A C BRIEFS Highlights of Articles in This Issue
Computer Methods in Analytical Mass Spectrometry. Structure Codes in Processing Mass Spectral Data
Effects of Organic Solvents on Tin Absorbance in an Air—Hydrogen Flame
A compact, unambiguous tabulation of organic chemical structures and a method for converting a tabulation into a structural diagram are described for the computer analysis of mass spectra.
The presence of alcohols, ketones, and organic acids, even at low concentrations, is shown to reduce greatly tin atomic absorbance. The effect increases with carbon number and increased chain branching.
L. R. CRAWFORD, Division of Chemical Physics, CS/RO Chemical Research Laboratories, P. O. Box 160, Clayton, Victoria, Australia 3168, J. D. MORRISON, Division of Physical Chemistry, La Trobe University, Bundoora, Vic toria, Australia 3083
W. W. HARRISON and P. 0. JULIANO, Department of Chemistry, University of Virginia, Charlottesville, Va. 22901
Anal. Chem., 41, 994
(1969)
Ultra-Trace Mass Spectrometric Metal Analysis Using Heptafluorodimethyloctanedione Chelates Quantitative results have been obtained on the order of 10"12 gram of the metal and sensitivities as low as 10"14 gram. B. R. KOWALSKI and T. L. ISENHOUR, Department of Chemistry, University of Washington, Seattle, Wash. 98105, R. E. SIEVERS, Aerospace Research Laboratories, ARC, Wright-Patterson Air Force Base, Ohio 45433 Anal. Chem., 41, 998
(1969)
Metal Complexing Properties and Proton Magnetic Resonance Spectra of 5-Halo-8-Quinolinols The electronic effects caused by introducing halogen substituents in the 5-position of the 8-quinolinol ring system have been evaluated. R. G. BEIMER and QUINTUS FERNANDO, Department Chemistry, University of Arizona, Tucson, Ariz. Anal. Chem., 41, 1003
of
(1969)
Solvent Extraction in the Presence of Emulsion-Forming Residues. Application to the Atomic Absorption Determination of Gold in Low Grade Ores Volume change factors are studied, resulting in quantitative data from the small quantity of M I B K which separates from the emulsion. STEPHEN L. LAW and THOMAS E. GREEN, U. S. Depart ment of the Interior, College Park Metallurgy Research Center, College Park, Md. Anal. Chem., 41, 1008
(1969)
Anal. Chem., 41, 1016
(1969)
Emission Spectrometric Detection of the Elements at the Nanogram per Milliliter Level Using Induction-Coupled Plasma Excitation Emission detection limite for all elements investigated (in cluding Ce, Ta, Hf, Th, U, Zn, and Zr) fall in the nanogram to fractional microgram per milliliter range. GEORGE W. DICKINSON and VELMER A. FASSEL, Institute for Atomic Research and Department of Chemistry, Iowa State University, Ames, Iowa 50010 Anal. Chem., 41, 1021
(1969)
Determination of Metallurgical^ Dissolved Nitrogen in Aluminum-Killed, Low Carbon Steel by Hot Extraction with Hydrogen Hot extraction of interstitial nitrogen with hydrogen is un affected by the presence of ultra-fine aluminum nitride. The technique is more accurate than the ester-halogen technique. T. R. DULSKI and R. M. RAYBECK, Jones & Laughlin Steel Corp., Graham Research Lab., 900 Agnew Rd., Pittsburgh, Pa. 15230 Anal. Chem., 41, 1025
(1969)
High Frequency Excitation of Independently Vaporized Samples in Emission Spectrometry Construction of the discharge chamber is described. The sample is evaporated from a graphite disk which is heated by ohmic current. Detection limite ranging from 0.008 to 15 ng are achieved. IMRICH KLEINMANN and VRATISLAV SVOBODA, Institute for Research, Production, and Use of Radioisotopes, Pristavni, 24, Prague, Czechoslovakia Anal. Chem., 41, 1029
(1969)
Quantitative Determination of Gold in Solution by Solvent Extraction and Atomic Absorption Spectrometry
Direct Spectrophotometric Determination of Sulfate in Natural Waters by Formation of the Ferric Sulfate Complex
Tertiary and quaternary amines are used for the quantitative extraction of gold complex ions into diisobutyl ketone. As little as 5χΚ>- 8 Μ (0.01 mg/1) of gold(III) can be deter mined.
