Briefs Microcomputer-Controlled Interface between a High Performance Liquid Chromatograph and a Diffuse Reflectance Infrared Fourier Transform Spectrometer 1394 Interfacing yields submicrogram detection limits. T h e solvent is automatically eliminated prior to t h e m e a s u r e m e n t of t h e spectrum. Donald T. Kuehl and Peter R. Griffiths,* Department of Chemistry, Ohio University, Athens, Ohio 45701 Anal. Chem., 52 (1980) Detector Based on Optical Activity for High Performance Liquid Chromatographic Detection of Trace Organics 1399 T r a c e levels of optically active molecules are d e t e r m i n e d in a micro-polarimeter based on laser optics. A detection limit of 0.5 μg in 200 μ ι , is achieved for separation of two sugars. Edward S. Yeung,* Larry E. Steenhoek, Steven D. Woodruff, and J. C. Kuo, Ames Laboratory and Department of Chemistry, Iowa State University, Ames, Iowa 50011 Anal. Chem, 52 (1980) Utility of Mixed Packings in Gas-Liquid Chromatography
1415
T h e precision of the m e t h o d for quantitatively comparing two absorbance spectra by the weighted least-squares m e t h o d with a two-parameter model is improved, and errors due to flicker and stray light are rejected. Kenneth L. Ratzlaff, Department of Chemistry, The Michael Faraday Laboratories, Northern Illinois University, DeKalb, 111. 60115 Anal. Chem., 52 (1980) Double Beam-in-Time Photoacoustic Spectrometer 1420 T h e double beam-in-time P A S system employs an oscillating mirror a n d a cell having a single microphone. It inherently compensates for wavelength variations in the source radiation. Michael F. Cox, Geoffrey N. Coleman,* and T e r r y W. McCreary, Department of Chemistry, University of Georgia, Athens, Ga. 30602 Anal. Chem., 52 (1980) Determination of Nitrogen Oxides and Nitric Acid Vapor by Infrared Spectrometry 1424
1402
Retentions with mechanical mixtures of p u r e - p h a s e GLC packings are shown t o correspond to a simple relationship. Separations m a y t h u s be predicted with confidence from d a t a pertaining only to the pure solvents. C.-F. Chien and R. J. Laub,* Department of Chemistry, The Ohio State University, Columbus, Ohio 43210, and M. M. Kopecni, Chemical Dynamics Laboratory, Boris Kidric Institute of Nuclear Sciences—VINCA, P.O. Box 522, 11001-Beograd, Yugoslavia Anal. Chem., 52 (1980) Replication of Gas-Liquid Chromatographic Retentions with Silicone Stationary Phases
Linear Parameter Estimation in Rapid-Scan Spectrophotometry
1407
Relative retentions (hence, separations) with p u r e OV methylphenylsilicone phases are replicated with mechanical mixtures of packings of other selective a n d nonselective OV phases. C.-F. Chien and R. J . Laub,* Department of Chemistry, The Ohio State University, Columbus, Ohio 43210, and M. M. Kopecni, Chemical Dynamics Laboratory, Boris Kidric Institute of Nuclear Sciences—VINCA, P.O. Box 522, 11001-Beograd, Yugoslavia Anal. Chem., 52 (1980) Determination of BHT, Irganox 1076, and Irganox 1010 Antioxidant Additives in Polyethylene by High Performance Liquid Chromatography 1411 R S D s are 1.2, 1.3, a n d 2.0% for B H T , Irganox 1076, a n d Irganox 1010, respectively. Limits of detection are 0.0006, 0.002, and 0.004% for B H T , Irganox 1076, a n d Irganox 101Ô, respectively, in polyethylene. J . F. Schabron* and L. E. Fenska, Phillips Petroleum Company Research Center, Bartlesville, Okla. 74004 Anal. Chem., 52 (1980)
* Corresponding author. • S u p p l e m e n t a r y material available. 976 A · ANALYTICAL CHEMISTRY, VOL. 52, NO. 9, AUGUST 1980
