A C BRIEFS Highlights of Articles in This Issue
Anion-Exchange Chromatography of Some Aromatic Organic Acids in Ferric Chloride—Organic Solvent Medium
Homogeneous Chemiluminescent Measurement of Nitric Oxide with Ozone. Implications for Continuous Selective Monitoring of Gaseous Air Pollutants
Volume distribution coefficients of some organic acids at various compositions of ferric chloride-organic solvent eluants using the anion exchange resin are presented.
Homogeneous chemiluminescent gas reactions can be used for air pollutant monitors which will give continuous records and are both specific and multifunctional. This is demonstrated by measurements of NO using the N O + Os —» N 0 2 + 0 2 + hv reaction and calculations based on prior studies of the ( N O + NO2/O) and C O / O reaction systems.
K/L SANG LEE, DAI WOON LEE, and EUY KYUNG YU LEE, Department of Chemistry, Yonsei University, Seoul, Korea Anal. Chem., 42, 554 (1970)
Determination of Phosphides and White Phosphorus in Biological Materials by Neutron Activation Analysis A method has been developed using the Neutron Activation Analysis technique, to determine toxic phosphorus in biological materials in nanogram levels. S. S. KRISHNAN and R. C. GUPTA, The Center of Forensic Sciences, Province of Ontario, 8 Jarvis Street, Toronto 2, Ontario, Canada Anal. Chem., 42, 557 (1970)
Diethyl Oxalate as New Reagent for Spectrophotometric Determination of Ketosteroids
ARTHUR FONTUN, ALBERTO J. SABADELL, and RICHARD J. RONCO, AreoChem Research Laboratories, Inc., P.O. Box 12, Princeton, N. J. 08540 Anal. Chem., 42, 575
(1970)
Sensitive, Wide-Range, Temperature-Controlled Cell A cell was developed in which temperature can be changed rapidly over a wide range (—190 °C to 300 °C) b y a control system operating in a maximum-rate mode and maintained at a set rate by the system operating in a proportional mode. E. W. OWEN, Lawrence Radiation Laboratory, University of California, Livermore, Calif. 94550 Anal. Chem., 42, 579 (1970) Exponentially Loaded Column Gas Chromatography
A spectrophotometric method has been developed which is suitable for the characterization and quantitative determination of ketosteroids, particularly in t h e assay of mixtures and pharmaceutical formulations.
Columns possessing an exponential gradient in k have been treated theoretically from the viewpoints of solute retention, column efficiency, and resolution.
SANDOR GOROG, Chemical Works G. Richter, Budapest X., Hungary Anal. Chem., 42, 560 (1970)
THOMAS BUNTING and CLIFTON E. MELOAN, Department of Chemistry, Kansas State University, Manhattan, Kan. 66502 Anal. Chem., 42, 586 (1970) Ultraviolet and Visible Refractive Indices of Spectro-Quality Solvents
Thin-Layer Chromatography of Amine Oxidation Products A comparative study was made of spray reagents for amines and their iV-oxides, carbazoles, benzidines, and nitrobenzene reduction products. Oxidation—reduction indicators, complex ion reagents, complexing agents, and several other types of visualizing agents were employed. JOSEPH H. ROSS, Department of Chemistry, Indiana University at South Bend, South Bend, Ind. 46615 Anal. Chem., 42, 564
(1970)
Nuclear Magnetic Resonance Study of Ion-Exchange Resins
Refractive index data down to 1900 Â are reported for seven spectro-quality solvents in terms of constants for the dispersion equation. On the basis of water and sodium D line data, an accuracy of ±0.002 is expected. J. R. KRIVACIC and D. W. URRY, Institute for Biomedical Research, Education and Research Foundation, American Medical Association, Chicago, III. 60610 Anal. Chem., 42, 596
(1970)
Conformational Studies of Chelated Ethylenediamines by Nuclear Magnetic Resonance. Tris-(ethylenediamine)Nickel(ll) Ion in Aqueous Solution
Nuclear magnetic resonance is shown to be useful in studying the ionic nature of exchange resins. Hydration numbers of several counterions were obtained and discussed.
