhaust Hydrocarbon Analysis by Gas Chromatography A modified commercial gas chromatograph was used for the analysis of the complete range of hydrocarbons in raw and highly diluted exhaust gas. Sampling of exhaust gas and hydrocarbon calibration mixtures was investigated.
A Trifluoroaeetylation-Fluorine-19 Nuclear Magnetic Resonance Technique f o r Characterization of Hydroxyl Groups in Poly (Propylene Oxides)
DAVID J. McEWEN, Fuels and Lubricants Department, Research Laboratories, General Motors Corp., Warren, Mich.
STANLEY L MANATT, D. DAVID LAWSON, J O H N D. ING H A M , NEVILLE S. RAPP, and J I M P. HARDY, Space Sciences and Propulsion Division, Jet Propulsion Laboratory, California Institute of Technology, Pasadena, Calif. 91103
Anal. Chem. 38, 1047 (1966)
Anal. Chem. 38, 1063 (1966)
Determination of Micro Quantities of the Cj—C4 Primary and Secondary Amines by Electron Affinity Detection T h i n layer and gas chromatography were used for t h e separation, identification, a n d determination of the 11 G - C i primary and secondary amines. Complete separa tion of all the amines was obtained. Most of them could be determined at a concentration of 1.0 /ug./ml. or less in aqueous solutions. EDGAR W . DAY, JR., TOMASZ GOLAB, and J O H N R. KOONS, Eli Lilly and Co., Greenfield Laboratories, Greenfield, Ind.
Voltammetric Determination of Aluminum by Oxidation of Its Solochrome Violet RS Complex a t the Rotated Pyrolytic Graphite Electrode T. M. FLORENCE, F. J . MILLER, and H. E. ZITTEL, Analytical Chemistry Division, Oak Ridge National Laboratory, Oak Ridge, Tenn. Anal. Chem. 38, 1065 (1966)
Anal. Chem. 38, 1053 (1966)
Salt Effects on the Titration of Neutral Bases
Scientific Communications The Mass Spectrum of a Compound of Formula C72H240gF128N4P4 and Molecular W e i g h t 3628
MARIO OJEDA, RENATO PE'REZ, and P. A . H. WYATT, Facultad de Quimica y Farmacia, Universidad de Chile, Santiago, Chile Anal. Chem. 38, 1068 (1966)
HENRY M. FALES, Section on Chemistry, Laboratory of Metabo lism, National Heart Institute, Bethesda, M d . 20014 Anal. Chem. 38, 1058 (1966)
N e a r Ultraviolet-Visible Atomic Absorption Spectra of the Noble Gases J. A . GOLEB, Chemistry Division, Argonne National Laboratory, Argonne, I I I . Anal. Chem. 38, 1059 (1966)
Correspondence Factors Affecting Line Intensities in the Flame Spectrometry of Metals in Organic Solvents JACOB ELHANAN and W . D. COOKE, Department of Chemistry, Cornell University, Ithaca, Ν. Υ. Anal. Chem. 38, 1062 (1966)
Study on α Detector f o r Gaseous Components Using Semiconductive Thin Films TETSURO SEIYAMA and SHUICHI K A G A W A , Department of Applied Chemistry, Faculty of Engineering, Kyushu University, Hakozaki-machi, Fukuoka-shi, Japan Anal. Chem. 38, 1069 (1966)
Some Precautions Required in the Calibration of Fluorescence Spectrometers in the Ultraviolet Region H. C. BORRESEN and C. A . PARKER, Institute of Clinical Bio chemistry, Rikshospitalet, University of Oslo, Oslo I, Norway Anal. Chem. 38, 1073 (1966) VOL. 38, NO. 8, JULY 1966 ·
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AC Polarographie Reduction of the Pyridinium Ion in Pyridine-Water Mixtures LAYA FLOCH, MICHAEL S. SPRITZER, and PHILIP J. ELVING, Department of Chemistry, The University of Michigan, Ann Arbor, Mich. Anal. Chem. 38, 1074 (1966)
A Secondary Alkanol Stationary Liquid for Selective Separation of Alkanols by Gas Chromatography
BRIEFS
Alkali Titration of Germanium J A M E S F. REED, Pennsylvania State University, McKeesport, Pa. 15132 A n a l . C h e m . 3 8 , 1085 ( 1 9 6 6 )
Light Scattering by Particles in Atomic Absorption Spectrometry S. R. K O I R T Y O H A N N and Ε. Ε. PICKETT, Department of A g r i cultural Chemistry, University of Missouri, C o l u m b i a , M o . A n a l . C h e m . 3 8 , 1087
A . B. LITTLEWOOD and F. W . WILLMOTT, University of New castle upon Tyne, School of Chemistry, The University, Newcastle upon Tyne, I, England Anal. Chem. 38, 1076 (1966)
(1966)
1,2-Dichloroethane as a Solvent for Perchloric Acid-Catalyzed Acetylation Emission Spectrographs Determination of Plutonium, Thorium, and Rare Earths in Americium Following Anion Exchange Separation