With the described method, sulfate can be determined in the range of 10-500 mg/1 using the absorption of the FeSOi + complex a t optimal wavelengths between 325 and 360 nm.
THEO GROENEWALD, Chamber of Mines of South Africa, Research Organisation, Johannesburg, South Africa
REINER GOGUEL, Chemistry New Zealand
Anal. Chem., 41, 1012
(1969)
Division,
D.S.I.R.,
Anal. Chem., 41, 1034 VOL. 4 1 , NO. 8, JULY 1969
Petone, (1969) . 11 A
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BRIEFS
Stable Pattern Formation and Determination of Molecular Size by Pore-Limit Electrophoresis
Fractionation of Low Temperature Coal Tar by Gel Permeation Chromatography
After sufficient time, a protein mixture forms a distinct pattern which remains constant from 18,000 to 26,000 V-hrs. The proteins traverse a distance proportional to their m o lecular weight.
The method permits separation of coal tars, including t h e "pitch" portion ordinarily discarded, into aliphatic, aromatic, and tar acid components.
GRANT G. SLATER, Neurobiochemistry Laboratory, erans Administration Center, Los Angeles, Calif. Anal. Chem., 41, 1039
Vet(1969)
BENJAMIN C. B. HSIEH, R. E. WOOD, L. L. ANDERSON, and G. R. HILL, Department of Mineral Engineering, University of Utah, Salt Lake City, Utah 84112 Anal. Chem., 41, 1066
(1969)
Automatic Sample Loader for Column Chromatography
An Oxyacidic Flux Method for Determination of Carbon in Sodium T h e method employs KaCrzOî flux to eliminate gettering of C 0 2 by NaaO and achieves a low blank. Good precision a t low oarbon levels is obtained.
Up to 12 fluid samples are loaded onto absorbent contained in small tubes. These are in turn introduced automatically into the fluid feed to a separating column. No loss of resolution or reproducibility is introduced.
C. C. MILES, Argonne National Laboratory, Idaho Facilities, P.O. Box 2528, Idaho Falls, Idaho
A. R. THOMSON and J. W. EVELEIGH, Wantage Research Laboratory (A.E.R.E.), Wantage, Berks, England
Anal. Chem., 41, 1041
The Palladium Transmodulator: for the Gas Chromatograph
(1969)
A New Component
With this component, a gain in sensitivity of a t least 40-fold is demonstrated in analyses using thermal conductivity and ionization cross-section detectors. J. E. LOVELOCK, K. W. CHARLTON, and P. G. SIMMONDS, Jet Propulsion Lab., California Institute of Technology, 4800 Oak Grove Dr., Pasadena, Calif. 91103 Anal. Chem., 41, 1048
(1969)
Separation of Zinc(ll), Nickel(ll), and Cobalt(ll) with Dithizone Based on Differences in Rates of Extraction Values for the extraction constant, K*, are reported. Analysis of synthetic samples of the pairs of ions gave acceptable results except in the case of C o - N i . B. E. McCLELLAN and PATSY SABEL, Department of Chemistry, Murray State University, Murray, Ky. 42071 Anal. Chem., 41, 1077 (1969)
(1969)
Determination of Fluoride in Biological Samples by a Nonfusion Distillation and Ion-Selective Membrane Electrode Method
Variables in the Preparation of Modified Silica Adsorbents Capacity is increased by slow gelation, longer aging and drying times, and the use of pure methanol for washing the gel. Selectivity is greatly affected b y the structure of the tailoring agent. R. E. MAJORS and L. B. ROGERS, Chemistry Purdue University, Lafayette, Indiana 47907
Anal. Chem., 41, 1073
Department
Anal. Chem., 41, 1052
(1969)
Samples with as low as 2 ppm fluoride are analyzed with less than a 0.5% relative standard deviation. Results compare favorably with t h e AOAC method. PAUL J. KE, LLOYD W. REGIER, and HENRY E. POWER, Fisheries Research Board of Canada, Halifax Laboratory, Halifax, Nova Scotia Anal. Chem., 41, 1081
(1969)
Effects of Structural Changes of the Pretreating Agent on Adsorption by Modified Silica Adsorbents
Nitrogen and Oxygen Compound Types in Petroleum. Total Analysis of an 8 5 0 - 1 0 0 0 °F Distillate from a California Crude Oil
Use of substituted p-aminoazobenzenes as pretreating agents in silica hydrogels results in xerogels which are quite selective for structurally-related azo dyes.
