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A C BRIEFS Highlights of Articles in This Issue

Quantitative Gas Phase Analysis by Means of Electron Impact Spectrometry

An Automated Instrumental System for Fundamental Characterization of Chemical Reactions

Energy loss electron impact spectrometry applied to qualita­ tive and quantitative chemistry offers high sensitivity and specificity with easy data interpretation. This technique is related to optical absorption spectrometry, but offers con­ siderable advantages over the latter.

A computer-controlled instrumental system for the auto­ mated characteristics of chemical reactions is reported.

RICHARD E. GROJEAN, Northeastern University, Boston, Mass., and JOHN F. RENDINA, McPherson Instrument Corp., a Subsidiary of GCA Corp., Acton, Mass. Anal. Chem., 43, 162 (1971)

STANLEY N. DEMING and H. L. PARDUE, Department Chemistry, Purdue University, Lafayette, Ind.

of

Anal. Chem., 43, 192 (1971)

Determination of Aluminum by Thermometric Titration

Expanded Capability of the Coulter Counter with a New Aperture Apparatus

Aluminum can be determined accurately by thermometric titration with potassium fluoride in sodium chloride-sodium acetate solution. Most common metals either do not inter­ fere or can be masked.

Sample suspensions can be repeatedly cycled through the aperture to obtain improved counting statistics on small numbers of particles of a given size, the total sample being recoverable after analysis.

W. L. EVERSON, Shell Development ville, Calif.

D. A. FLINCHBAUGH, Homer Research Laboratories, Bethlehem Steel Corporation, Bethlehem, Pa. 18016 Anal. Chem., 43, 172 (1971)

Company,

Emery­

Anal. Chem., 43, 201 (1971) Hydrogen Chloride Partial Pressure of Dilute Hydrogen Chloride-Concentrated Lithium Chloride Aqueous Solutions

Use of a Modified Coulter Counter for Determining Size Distribution of Macroinclusions Extracted from Plain Carbon Steels

An apparatus and a procedure are described for measure­ ments of hydrogen chloride partial pressure (PHCI) of solvent systems with low water activity.

By using a Coulter Counter equipped with a new type of aperture apparatus, it is now practical to size and count small numbers of very large inclusions without prior size fractionation of chemically extracted and purified residues.

ELIO SCARANO, GIOVANNI GAY, and MICHELE FORINA, Institute of Analytical Chemistry, Faculty of Pharmacy, University of Genoa, Italy

D. A. FLINCHBAUGH, Homer Research Laboratories, Bethlehem Steel Corporation, Bethlehem, Pa. 18016 Anal. Chem., 43, 178 (1971) Theory of Heatburst Calorimetry A mathematical theory has been developed to explain the principle of heatburst calorimetry. This theory can be used for the design of new heatburst calorimeters and for the im­ provement of the performance of those already in operation. F. H. VERHOFF, Department of Chemical Engineering, University of Notre Dame, Notre Dame, Ind. 46556 Anal. Chem., 43, 183 (1971)

Anal. Chem., 43, 206

(1971)

Carbon Rod Atomizer in Atomic Absorption and Fluorescence Spectrometry and Its Clinical Application A new carbon rod atomizer which may be used together with a diffusion flame, has been constructed and evaluated for several elements. Its application to lead analysis in blood and urine is described. M. D. AMOS, P. A. BENNETT, K. G. BRODIE, P. W. Y. LUNG, and J. P. MATOUSEK, Varian Techtron Pty. Ltd., North Springvale, Melbourne, Victoria, Australia Anal. Chem., 43, 211

(1971)

Some Analytical Characteristics of Organic Liquid Fuel Flames in Atomic Absorption Spectrometry

Flame Emission Spectrometric Determination of Aluminum, Cobalt, Chromium, Copper, Manganese, Niobium, and Vanadium in Low and High Alloy Steels A flame emission spectrometric procedure for the determina­ tion of Al Co, Cr, Cu, Mn, Ni, and V in low and high alloy steels without prior separation of the iron is presented.

Atomic absorption measurements using organic liquid fuel flames show greater sensitivity for most of the metals ex­ amined than is obtained using the conventional air/acety­ lene flame. Sensitivity date is reported for Cu, Pe, Ag, P b , Mn, Zn, and Ca.