In gas mixtures containing nitrogen oxides and water, nitrous acid vapor can be detected, especially at high N O / NO2 ratios. J a n B. Lefers* and Pieter J . van den Berg, Laboratory of Chemical Technology, Delft University of Technology, Julianalaan 136, 2628 BL Delft, The Netherlands Anal. Chem., 52 (1980) Mixed Immobilized Enzyme-Porous Electrode Reactor 1426 T h e design, operation, and characteristics are described for a mixed e n z y m e - p o r o u s carbon electrode reactor. W. J . Blaedel* and Joseph Wang, Department of Chemistry, University of Wisconsin—Madison, Madison, Wis. 53706 Anal. Chem., 52 (1980) Quantitative Determination of Chloride, Chlorite, and Chlorate Ions in a Mixture by Successive Potentiometric Titrations 1430 Precision is > 2% (2-15 μιτιοί), a n d the results are in good agreement with other m e t h o d s . Air oxidation is eliminated, a n d direct comparison is p e r m i t t e d between t h e chlorine balance and t h e redox balance in solutions containing mixtures of oxychlorine species. Tsung-Fei Tang and Gilbert Gordon,* Department of Chemistry, Miami University, Oxford, Ohio 45056 Anal. Chem., 52 (1980) Determination of Labilities of Soluble Trace Metal Species in Aqueous Environmental Samples by Anodic Stripping Voltammetry and Chelex Column and Batch Methods 1433 Sequential preconcentration procedures divide p p b and s u b - p p b concentrations of Cd, Cu, P b , and Zn into four lability categories (operationally defined). Diverse environmental samples yield similar p a t t e r n s . Paul Figura and Bruce McDuffie,* Laboratory for Trace Methods and Environmental Analysis, Department of Chemistry, State University of New York at Binghamton, Binghamton, N Y . 13901 Anal. Chem., 52 (1980)
Briefs
Measurement of Direct Currents and Pulse Components for Analytical Evaluation of Differential Pulse Polarography and Voltammetry 1439
Automated Purity Determination by Stepwise Melting in Differential Scanning Calorimetry 1474H An equation is developed for use in accurate purity determinations without arbitrary d a t a manipulation. Error is within 10% of the doped impurity level (maximum 10 mol %). Arnold C. Ramsland, Hoffmann-La Roche Inc., Research and Diagnostic Products Section, Quality Control Department, Nutley, N.J. 07110 Anal. Chem., 52 (1980)
Additional data are obtained by simple modifications of differential pulse polarographs. Access to the additional d a t a aids in the analytical and theoretical evaluation of differential pulse polarography and voltammetry. J . E. Anderson and A. M. Bond,* Division of Chemical and Physical Sciences, Deakin University, Waurn Ponds 3217, Victoria, Australia Anal. Chem., 52 (1980)
Characterization of a 2,2'-DiaminoethylamineCellulose Filter toward Metal Cation Extraction
Use of the Oxygen KLL Auger Lines in Identification of Surface Chemical States by Electron Spectroscopy for Chemical Analysis 1445 T h e oxygen K L L Auger group is recorded for 130 organic a n d inorganic compounds. T h e line energies and variable line distributions are useful in identification of surface chemical states. C. D. Wagner,* Surfex Company, 29 Starview Drive, Oakland, Calif. 94618, and D. A. Zatko, Department of Chemistry, University of Alabama, Tuscaloosa, Ala. 35486, and R. H. •Raymond, Shell Development Co., P.O. Box 1380, Houston, Tex. 77001 Anal. Chem., 52 (1980) Determination of Gross Alpha, Plutonium, Neptunium, and/or Uranium by Gross Alpha Counting on Barium Sulfate 1452 Alpha emitters are separated selectively by precipitation with barium sulfate u n d e r controlled oxidation conditions in a form suitable for direct alpha counting. Overall recoveries are 98%. Claude W. Sill, Radiological and Environmental Sciences Laboratory, Department of Energy, Idaho Falls, Idaho Anal. Chem., 52 (1980) Simplex Techniques for Nonlinear Optimization 1460 T h e utility of the nonlinear optimization technique, based on the modified simplex method of Neider and Mead, is demonstrated for several experimentally relevant functions. P. B a r r y Ryan,* Richard L. Barr, and H. David Todd,* HallAtwater Laboratories Chemistry, Wesleyan University, Middletown, Conn. 06457 Anal. Chem., 52 (1980)