All compound types present in more t h a n trace amounts are accounted for, their molecular structures determined, and their concentrations measured.
R. E. MAJORS and L. B. ROGERS, Department istry, Purdue University, Lafayette, Ind. 47907
L. R. SNYDER, Union Oil Co. of California, Union Research Center, Brea, Calif.
of Chem-
Anal. Chem., 41, 1058
(1969)
Anal. Chem., 41, 1084 VOL. 4 1 , NO. 8, JULY 1969
(1969) ·
13 A
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BRIEFS
Notes
Separation of Gold from Solutions of Base Metals by Cation Exchange
Determination of Major Constituents by Atomic Absorption Spectrometry
Microgram and milligram amounts of gold may be recovered quantitatively from a large excess of iron, copper, and nickel as chlorides. Several gold ores have been analyzed.
Methods for determining major constituents of cement, stainless steel, bronze, aluminum alloys, and feeds are pre sented. Internal standardization improved precision two fold.
ANTONY E. PITTS and FRED E. BEAMISH, Department of Chemistry, University of Toronto, Toronto 5, Canada Anal. Chem., 41, 1107
(1969)
FREDRIC J. FELDMAN, JANE A. BLASI, and STANLEY B. SMITH, Jr., Instrumentation Laboratory, Inc., 113 Hartwell Ave., Lexington, Mass. 02173 Anal. Chem., 41, 1095
(1969)
Solvation of Aluminum(lll) ion in DimethylsulfoxideWater Solution by Proton Magnetic Resonance Spectrometry P M R spectrometry is used to evaluate equilibrium constante for the displacement of DMSO molecules in the first solva tion sphere of Al(III) by water. D. P. OLANDER, R. S. MARIANELLI, and R. C. LARSON, Department of Chemistry, University of Nebraska, Lin coln, Neb. 68508
Quantitative Analysis for Trace Chromium in Ferrous Alloys by Electron Capture Gas Chromatography The technique involves reacting samples directly with trifluoroacetylacetone in the presence of catalytic amounts of an inorganic acid. Amounts of Or determined are between 10 11 ΙΟ" and 10" gram. W. D. ROSS, Monsanto Research Corporation, Dayton, Ohio 45407, and R. E. SIEVERS, Aerospace Research Lab oratories, Wright-Patterson Air Force Base, Ohio 45433 Anal. Chem., 41, 1109
(1969)
Anal. Chem., 41, 1097 (1969) Determination of Mixtures of Copper(ll) and Manganese(ll) by Electron Spin Resonance
Determination of Samarium and Gadolinium in Rare Earth Ores by Neutron Capture Gamma-Ray Activation Analysis
M n ( I I ) and C u ( I I ) are determined either alone or in mix tures in the concentration range 10"1 to 10~SM with a pre cision of 0.4% by E S R spectrometry.
Sm and Gd are simultaneously determined in four rare earth ores with a relative standard deviation of less than 6% in 57 determinations.