From the temperature dependence of the contact shifts, thermodynamic parameters (ΔΗ = 0.36 ± 0.03 kcal/mole, AS = 0.20 rh 0.02 e.u.) involved in the D-kkk (more stable) to D-k'k'k' (less stable) form, racemization rate (5.5 X 10s sec 1 ) and degree of ring puckering are evaluated.
R. W. CREEKMORE and C. N. REILLEY, Department of Chemistry, University of North Carolina, Chapel Hill, N. C. 27514 Anal. Chem., 42, 570 (1970)
FLOYD F.-L. HO and CHARLES N. REILLEY, Department of Chemistry, University of North Carolina, Chapel Hill, N. C. 27514 Anal. Chem., 42, 600 (1970) ANALYTICAL CHEMISTRY, VOL. 42, NO. 6, MAY 1970
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AC BRIEFS General Purpose System for Computer Data Acquisition and Control
Calorimetric Determination of Equilibrium Constants for Very Stable Metal-Ligand Complexes
An electronic system using D T L logic and commercial com ponents is described which can input data at 10 kHz with 12-bit accuracy either as X - Y pairs or in a random fashion from eight separate inputs.
Log Κ, Δ Η ° , and AS" values have been calorimetrically de termined for the interaction of Hg 2+ ion with 2-aminoethanol and of Cu 2+ and Zn 2t ions with 1,10-phenanthroline in aque ous solution at 25 °C.
LOUIS RAMALEY and GEORGE S. WILSON, Department Chemistry, University of Arizona, Tucson, Ariz. 85721
DELBERT J. EATOUGH, Shell Development Company, Emeryville, Calif. Anal. Chem., 42, 635 (1970)
Anal. Chem., 42, 606
of
(1970)
Improved Instrumentation for Phosphorimetry of Organic Molecules in Rigid Media
High-Speed Autoranging Amplifier for Digital Data Acquisition An eight-range, high-speed autoranging amplifier for digital data acquisition is described. With an accuracy of 0.5% and linearity better than 0.2%, the amplifier can reliably track a signal varying at 104 volts/sec while storing a coded gain range for computer processing. GEORGE S. WILSON and LOUIS RAMALEY, Department of Chemistry, University of Arizona, Tucson, Ariz. 85721 Anal. Chem., 42, 611
By means of a rotating sample cell, a more stable light source, and a better solvent clean-up in phosphorimetry, de tection limits have been lowered, precision and accuracy in creased, and sampling and measurement time reduced as compared to phosphorimetry with standard commercial in strumentation. RUTH ZWEIDINGER and J. D. WINEFORDNER, Department of Chemistry, University of Florida, Gainesville, Fla. 32601 Anal. Chem., 42, 639 (1970)
(1970)
Decomposition of Monoalkyl Dithiocarbamates Differential Potentiometry with Ion-Selective Electrodes. A New Instrumental Approach A differential high input impedance amplifier is described and applications in the measurement of the potentials of cells consisting of two ion-selective electrodes are illustrated. M. J. D. BRAND and G. A. RECHNITZ, Chemistry Depart ment, State University of New York, Buffalo, Ν. Υ. 14214 Anal. Chem., 42, 616
SERGE J. JORIS, KEIJO I. ASPILA, and CHUN/ L. CHAKRABARTI, Department of Chemistry, Carleton University, Ottawa 1, Ontario, Canada Anal. Chem., 42, 647 (1970)
(1970)
Simple Ion Exchange Separation of Magnesium from Calcium and Other Metal Ions Using EthyleneglycolBis(2-Aminoethylether) Tetraacetic Acid as a Complexing Agent
Structural Studies of Asphaltics by X-Ray Small Angle Scattering The object of this endeavor was to obtain further informa tion concerning the structure of petroleum asphaltics in order to fully establish the framework of their macrostruc ture. SIDNEY S. POLLACK, Mellon Institute, Carnegie-Mellon University, Pittsburgh, Pa. 15213 and TEH FU YEN, De partment of Chemistry, California State College at Los Angeles, Los Angeles, Calif. 90032 Anal. Chem., 42, 623
An attempt has been made to rationalize the different mech anisms that have been proposed for the decomposition of the monoalkyl dithiocarbamates in alkaline solution. Pos sible side reactions in the decomposition have been discussed.