1479
A cellulose filter with 2,2'-diaminodiethylamine functional groups provides collection yields less 85% for filtration velocities u p t o 2 m L m i n - 1 c m - 2 for the preconcentration of transition metal cations from aqueous samples. Practically no a b u n d a n t substance interferes with the transition metal collection. J . A. Smits and René Van Grieken,* Department of Chemistry, University of Antwerp (U.I.A.), Universiteitsplein 1, B-2610 Wilrijk, Belgium Anal. Chem., 52 (1980) Coating for a Piezoelectric Crystal Sensitive to Organophosphorus Pesticides 1484 A piezoelectric quartz crystal coated with 3-PAD, T r i t o n X-100, and N a O H possesses higher sensitivity, faster response, and a longer lifetime t h a n previously described coatings. Yutaka Tomita and George G· Guilbault,* Department of Chemistry, University of New Orleans, New Orleans, La. 70122 Anal. Chem., 52 (1980) Continuous Detection of Toluene in Ambient Air with a Coated Piezoelectric Crystal 1489 Carbowax 550 as the coating permits toluene vapor to be detected in the range 30-300 p p m with an R S D >4%. Response time is 30 s and the detector lifetime is > 2 months. Mat H. Ho and George G. Guilbault,* Department of Chemistry, University of New Orleans, New Orleans, La., and Bernd Rietz, National Institute of Working Environment, DK2900 Hellerup, Denmark
Measurement of Sputtering Yields and Ion Beam Damage to Organic Thin Films with the Quartz Crystal Microbalance 1467 T h e a p p a r a t u s is tested with Ag films deposited on the quartz crystal, and then extended to m e a s u r e m e n t s on organic overlayers in the 3000-7000 Â thickness regime. Results are given for the sputtering of thin films of polystyrene and polymethylmethacrylate. Dale M. Ullevig and J o h n F. Evans,* Department of Chemistry, University of Minnesota, Minneapolis, Minn. 55455 Anal. Chem., 52 (1980)
978 A · ANALYTICAL CHEMISTRY, VOL. 52, NO. 9, AUGUST 1980
Ultrasonic Extraction of Polychlorinated Dibenzo-pdioxins and Other Organic Compounds from Fly Ash from Municipal Incinerators 1492 E x t r a c t s analyzed directly by G C / M S yield averages a n d s t a n d a r d deviations (ng/g) for the tetra- to octachlorinated dibenzo-p-dioxins of 8.6 ± 2.2,15.0 ± 4.0, 13.0 ± 3.4, 3.2 ± 1.0, a n d 0.4 ± 0.1, respectively. G. A. Eiceman, A. C. Viau, and F. W. Karasek,* GuelphWaterloo Centre for Graduate Work in Chemistry, Waterloo Campus, Department of Chemistry, University of Waterloo, Waterloo, Ontario N2L 3G1 Canada Anal. Chem., 52 (1980)
Briefs
Radioimmunoassay for Quantitation of 2,3,7,8Tetrachlorodibenzofuran
1497
Voltammetric Methods for Determination of Metal Binding by Fulvic Acid 1515
Nonionic d e t e r g e n t solubilizes t h e h y d r o p h o b i c dibenzofurans p e r m i t t i n g t h e i r binding t o antibodies. Detection limits range between 20 pg a n d 4.0 ng 2,3,7,8TCDF. Michael I. Luster,* Phillip W. Albro, K u n Chae, Lela D. Lawson, J e a n T. Corbett, and J a m e s D. McKinney, Laboratory of Environmental Chemistry, National Institute of Environmental Health Sciences, P.O. Box 12233, Research Triangle Park, N.C. 27709 Anal. Chem., 52 (1980)