VELMER A. FASSEL, ROBERT W. SLACK, and RICHARD N. KNISELEY, Institute for Atomic Research and Department of Chemistry, Iowa State University, Ames, Iowa 50010

B. W. BAILEY and J. M. RANKIN, Division of Laboratories and Research, New York State Department of Health, New Scotland Avenue, Albany, Ν. Υ. 12201

Anal. Chem., 43, 186 (1971)

Anal. Chem., 43, 216 (1971)

ANALYTICAL CHEMISTRY, VOL. 43, NO. 2, FEBRUARY 1971

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Some Physical Characteristics of Flames Produced from Organic Liquid Fuels

Atomization of Suspensions in Atomic Absorption Spectrometry

Investigation of physical properties of organic liquid fuel flames show them to be cooler, slower burning, and much lower in background radiation than those flames commonly employed in flame spectrometry.

The atomization of stannic oxide, stannic sulfide, and stannous oxide suspensions was compared to the atomiza­ tion of stannic tin in solution. W. W. HARRISON and P. O. JULIANO, Department of Chemistry, University of Virginia, Charlottesville, Va. 22901

B. W. BAILEY and J. M. RANKIN, Division of Laboratories and Research, New York State Department of Health, New Scotland Avenue, Albany, Ν. Υ. 12201

Anal. Chem., 43, 248 (1971)

Anal. Chem., 43, 219 (1971) High Sensitivity Internal Reflection Spectroelectrochemistry for Direct Monitoring of Diffusing Species Using Signal Averaging

Automated Thermoanalytical Techniques: An Automated Thermobalance

The variables which influence the sensitivity to optically monitoring a light absorbing species by internal reflection spectrometry at optically transparent electrodes are ex­ amined and evaluated.

This paper described an automated thermobalance which is capable of recording the T G curves of eight samples in a sequential manner. Operation of the thermobalance is com­ pletely automatic and requires no operator attention once started. W. S. BRADLEY and W. W. WENDLANDT, Thermochemistry Laboratory, Department of Chemistry, University of Hous­ ton, Houston, Texas 77004 Anal. Chem., 43, 223 (1971)

NICHOLAS WINOGRAD and THEODORE KUWANA, Depart­ ment of Chemistry, Case Western Reserve University, Cleveland, Ohio 44106 Anal. Chem., 43, 252 (1971)

Notes Alternating Current Polarographic Method of Analysis in the Presence of Oxygen and Other Irreversibly Reduced Species

Phase Solubility Analysis: Alteration of a Sample in Situ to Avoid Solid Solution Phase solubility analysis fails when the impurities form solid solutions with the major component. A case is de­ scribed where this is circumvented by converting the com­ pound to a salt during the analysis.

Influence of irreversible electrode processes on the analytical applications of ac polarography has been investigated and shown to be critical even though they themselves do not produce sensitive ac waves. A. M. BOND and J. H. CANTERFORD, Department of In­ organic Chemistry, University of Melbourne, Parkville, Victoria 3052, Australia Anal. Chem., 43, 228 (1971)

GEORGE V. DOWNING, Jr., GEORGE B. SMITH, and ALAN B. WHITE, Merck Sharp & Dohme Research Laboratories, Rahway, N. J. 07065 Anal. Chem., 43, 260 (1971)

Determination of Trace Quantities of Aluminum and Chromium in Uranium by Gas Phase Chromatography

Spectrophotometric Determination and Spectrophotometric Titration of Palladium. for the Pd(ll)-Nitroso R Complex

The reported method, combining solvent extraction and gas phase chromatography, makes possible the quantitative de­ termination of aluminum and chromium in uranium for con­ centrations as low as 0.1 ppm.

Two spectrophotometric methods have been developed for determination of palladium employing nitroso R. Formula for the Pd(II)-nitroso R complex was determined by solu­ tion studies and analysis of its sodium derivative.

CLAUDE GENTY, COLETTE HOUIN, PIERRE MALHERBE, and ROGER SCHOTT, Commissariat a l'Energie Atomique, Centre d'Etudes de Bruyeres-le-Chatel, Boite Postale 61, 92 Montrouge, France Anal. Chem., 43, 235 (1971)

ORVILLE W. ROLLINS and MORRIS M. OLDHAM, Depart­ ment of Chemistry, U. S. Naval Academy, Annapolis, Md. 21402 Anal. Chem., 43, 262 (1971)

Formula

Structure Elucidation of Aliphatic Aldehydes by Mass Spectrometry of Alkenyl Ethers

Study of High Explosives by Optical Thermal Analysis In this work an automatic thermomicroscopy method was used to study the polymorphic transitions of several high explosives. The transition temperatures for dipentaerythritol-hexanitrate, tripentaerythritol-octanitrate, and tetrapentaerythritol-decanitratc are reported.