Over the p H range 6.5 to 7.0, calcium and other metal ions form with E G T A negatively charged complexes. The free magnesium ion is quantitatively adsorbed by a cation ex changer. MILAN MARHOL and K. L. CHENG, Department of Chem istry, University of Missouri—Kansas City, Kansas City, Missouri 64110 Anal. Chem., 42, 652 (1970)
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Notes Titration of Microgram Amounts of Aminopolycarboxylic Acids with Manganese(ll) and Catalytic End-Point Indication
Fluorescence of Acetylsalicylic Acid in Solution and Its Measurement in Presence of Salicylic Acid
The catalytic end-point indication approach is applied to the microgram determination of some aminopolycarboxylic anions and is compared with a more conventional and in direct method of analysis.
Acetylsalicylic acid (aspirin) has been found to fluoresce at 335 nm with a quantum efficiency of 0.02. Aspirin tablets can be analyzed fiuorometrically for both acetylsalicylic acid and salicylic acid.
HORACIO A. MOTTOLA, Department of Chemistry, homa State University, Stillwater, Okla. 74074
CORBIN I. MILES and GEORGE H. SCHENK, Department of Chemistry, Wayne State University, Detroit, Mich. 48202
Okla
Anal. Chem., 42, 630 (1970)
Anal. Chem., 42, 656 ANALYTICAL CHEMISTRY, VOL. 42, NO. 6, MAY 1970
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BRIEFS
Chromogenic Reaction between p-Dimethylaminobenzaldehyde and Hydrogen Peroxide
New Determination of Stoichiometry of the lodometric Method for Ozone Analysis at pH 7.0
Treatment of p-dimcthylaminobenzaldehyde with H2O2 pro duced visible colors and formic acid. The decarbonylated aldehyde, p-dimethylaminophenol, on further oxidation ap pears to generate a quinone responsible for the color.
A value of 1.53 ± 0.12 for the ratio L " / 0 3 for iodide solution at p H 7.0 has been determined using ozone from electron pulse irradiation of oxygen. The ozone was measured spectrophotometrically. A mechanism is proposed to explain the previously observed p H dependence of the ratio.
BIBHUTI R. DasGUPTA, Biology Department, College, Bryn Mawr, Pa. 19010
Bryn Mawr
Anal. Chem., 42, 659 (1970) Reduction—Gas Chromatographic Determination of Cyclic Monomer and Oligomers in Polyamides The individual contents of the cyclic monomer and oligo mers in polyamides were determined by reducing them to the corresponding cyclic amines followed by gas chroma tography. SADAO MORI and MOTOHISA FURUSAWA, Laboratory of Chemistry, Faculty of Engineering, Yamanashi University, Kofu, Japan and TSUGIO TAKEUCHI, Department of Syn thetic Chemistry, Faculty of Engineering, Nagoya Univer sity, Nagoya, Japan Anal. Chem., 42, 661 (1970) Spectrophotometry Determination of Diphenylamine, 2-Nitrodiphenylamine, and 4-Nitrodiphenylamine by Oxidation with Ferric Iron A method was developed for diphenylamine analysis which is not subject to many of the interferences of present meth ods. The ferric oxidation method described meets the re quirements and is also applicable to 2-nitrodiphenylamine and 4-nitrodiphenyIamine. WILBUR W. DEATLEY, Naval Ordnance Station, Indian Head, Md. 20640 Anal. Chem., 42, 662 (1970) Direct Reading Emission Spectrometric Determination of Trace Elements in Rare Earth Compounds Incorporating a Rotating Electrode. Effects of Alkali Chlorides as Radiation Buffers Alkali chlorides added as radiation buffers enhanced the emission intensity of the spectral line and made possible the determination of microquantities of rare earth elements (as much as 10 ppm in the highly pure oxides). YASUAKI OSUMI, AKIHIKO KATO, and YOSHIZO MIYAKE, Government Industrial Research Institute, Osaka, Midorigaoka, Ikeda-shi, Osaka-fu, Japan Anal. Chem., 42, 664
(1970)
