Briefs Analysis of Coal Asphaltenes by Carbon-13 Fourier Transform Nuclear Magnetic Resonance Spectrometry 1794 Aromaticity is determined by three methods and t h e accuracy studied by analysis of variance. Molecular size is estimated. Valdmir Sklenâr,* Milan Hâjek, Gustav Sebor, Ivo Lang, Miloslav Suchanek, and Zenon Starcuk, Institute of Scientific Instruments, Czechoslovak Academy of Sciences, 612 64 Brno, Czechoslovakia Anal. Chem., 52 (1980) Ion Mobilities and Residence Times under Chemical Ionization Conditions 1797 A pulsed chemical ionization (CI) source employs a coaxial electron entrance-ion exit to obtain ion mobility data in good agreement with drift tube measurements and residence times a t 125-150 °C under typical CI conditions. C. W. Polley, Jr., A. J. lilies, and G. G. Meisels, * Department of Chemistry, University of Nebraska-Lincoln, Lincoln, Neb. 68588 Anal. Chem., 52 (1980) Repetitive Laser Desorption Mass Spectrometry for Nonvolatile Organic Compounds 1803 Values for various instrumental parameters and sample conditions are optimized using sucrose as a test compound. Repetitive pulsed laser desorption (RLD) mass spectra of sucrose and other nonvolatile organic compounds are obtained with a scanning mass spectrometer. Franz Heresch,* E. R. Schmid, and J . F. K. Huber, Institute of Analytical Chemistry, University of Vienna, Waehringerstr. 38, A1090 Vienna, Austria Anal. Chem., 52 (1980) Determination of Molecular Weight Distributions of Polystyrene Oligomers by Field Desorption Mass Spectrometry 1808 Field desorption M S (FDMS) determines molecular weight averages (M n a n d M w ) for three polystyrene standards having weights up t o 5300 amu. Values compare favorably to those obtained by conventional techniques. Robert P. Lattimer* and Dale J . Harmon, The BFGoodrich Research and Development Center, 9921 Brecksville Road, Brecksville, Ohio 44141, and Gordon E. Hansen, Department of Pharmacology and Experimental Therapeutics, The Johns Hopkins University School of Medicine, 725 North Wolfe Street, Baltimore, Md. 21205 Anal. Chem., 52 (1980) Isotope Ratio Measurements of Urinary Calcium with a Thermal Ionization Probe in a Quadrupole Mass Spectrometer 1811 Natural abundance isotope ratios are measured with average relative accuracies >2% and average relative precisions ~ 1 % standard deviation. Alfred L. Yergey,* Nancy E. Vieira, and James W. Hansen, Intramural Research Program and Neonatal and Pediatric Medicine Branch, National Institute of Child Health and Human Development, National Institutes of Health, Bethesda, Md. 20205 Anal. Chem., 52 (1980)
Corresponding author. I Supplementary material available.
Thin-Layer Chromatographic and High Resolution Mass Spectrometric Determination of jd-Hydroxyphenylethylamines in Tissues as DansylAcetyl Derivatives 1815 Acetylation of t h e /3-hydroxy group prevents dehydrogenation a n d reduces blanks obtained with only dansyl derivatives. T h e /3-hydroxyphenylethylamines can be q u a n t i t a t e d to 200 pg (1-2 nmol) in samples. David A. Durden,* Augusto V. Juorio, and Bruce A. Davis, Psychiatric Research Division, 508A University Hospital, Saskatoon, Saskatchewan, Canada S7N 0X0 Anal. Chem., 52 (1980) Base Peak Profiles of Gas Chromatography-Mass Spectrometric Data Obtained from Thermal Desorption of Activated Carbons 1821 Computer-calculated base peak profiles reveal in a numerical format t h e major volatile compounds adsorbed on activated carbons used in water treatment. Complementary base peak profiles generated by electron impact- and chemical ionization-mass spectrometry suggest their potential for water t r e a t m e n t process monitoring. Katherine Alben, Environmental Health Center, Division of Laboratories and Research, New York State Department of Health, Albany, N.Y. 12201 Anal. Chem., 52 (1980) Gas Chromatographic-Mass Spectrometric Analysis of Chlorination Effects on Commercial Coal-Tar Leachate 1825 A b u n d a n t oxygenated and halogenated polycyclic aromatic hydrocarbons (PAHs) are found in chlorinated coal tar leachate samples, whereas parent PAHs, alkyl, and nitrogen-substituted P A H s are predominant in nonchlorinated samples. Katherine Alben, Environmental Health Center, Division of Laboratories and Research, New York State Department of