Anodic s t r i p p i n g v o l t a m m e t r i c a n d differential pulse polarographic results for characterizing Cd, Cu, P b , N i , a n d Zn complexation with fulvic acid indicate t h a t fulvic acid adsorbs on t h e H g electrode surface a n d forms electroactive complexes. T h e s e m e t h o d s should be used cautiously for s t u d y i n g m e t a l binding by fulvic acid. S. A. Wilson, T. C. Huth, R. E. Arndt, and R. K. Skogerboe,* Department of Chemistry, Colorado State University, Fort Collins, Colo. 80523 Anal. Chem., 52 (1980)
Carbon Monoxide Detection in Nitrogen Gas by Atmospheric Pressure Ionization Mass Spectrometry 1500
Cation Chromatography with a Conductivity Detector 1519
A d d i t i o n of 100 p p m K r t o s a m p l e gas eliminates m o s t ion species p r o d u c e d from nitrogen a n d only ions relating t o CO ((CO>2 + a n d K r + C O ) a r e d e t e c t e d . C O c o n c e n t r a t i o n in a purified nitrogen gas is ~ 1 1 0 p p b . Hideki Kambara,* Yukiko Ogawa, Yasuhiro Mitsui, and Ichiro Kanomata, Central Research Laboratory, Hitachi, Ltd., Kokubunji, Tokyo 185, Japan Anal. Chem., 52 (1980) Tubular Flow Donnan Dialysis
A cation-exchange column of low capacity provides good resolution for t h e s e p a r a t i o n of m e t a l a n d a m m o n i u m ions. S e p a r a t i o n s require 5 - 1 0 m i n a n d are d e m o n s t r a t e d for alkali m e t a l ions, a m m o n i u m , Mg(II), a n d Ca(II) in d r i n k i n g water. J a m e s S. Fritz,* Douglas T. Gjerde, and Rose M. Becker, Ames Laboratory and Department of Chemistry, Iowa State University, Ames, Iowa 50011 Anal. Chem., 52 (1980)
1503 6
-8
L i n e a r calibration curves in t h e range 10~ t o 1 0 M Cu, Cd, a n d Zn a n d 50-fold e n r i c h m e n t s a r e achieved in 20 min. J a m e s A. Cox* and Zbigniew Twardowski, Department of Chemistry and Biochemistry, Southern Illinois University at Carbondale, Carbondale, 111. 62901 Anal. Chem., 52 (1980) Double Layer Capacitance Measurements with Digital Synchronous Detection at a Dropping Mercury Electrode 1506 T h e m e t h o d described employs a H a d a m a r d t r a n s f o r m algorithm. Advantages a n d disadvantages a r e c o m p a r e d for H a d a m a r d transform algorithm vs. Fourier t r a n s f o r m ac polarography. Paul F . Seelig and Robert de Levie,* Department of Chemistry, Georgetown University, Washington, D.C. 20057 Anal. Chem., 52 (1980) Gel Permeation Chromatography of Coal-Derived Products with On-Line Infrared Detection 1511 I R detection is applied t o size separation of h e x a n e soluble solvent refined coal (SRC) a n d various S R C fractions previously s e p a r a t e d on a silica column. R. S. Brown, D. W. Hausler, a n d L. T. Taylor,* Department of Chemistry, Virginia Polytechnic Institute and State University, Blacksburg, Va. 24061 Anal. Chem., 52 (1980)
980 A · ANALYTICAL CHEMISTRY, VOL. 52, NO. 9, AUGUST 1980
Correspondence Low-Power Inductively Coupled Nitrogen Plasma Discharge for Spectrochemical Analysis 1523 Ramon M. Barnes,* a n d G e r h a r d A. Meyer, Department of Chemistry, GRC Tower I, University of Massachusetts, Amherst, Mass. 01003 Anal. Chem., 52 (1980) Resolution and Signal-to-Noise in Fourier Transform Mass Spectrometry 1525 Robert L. White, E d w a r d B. Ledford, J r . , Sahba Ghaderi, Charles L. Wilkins,* a n d Michael L. Gross,* Department of Chemistry, University of Nebraska—Lincoln, Lincoln, Neb. 68588 Anal. Chem., 52 (1980) Breakdown of Methylmercury in Sodium Hydroxide Solution 1527 Chris J . Cappon* and J . Crispin Smith, Environmental Health Sciences Center and Department, of Pharmacology and Toxicology, University of Rochester School of Medicine and Dentistry, Rochester, N.Y. 14642 Anal. Chem., 52 (1980)