A. WILLIAM BOYD, CLIVE WILLIS, and RONALD CYR, Physical Chemistry Branch, Chalk River Nuclear Labora tories, Atomic Energy of Canada Limited, Chalk River, Ontario, Canada Anal. Chem., 42, 670 (1970) Spark Source Mass Spectrographic Analysis of Ingot Iron for Silver, Copper, Molybdenum, and Nickel by Isotope Dilution and for Cobalt by an Internal Standard Technique A spark source mass spectrographic method was developed for simultaneously determining low concentrations of Co, Ag, Cu, Mo, and Ni in 100-mg ingot iron samples. Concen trations ranged from 0.00050% for Ag to 0.025% for Ni. PAUL J. PAULSEN, ROBERT ALVAREZ, and CHARLES W. MUELLER, Spectrochemical Analysis Section, Analytical Chemistry Division, National Bureau of Standards, Wash ington, D. C. 20234 Anal. Chem., 42, 673 (1970) Guggenheim Exponential Method for Unequal Intervals The standard Guggenheim exponential method for equal intervals of the dependent variable has been modified for use with unequal intervals by series expansion. Analysis of data for binary diffusion in porous glass disks permits esti mates of precision and accuracy of these methods. ROBERT L. CLELAND, Department of Chemistry, mouth College, Hanover, Ν. Η. 03755
Anal. Chem., 42, 675 (1970)
Activity Measurements Using a Potassium-Selective Liquid Ion-Exchange Electrode Aqueous KC1 solutions and K C l - N a C l solutions were studied using a cell without liquid junction. In KC1 solu tions, the potential varied with concentration with a slope 90% of the theoretical Nernst value. JAMES N. BUTLER and RIMA HUSTON, Tyco Inc., Waltham, Mass. 02154
Inverse Gas-Liquid Chromatographic Studies of Asphalt. Variations in Experimental Parameters
Laboratories
Anal. Chem., 42, 676 (1970)
The parameters studied are carrier gas pressure and flow rate, column temperature, size of column packing, test compound sample size, possible column poisoning, and presence of water in the test compounds. F. A. BARBOUR, S. M. DORRENCE, and J. C. PETERSEN, Laramie Petroleum Research Center, Bureau of Mines, U. S. Department of the Interior, Laramie, Wyo. Anal. Chem., 42, 668
Dart
(1970)
Correspondence Calibration of Methanol Nuclear Magnetic Resonance Thermometer at Low Temperature ANTHONY L. VAN GEET, Department of Chemistry, Oak land University, Rochester, Mich. 48063 Anal. Chem., 42, 679 ANALYTICAL CHEMISTRY, VOL. 42, NO. 6, MAY 1970
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L. J. CSANYI, Institute of Inorganic and Analytical Chemistry, Jozsef Attila University, P. O. Box 440, Szeged, Hungary Anal. Chem., 42, 680 (1970)
Simultaneous Spectrophotometric Determination of Hydrogen Peroxide and Peroxyacids of Sulfur M. H. MARIANO, Junta de Energia Nuclear, DireccaoGérai de Combustiveis e Reactores Nucleares Industrials, Av. da Republica 45-5, Lisboa, Portugal Anal. Chem., 42, 682 (1970)
Aids for Analytical Chemists Correct Procedures for the Calibration and Use of Rotameter-Type Gas Flow Measuring Devices
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CLAUDE VEILLON and JOHN Y. PARK, Department of Chemistry, University of Houston, Houston, Texas 77004
Punched cards
Anal. Chem., 42, 684 (1970)
Tapes Discs On-Line Computer Interfacing of a Densitometer Film Reader for Measuring the Size of Radioactive Colloid Particles
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T. R. BARCLAY, A. C. MORRIS, JR., R. L. HAYES, J. E. CARLTON, and A. E. McDOW, JR., Medical Division, Oak Ridge Associated Universities, Inc., Oak Ridge, Tenn. 37830 Anal. Chem., 42, 685 (1970)
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Director Publications American Society for Testing and Materials 1916 Race St., Philadelphia, Pa. 19103
HAROLD R. MURDOCK, JR., Veterans Administration Hospital, Livermore, Calif. Anal. Chem., 42, 687 (1970)
Please send complete FREE brochure on Atomic and Molecular Data Name
Determination of Volatile Materials in Polymers J. N. ROPER, JR., Research Laboratories, Tennessee Eastman Company, Division of Eastman Kodak Company, Kingsport, Tenn. 37662 Anal. Chem., 42, 688 (1970)
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