Health, Albany, N.Y. 12201 Anal. Chem., 52 (1980) Interlaboratory Comparison of Determinations of Trace Level Hydrocarbons in Mussels 1828 • Concentrations of total extractable hydrocarbons, total hydrocarbons in t h e gas chromatographic elution range, and individual hydrocarbon compounds differed by less than a factor of four. Factors are discussed which contribute to t h e intralaboratory precision (1 σ) of ±40%. S. A. Wise,* S. N. Chesler, F. R. Guenther, H. S. Hertz, L. R. Hilpert, W. E. May, and R. M. Parris, Organic Analytical Research Division, Center for Analytical Chemistry, National Bureau of Standards, Washington, D.C. 20234 Anal. Chem., 52 (1980) Determination of /V-Nitrosamines from Diesel Engine Crankcase Emissions 1833 Detection limits for a 60-L sample are 0.1 Mg/m 3 for 2Vnitrosodimethylamine and 0.16 μg/m 3 for Nnitrosomorpholine. E. Ulku Goff,* James R. Coombs, and David H. Fine, New England Institute for Life Sciences, 125 Second Avenue, Waltham, Mass. 02154, and Thomas M. Baines, Environmental Protection Agency, 2565 Plymouth Road, Ann Arbor, Mich. 48105 Anal. Chem., 52 (1980)
1236 A · ANALYTICAL CHEMISTRY, VOL. 52, NO. 12, OCTOBER 1980
Briefs Volatile Environmental Pollutants in Biological Matrices with a Headspace Purge Technique
1836
Volatile organic compounds are determined in h u m a n blood, urine, adipose tissue, and milk with a dynamic headspace and recoveries of 60-95%. Larry C. Michael,* Mitchell D. Erickson, Sandra P. Parks, and Edo D. Pellizzari, Chemistry and Life Sciences Group, Research Triangle Institute, P.O. Box 12194, Research Triangle Park, N.C. 27709 Anal. Chem., 52 (1980) Gas-Phase Coulometric Detector for Gas Chromatography
1842
T h e pulsed electron capture of displaced coaxial design provides greater accuracy in the measurement of its electron density and electron loss by reaction with CC14 t h a n does the concentric coaxial design. E. P. Grimsrud* and S. W. Warden, Department of Chemistry, Montana State University, Bozeman, Mont. 59717 Anal. Chem., 52 (1980) Determination of α-Chloroacetanilides in Water by Gas Chromatography and Infrared Spectrometry 1845 After extractive workup, α-chloroacetanilides in water are determined at the low p p b level by GC with nitrogenselective detection. Confirmation is obtained by GCFourier transform IR spectrometry. Jimmy W. Worley,* Melvin L. Rueppel, and Fredrick L. Rupel, Research Department, Monsanto Agricultural Products Company, 800 North Lindbergh Boulevard, St. Louis, Mo. 63166 Anal. Chem., 52 (1980) Diffuse Reflectance Infrared Spectrometric Analysis of Ultrathin Film Carbowax 20M on Chromosorb W 1849 After heating, several spectral changes are noted that indicate a condensation reaction between the Carbowax 20M and silica hydroxyls and a conformational change of the Carbowax 20M ether units. M. A. Kaiser* and D. B. Chase, Central Research & Development Department, E. I. du Pont de Nemours and Co., Experimental Station, Wilmington, Del. 19898 Anal. Chem., 52 (1980) Aromatic Disulfides in the Detection of Thiols
1851
Seven dithiodianils are compared with 3,3'-dithiobis[6-nitrobenzoic acid] (Ellman's reagent) in a spot detection test for thiols. Detection limits for 1-butanethiol are 0.5-2 μg with the dithiodianils and 10 Mg with Ellman's reagent. Thaddeus J. Novak,* Stephen G. Pleva, and Joseph Epstein, Research Division, Chemical Systems Laboratory, Aberdeen Proving Ground, Md. 21010 Anal. Chem., 52 (1980) Spectrophotometric Determination of Micro Amounts of Trithionate via Mercury(II) Thiocyanate Reaction 1855 T h e method gives an RSD of 0.60% for 1 Χ ΙΟ" 4 Μ trithionate. Yasuyuki Miura* and Tomozo Koh, Department of Chemistry, Faculty of Science, Tokai University, Hiratsuka, Kanagawa 25912, Japan Anal. Chem., 52 (1980)