GAS SAMPLING CYLINDERS
Briefs Solvent Swelling for Enhancement of Carbon-13 Nuclear Magnetic Resonance Spectral Information from Insoluble Polymers: Chloromethylation Levels in Crosslinked Polystyrenes 1529 Stanley L. Manatt,* and David Horowitz, Information Systems, Research Section, Jet Propulsion Laboratory, California Institute of Technology, Pasadena, Calif. 91103, and Robert Horowitz, Fruit and Vegetable Chemistry Laboratory, U.S. Department of Agriculture, Science and Education Administration, Pasadena, Calif. 91106, and Robert P. Pinnell,* Joint Science Department, Scripps, Pitzer, and Claremont Men's Colleges, Claremont, Calif. 91711 Anal. Chem., 52 (1980)
Polymer Membrane Electrode-Based Potentiometric Ammonia Gas Sensor 1532 Mark E. Meyerhoff, Department of Chemistry, The University of Michigan, Ann Arbor, Mich. 48109 Anal. Chem., 52 (1980)
Hydrogen Sulfide Removal with Boric Acid
1534
Marian M. Schnepfe, U.S. Geological Survey, Reston, Va. 22090 Anal. Chem., 52 (1980)
Aids for Analytical Chemists Sampling Error in Fourier and Hadamard Transform Capacitance Measurements 1535 Robert de Levie, Department of Chemistry, Georgetown University, Washington, D.C. 20057 Anal. Chem., 52 (1980)
Modification of a Conventional Flame Photometric Detector for Increased Tin Response 1537 Walter A. Aue* and Christopher G. Flinn, Department of Chemistry, Dalhousie University, Halifax, Nova Scotia B3H 4J3, Canada Anal. Chem., 52 (1980)
Use of an Automated, Stepping Differential Calorimeter for the Determination of Molecular Weight 1538 J . Zynger* and A. D. Kossoy, Lilly Research Laboratories, Eli Lilly and Company, Indianapolis, Ind. 46206 Anal. Chem., 52 (1980)
Microdetermination of Selenium with Ascorbic Acid 1540 Fawzy F. El-Enany*, Kariman Mahmoud, and M. M. Varma, Office of Occupational Health and Industrial Hygiene, Ministry of Public Health, P.O. Box 5, Kuwait, Arabian Gulf Anal. Chem., 52 (1980)
Matheson offers gas sampling cylinders in a wide variety of sizes, configurations and materials of construction. The units may be used to sample numerous gases and ambients (stack gases, biomedical atmospheres, auto emissions, etc). The latest addition to the line is the Matheson 1.3, named for its 1.3 liters (1300 cc) capacity. This all-aluminum, single-ended sampling cylinder comes with a diaphragm sealed aluminum, packless valve. The standard 1/4" FNPT valve connection provides convenient hookup. A unique member of the sampling cylinder line is a 250 ml glass bulb which comes with a special high-vacuum Teflon stopcock. All contact surfaces are inert and non-contaminating. Open the stopcock of the evacuated cylinder to capture the sample. Also available from Matheson are stainless steel 304, stainless steel 316 and monel gas sampling cylinders in single 'ended and double ended configurations. More information is available from Matheson, 1275 Valley Brook Avenue, P.O. Box E, Lyndhurst, NJ 07071. CIRCLE 153 ON READER SERVICE CARD
NBS TRACEABLE CALIBRATION GAS STANDARDS To meet the performance standards of the Environmental Protection Agency, stationary sources required to continuously monitor for gaseous pollutants must be calibrated and audited with calibration gas standards that are both accurate and stable. When it's time to calibrate your continuous monitor, you can rely on Matheson's NBS Traceable Gas Mixtures. Matheson makes gas mixture standards for air pollutants such as sulfur dioxide, nitric oxide, nitrogen dioxide, oxygen, carbon dioxide and carbon monoxide. Component concentrations in