J . A . M A G N U S O N and R. J . C E R R I , Silicone Products Depart ment, G e n e r a l Electric Co., W a t e r f o r d , Ν . Υ . A n a l . C h e m . 38, 1088 ( 1 9 6 6 )
H. N. BARTON, The Dow Chemical Co., Rocky Flats Division, Golden, Colo. Anal. Chem. 38, 1077 (1966)
Ion Exchange Behavior of Some Substituted Ammonium Ions on Zirconium Phosphate Separation and Determination of Lead, Cadmium, and Tin by Controlled Potential Coulometry
R. L REBERTUS, C e n t r a l Research Laboratories, Minnesota ing and Manufacturing C o . , St. Paul, M i n n . 551 19 A n a l . C h e m . 3 8 , 1089
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(1966)
W . M. WISE and D. E. CAMPBELL, Research and Development Laboratories, Corning Glass Works, Corning, Ν. Υ. Anal. Chem. 38, 1079 (1966)
Analysis of Gases for Nitric Oxide, Nitrogen Dioxide, and Oxygen in a Pressure Nitric Acid Plant Nondestructive Activation Analysis of Crude Oils for Arsenic to One Part per Billion, and Simultaneous Determination of Five Other Trace Elements
H . L. F A U C E T T , T. C . M c R I G H T , and H . G . G R A H A M , JR., Ten nessee V a l l e y Authority, Muscle Shoals, A l a . A n a l . C h e m . 38, 1090 ( 1 9 6 6 )
DEAN J. VEAL, Research and Development Department, Phillips Petroleum Co., Bartlesville, Okla. Anal. Chem. 38, 1080 (1966)
Determination of Chromium in Low Alloy Steels by Atomic Absorption Spectrometry LUCIEN BARNES, JR., Air Reduction Co., Inc., Central Research Laboratories, Murray H i l l , N. J . 07971 Anal. Chem. 38, 1083 (1966)
Aids for Analytical Chemists Extraction in a Beaker EVAN MORGAN, Richmond, V a .
Metallurgical
Laboratories,
Reynolds
A n a l . C h e m . 3 8 , 1093
VOL 38, NO. 8, JULY 1966
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AC BRIEFS Improved Sulfur-Reacting Microcoulometric Cell for Gas Chromatography D O N A L D F. A D A M S , G E O R G E A . J E N S E N , J . P A U L STEADM A N , ROBERT K. KOPPE, and T H O M A S J . R O B E R T S O N , C o l lege of Engineering Research Division, Washington State University, Pullman, W a s h . A n a l . C h e m . 38, 1094 ( 1 9 6 6 )
Evaporation Manifold for Septum-Sealed Vials G E R A L D J . LITT and N O R M A N A D L E R , Merck Chemical M a n u facturing Division, Merck & C o . , Inc., Rahway, N . J . A n a l . C h e m . 3 8 , 1096 ( 1 9 6 6 )
Automatic Vapor Sampling for Gas Chromatographic Analysis G . SZÉKELY, G . R Â C Z , and G . TRAPLY, Department of Physical Chemistry, Technical University of Budapest, Budapest, Hungary A n a l . C h e m . 38, 1097 ( 1 9 6 6 )
In-Place Fabrication of Fritted Glass Discs D E R W O O D B. BIRD, Biochemical Research Program, Administration Hospital, San Francisco, C a l i f .
Veterans
A n a l . C h e m . 38, 1098 ( 1 9 6 6 )
Uranium Isotope Analysis by Optical Emission Spectrometry J . A . LEYS and R. E. PERKINS, 3 M C o . — C e n t r a l Research, 2301 Hudson Road, St. Paul, M i n n .
Precision and ultra precision
A n a l . C h e m . 3 8 , 1099 ( 1 9 6 6 )
All RGI micrometric burets and syringes offer unmatched accuracy and operating convenience.
Simplified All-Transistor Chronopotentiostat T H O M A S F. M A R T I N and J . W I L L I A M V O G T , T R W Inc., 23555 Euclid A v e . , C l e v e l a n d , O h i o A n a l . C h e m . 38, I 102 ( 1 9 6 6 )
The ultimate is the new RGI Ultra-Precision Micrometer Buret and Syringe with digital readout and parallax-free vernier. Built around a Swiss made micrometer precise to one part in 25,000, this instrument is available in two sizes: 0.25 ml. in .00001 ml. divisions, and 2.5 ml. in .0001 ml. divisions. In manufacture, the micrometer lead screw is machined to 40 millionths of an inch and the plunger is ground to 50 millionths. This assures a reproducible accuracy of .02 to .04%. Cost is surprisingly low. Complete information is available in catalog form. Write for your free copy today.
High-Temperature Valve for Corrosive Gases A U G U S T U S R. G L A S G O W , JR., N a t i o n a l Bureau of Standards, W a s h i n g t o n , D. C . A n a l . C h e m . 38, I 104 ( 1 9 6 6 )
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