Absorption Correction via Scattered Radiation in Energy-Dispersive X-ray Fluorescence Analysis for Samples of Variable Composition and Thickness 1859 A precision of 5% or better is typically achieved for determinations of μ (2.956 keV) for sample thicknesses above 1.5 mg c m - 2 . Peter M. Van Dyck and Rene E. Van Grieken,* Department of Chemistry, University of Antwerp (UIA), Universiteitsplein 1, B-2610 Wilrijk, Belgium Anal. Chem., 52 (1980) Identification of Tetrachlorodibenzo-p-dioxin Isomers at the 1-ng Level by Photolytic Degradation and Pattern Recognition Techniques 1865 Under equivalent light exposure conditions, photolytic half-lives are determined for 22 T C D D isomers in dilute hydrocarbon solution and as a diffuse molecular dispersion on a clean soft-glass surface. T. J. Nestrick* and L. L. Lamparski, Analytical Laboratories, Dow Chemical U.S.A., Michigan Division, Midland, Mich. 48640, and D. I. Townsend, Process Development, Dow Chemical U.S.A., Michigan Division, Midland, Mich. 48640 Anal. Chem., 52 (1980) Separation of Chloride and Bromide from Complex Matrices Prior to Ion Chromatographic Determination 1874 A silver-loaded cation exchange column separates the halides and eliminates most interferences observed in the direct analyses of the complex solutions as encountered in the nuclear fuel reprocessing industry. Darryl D. Siemer, Exxon Nuclear Idaho Company, Inc., P.O. Box 2800, Idaho Falls, Idaho 83401 Anal. Chem., 52 (1980) Determination of Molecular Weight Distributions of Polymerized Petroleum Pitch by Gel Permeation Chromatography with Quinoline Eluent 1877 Acquisition of a linear gel permeation chromatography polymerized pitch calibration curve, obtained for the 4502000 molecular weight range, indicates t h a t the technique is applicable for obtaining molecular weight distributions of petroleum pitch mesophases and semicokes having quinoline-insoluble contents approaching 100%. R. A. Greinke* and L. H. O'Connor, Union Carbide Corporation, Carbon Products Division, Parma Technical Center, P.O. Box 6116, Cleveland, Ohio 44101 Anal. Chem., 52 (1980) Determination of Extraction Constants for Lead(ll), Zinc(ll), Thallium(l), and Manganese(ll) Dithiocarbamates by a Two-Step Extraction Method 1882 A 2-step extraction method with radiometry determines relatively low extraction constants for the diethyldithiocarbamates and pyrrolidinedithiocarbodithioates. L. H. Shen, S. J. Yeh,* and J. M. Lo, Institute of Nuclear Science, National Tsing Hua University, Hsinchu, Taiwan 300, Republic of China Anal. Chem., 52 (1980)
1238 A · ANALYTICAL CHEMISTRY, VOL. 52, NO. 12, OCTOBER 1980
Briefs Glancing Incidence External Reflection Spectroelectrochemistry with a Continuum Source 1885
Determination of Atmospheric Sulfur Dioxide without Tetrachloromercurate(ll) and the Mechanism of the Schiff Reaction 1912
T h e previously reported technique is expanded to cover the entire UV-visible spectral range, and is useful on electrodes made from bulk metals or glassy carbon. Joan P. Skully and Richard L. McCreery,* Department of Chemistry, The Ohio State University, Columbus, Ohio 43210 Anal. Chem., 52 (1980)
A dilute solution of formaldehyde buffered at p H 4 collects and stabilizes atmospheric SO2 determined subsequently by a spectrophotometric method. A new mechanism is proposed for the chromogen formation. Purnendu K. Dasgupta,* Kymron DeCesare and James C. Ullrey, California Primate Research Center, University of California, Davis, Calif. 95616 Anal. Chem., 52 (1980)
Simultaneous Determination of Tin and Lead at the Parts-per-Billion Level by Coupling Differential Pulse Anodic Stripping Voltammetry with a Matrix Exchange Method 1889 T i n - l e a d interference in anodic stripping voltammetry is eliminated with citrate media as a supporting electrolyte. Elio Desimoni, Francesco Palmisano,* and Luigia Sabbatini, Instituto di Chimica Analitica dell'Università di Bari, Via Amendola, 173-70126 Bari, Italy Anal. Chem., 52 (1980) Anion-Selective Electrode Based on Oleophilic Anion Exchange Resin Membrane 1893 T h e membranes are impregnated with water-immiscible organic solvent and show good anion selectivity. Toshihiko I mat o, Akinori Jyo, and Nobuhiko Ishibashi,* Department of Applied Analytical Chemistry, Faculty of Engineering 36, Kyushu University, Fukuoka 812, Japan Anal. Chem., 52 (1980) Automated Continuous-Flow Determination of Serum Albumin by Differential Pulse Polarography 1896 Albumin is determined selectively in serum at 60 samples/h in the concentration range 10-500 mg/L, giving a correlation coefficient of 0.9934 with the bromocresol green colorimetric method. P. W. Alexander* and M. H. Shah, Department of Analytical Chemistry, University of New South Wales, P.O. Box 1, Kensington, 2033 New South Wales, Australia Anal. Chem., 52 (1980) Copper(II) Titration of Fulvic Acid Ligand Sites with Theoretical, Potentiometric, and Spectrophotometric Analysis 1901 Polyelectrolyte titration theory is developed for both experiments. T h e titration functions emphasize the stronger binding of Cu(II) by the first sites occupied. Donald S. Gamble,* Chemistry and Biology Research Institute, Agriculture Canada, Ottawa, Ontario, Canada K1A 0C6, and Alan W. Underdown and Cooper H. Langford,* Metal Ions Group, Chemistry, Carleton University, Ottawa, Ontario, Canada KlS 5B6 Anal. Chem., 52 (1980) Combustion-Ion Chromatographic Determination of Chlorine in Silicate Rocks 1908 Values from 10-1000 p p m are listed for 30 geochemical standards with a typical R S D of ±5%. T h e method compares favorably with neutron activation analysis and X-ray fluorescence. Keenan L. Evans and Carleton B. Moore,* Department of Chemistry, Arizona State University, Tempe, Ariz. 85281 Anal. Chem., 52 (1980)
High-Performance Digital Timing System
1923
T h e unit is particularly useful for time of flight mass spectrometers. T h e times of 15 events occurring in one timing period (up to 1.3 ms) can be determined with an accuracy of 5/8 ns. R. F. Bonner, D. V. Bowen, B. T. Chait, A. B. Lipton, and F. H. Field,* The Rockefeller University, New York, N.Y. 10021, and W. F. Sippach, Nevis Laboratories, Columbia University, Irvington, N.Y. 10533 Anal. Chem., 52 (1980) Piezoelectric Crystals as Detectors in Liquid Chromatography
1929
Piezoelectric crystals with modified surfaces detect adsorption of solute from a liquid via shifts in crystal resonance frequency. Pamela L. Konash, Department of Chemistry, Georgetown University, Washington, D.C. 20057, and Glenn J. Bastiaans,* Department of Chemistry, Texas A&M University, College Station, Tex. 77843 Anal. Chem., 52 (1980) High-Performance Liquid Chromatographic Determination of 5-Halopyrimidinone Interferon Inducers
1931
T h e method detects a new class of interferon inducers with an RSD of ±6.7% for serum concentrations of 15 μg/mL. M. A. Wynalda and F. A. Fitzpatrick,* Drug Metabolism Research, Unit 7256, Pharmaceutical Research and Development, The Upjohn Company, Kalamazoo, Mich. 49001 Anal. Chem., 52 (1980) Field Effect Transistor Sensitive to Penicillin
1935
T h e probe has a lifetime of two months, a response time T63 = 25 s and is immune to temperature fluctuations. Sensitivities and range are comparable to conventional penicillin-sensitive macroelectrodes. Steve Caras and Jif i Janata,* Department of Bioengineering, University of Utah, Salt Lake City, Utah 48112 Anal. Chem., 52 (1980) Adenosine-Selective Electrode
1937
T h e electrode can detect adenosine at the 2-10 μ Μ level a t p H 9.0 and 37 °C. Inna Deng and Chris Enke,* Department of Chemistry, Michigan State University, East Lansing, Mich. 48824 Anal. Chem., 52 (1980)
1240 A · ANALYTICAL CHEMISTRY, VOL. 52, NO. 12, OCTOBER 1980
Free GC Manual Applications of the Photoionization Detector In Gas Chromatography. • Analyses of drugs and pesticides at 10X below conventional detectors • Capillary column analyses at 100X below other detectors • Environmental and industrial hygiene determinations including V.C., TEL, PAH's, H2S, CS2, and other organic sulfurs
New high temperature
photoionization detector
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Preconcentration and Determination of Ferrocenecarboxaldehyde at a Chemically Modified Platinum Electrode 19
Detection is 10~ 7 M for a preconcentration time of 5 min No major interference is observed when analysis is in the presence of a 100-fold excess of ferrocene. John F. Price and Richard P. Baldwin,* Department of Chemistry, University of Louisville, Louisville, Ky. 40208 Anal. Chem., 52 (19
for gas chromatography
• Inorganics including phosphine, arsine, ammonia • Hydrocarbons including FAME'S, aliphatics, aromatics and Ketones. ' f - ; ....... , .. . . . . . , V :
Briefs
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The most significant new detector for gas chromatography in the past two decades
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Sedimentation Field Flow Fractionation of 1S Macromolecules and Colloids High-resolution separations of inorganic particulates, polymer latices, viruses and biopolymers are carried out