these calibration mixtures are traceable to the National Bureau of Standards, Standard Reference Materials via the E P A Traceability Protocol No. 1 or No. 2, dated June 15,1978. Each of these gas mixtures is compared to an NBS Standard Reference Material either directly, or through a gas manufacturer's primary standard which is referenced to an NBS Standard Reference Material. The stability of each reactive gas standard is verified before shipment and a written analysis is included with the cylinder to certify it has been analyzed according to the Protocol. For a current list of Matheson gas standards prepared via the E P A Traceability Protocol, write to Matheson, 1275 Valley Brook Avenue, P.O. Box E, Lyndhurst, NJ 07071. CIRCLE 154 ON READER SERVICE CARD
982 A · ANALYTICAL CHEMISTRY, VOL. 52, NO. 9, AUGUST 1980
Briefs
The quick and easy way t o precise density measurement·
Optically Transparent Thin-Layer Electrochemical Flow Cell for Liquid Chromatography 1542 Thomas C. Pinkerton, Kiamars Hajizadeh, Edward Deutsch, and William R. Heineman,* Department of Chemistry, University of Cincinnati, Cincinnati, Ohio 45221 Anal. Chem., 52 (1980)
Direct Constant-Current Electron Capture Detector 1544 Walter A. Aue* and K. W. Michael Siu, 5637 Life Sciences Centre, Dalhousie University, Halifax, Nova Scotia, Canada B3H 4J1 Anal. Chem., 52 (1980)
X-ray Photoelectron Spectra of Dithizone and Related Compounds 1546 A. Katrib* and A. Y. Kassim, Chemistry Department, Kuwait University, Kuwait Anal. Chem., 52 (1980)
Rotating Flow Mixing Device for Post Column Reaction in High Performance Liquid Chromatography 1548 Shin-Ichiro Kobayashi and Kazuhiro Imai,* Department of Analytical Chemistry, Faculty of Pharmaceutical Sciences, University of Tokyo, Hongo 7-3-1, Bunkyo-ku, Tokyo 113, Japan Anal. Chem., 52 (1980)
Liquid Chromatography Electrochemical Detector with a Porous Membrane Separator 1549
Measure solid concentrations, density, or specific gravity of your process liquids and gases with the Paar DMA55 density meter to assure consistent product quality. Small 0.7 ml samples from the process are injected, pumped, vacuum-suctioned or continuously flowed into the sample tube. In less than a second, the instrument calculates and displays a 5-place digital result on the readout. This can be automatically transferred to other instruments. The method is fast, simple and accurate. No need for separate temperature, weight or volume measurements. No pycnometer filling. Circle the number for full details. Mettler Instrument Corporation, Box 71, Hightstown, NJ 08520.
Kenneth A. Rubinson,* T. William Gilbert, and Harry B. Mark, Jr., Department of Chemistry, University of Cincinnati, Cincinnati, Ohio 45221 Anal. Chem., 52 (1980)
Determination of Low Levels of Copper by Atomic Absorption Spectrometry with a Simplified Extraction Technique 1551 W. Orville Calhoun* and R. B. Hurley, Badische Corporation, P.O. Drawer D, Williamsburg, Va. 23185 Anal. Chem., 52 (1980) Correction. Microcomputer Compatible Method of Resolving Rate Constants in Mixed First- and Second-Order Kinetic Rate Laws 1552 Paul B. Kelter and James D. Carr,* Department of Chemistry, University of Nebraska, Lincoln, Neb. 68588 Correction. Modification of a Commercial Micrometer Hanging Mercury Drop Electrode 1552 J. E. Bonelli, H. E. Taylor, and R. K. Skogerboe, U.S. Geological Survey, Denver Federal Center, Denver, Colorado 80225
Mettler
Electronic balances and weighing systems Thermal analysis instruments Titration instruments Automated laboratory systems
CIRCLE 148 ON READER SERVICE CARD 984 A · ANALYTICAL CHEMISTRY, VOL. 52, NO. 9, AUGUST 1980