GEORGE G. GUILBAULT and TIBOR MEISEL, Department of Chemistry, Louisiana State University in New Orleans, New Orleans, La. 70122
S. M. LOMBARD and T. L. ISENHOUR, Chemistry Depart ment, University of Washington, Seattle, Wash. 98105 Anal. Chem., 41, 1113
Anal. Chem., 41, 1100 Distinguishing Aliphatic Carboxylic Acids and Anhydrides by Proton Magnetic Resonance Spectrometry
l,2,3-Tris-(2-Diethylaminoethoxy)benzene Hydrochloride as Reagent for the Determination of Nitrite and Bromate Ions
Magnetic anisotropy of the carbonyl group causes the reso nance of the α-hydrogens in oarboxylic (anhydrides to be shifted downfield relative to the corresponding acids. JAMES R. PARKER, Analytical Research, PPG Inc., New Martinsville, W. Va. 26155
(1969)
(1969)
Industries,
Anal. Chem., 41, 1103
IVAN ODLER, Bratislava, (1969)
Differentiating Spectrophotometric Titration of Phenobarbital-Diphenylhydantoin Combinations in Nonaqueous Medium The mixtures are analyzed in acetonitrile with triethyl-nbutylammonium hydroxide in benzene methanol as titrant. The afosorbance change is noted at 293 nm, SURAJ P. AGARWAL, Department of Biochemistry, The Chicago Medical School, University of Health Sciences, Chicago, III. 60612, MARTIN I. BLAKE, Department of Pharmacy, University of Illinois at the Medical Center, Chicago, III. 60612 Anal. Chem., 41, 1104
The reactions of this reagent with N 0 2 " and Br0 3 " ions can be used in qualitative and quantitative analysis. Nitrite ions yield a brown complex, and bromate ions yield a yellow complex.
(1969)
Czechoslovakia Anal. Chem., 41, 1116
(1969)
Gas Chromatographic Determination of Polyhydric Alcohols in Oils and Alkyd Resins by Formation of Trimethylsilyl Derivatives A portion of the reaction mixture is injected onto a silicone grease column where the polyols, as their T M S ethers, are separated and determined simultaneously. GEORGE G. ESPOSITO and M. H. SWANN, U. S. Army Coating and Chemical Laboratory, Aberdeen Proving Ground, Md. 21005 Anal. Chem., 41, 1118 VOL. 4 1 , NO. 8, JULY 1969
(1969) ·
15 A
AC BRIEFS Chromatopolarographic Investigation of Radiolytic Products in the Aqueous—Ethylene System
Polarographic Studies on Chloroacetones
The radiolytic products detected b y this chromatopolaro graphic technique are: hydrogen peroxide, nitrous acid, and nitromethane. R. K. BROSZKIEWICZ and Z. PRZYBYLOWICZ, Department of Radiation Chemistry, Institute of Nuclear Research, Warsaw, Poland Anal. Chem., 41, 1121
FABRIZIO BRUNER, G. PAOLO CARTON/, and MASSIMILIANO POSSANZINI, Istituto Chimica Analitica, Univers/ta di Rome, Rome, Italy (1969)
Assay for Heroin in Illicit Preparations Using Partition Chromatography An ion pair extraction method using a Celite column system quantitatively separates heroin from diluents and impurities found in illicit preparations. GEORGE R. NAKAMURA and HERMAN J. MEURON, Al cohol, Tobacco, and Firearms Laboratory, Internal Revenue Service, Box 36075, San Francisco, Calif. 94102 (1969)
Determination of the Hydrocarbon-Type Composition of Petroleum Distillates Boiling up to 185 °C Using Type X Molecular Sieves T h e method is based on .the selective adsorption of aromatics on Type 10X molecular sieve. T h e apparatus is simple and easy to operate. J. V. BRUNNOCK and L. A. LUKE, BP Research Centre, The British Petroleum Co., Ltd., Chertsey Rd., Sunbury-onThames, Middlesex, England Anal. Chem., 41, 1126
Anal. Chem., 41, 1130
(1969)
Foam Separation of Lead(ll) with Sodium Lauryl Sulfate
The separation of methane molecules containing carbon iso topes C 12 , C 13 , C1*, and hydrogen, deuterium, and tritium with partial and complete substitution is reported.
Anal. Chem., 41, 1124
MAYNARD E. HALL and EDWARD M. HARRIS, University of Arkansas, Graduate Institute of Technology, Little Rock, Ark.
(1969)
Separation of Isotopic Methanes by Gas Chromatography
Anal. Chem., 41, 1122
D a t a indicate that the abnormally low diffusion currents obtained for polychlorina