This study was initiated to simplify the structure deter­ mination of oeirt-substituted aldehydes by mass spec­ trometry. The results showed that the mass of beta-substituents was demonstrated clearly by studying mass spectra of alk-1-cnyl methyl ethers derived from the aldehydes.

BILLY D. FAUBION, Mason and Hanger—S//as Mason Co., Inc., Pantex Plant, P. 0. Box 647, Amarillo, Texas 79105

P. E. MANNI, WILLIAM G. ANDRUS, and JACK N. WELLS, Department of Medicinal Chemistry and Pharmacognosy, School of Pharmacy and Pharmacal Sciences, Purdue University, Lafayette, Ind. 47907

Anal. Chem., 43, 241 (1971)

Anal. Chem., 43, 265 (1971)

ANALYTICAL CHEMISTRY, VOL. 43, NO. 2, FEBRUARY 1971

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Aflatoxin Detection by Thin-Layer ChromatographyMass Spectrometry

Lead Sulfide-lmpregnated Silicone Rubber Membranes as Selective Electrodes for Lead Ion

Mass spectral analysis in combination with thin-layer chromatography provides definitive evidence for the pres­ ence of carcinogenic aflatoxin compounds in agricultural commodities at levels of several ppb.

The potential response of PbS-impregnated silicone rubber membranes have shown that they are very useful as lead ion selective electrodes. The soaking effect before the measure­ ment, is investigated.

W. F. HADDON, MABRY WILEY, and A. C. WAISS, Jr., Western Regional Research Laboratory, Agricultural Re­ search Service, U. S. Department of Agriculture, Albany, Calif. 94710

HIROSHI HIRATA and KENJI DATE, Wireless Research Laboratory, Matsushita Electric Industrial Co., Ltd., Kadoma, Osaka, Japan Anal. Chem., 43, 279 (1971)

Anal. Chem., 43, 268 (1971) Rapid Method for Determination of Boron in Biological Materials A method for the determination of 1-5 fig of Β with a 1015% accuracy in 20—500 mg of tissue within 3 hours is de­ scribed.

Photometric Titration of Selenium(IV) with Permanganate in Sulfuric Acid Using Condensed Phosphoric Acid as Accelerator

ALEXANDER KACZMARCZYK, Department of Chemistry, Tufts University, Medford, Mass. 02155, and JANETTE R. MESSER and CYNTHIA E. PEIRCE, Neurosurgical Service, Massachusetts General Hospital, Boston, Mass. 02114

This work deals with a study of the conditions under which a direct titration of selenium(IV) could be made. P. P. NAIDU and G. G. RAO, Department Andhra University, Waltair (A.P.) India

Anal. Chem., 43, 271 (1971)

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Chemistry,

Anal. Chem., 43, 281 (1971)

Separation of Galium from Group III Elements, Germanium, Copper, Arsenic, and Iron Methyl ethyl ketone has been used for the quantitative ex­ traction of gallium from a 2M HC1, 1M NH.C1, \M H.-SO,, and ΪΜ (NHOaSCh water solution in the presence of Al, In, T l ( I I I ) , Se, Y. La, E u ( I I I ) , Tm, Dy, Ge(IV), C u ( I I ) , As(III),andFc(in). R. RAFAELOFF, Soreq Nuclear Research Centre, Yavne, Israel Anal. Chem., 43, 272 (1971)

Enzyme Electrode for Amygdalin G. A. RECHNITZ and RAMON LLENADO, Dept, of Chemis­ try, State University of New York at Buffalo, Buffalo, Ν. Υ. 14214

Quantitative Determination of Water in a Hydrophilic Macromolecular Sample (Dextran) by Gas Chromatography A gas chromatographic tative determination of ciently volatile to pass method was developed illustrale the technique.

Correspondence

Anal. Chem., 43, 283 (1971)

method is described for the quanti­ water in samples that are not suffi­ through a gas chromatograph. The using a polysaccharide sample to

WALLACE M. PASIKA and ARTHUR C. WEST III, Chemistry Department, Texas A&M University, College Station, Texas 77843 Anal. Chem., 43, 275 (1971)

Analysis of Mixtures of Hydrogen Peroxide and Formaldehyde R. A. GORSE and D. H. VOLMAN, Department of Chemis­ try, University of California, Davis, Calif. 95616 Anal. Chem., 43, 284 (.1971)

Determination of Trace Amounts of Inorganic Chloride in Glycols and Water-Soluble Alcohols A spectrophotometric procedure using mercuric thioeyanate and ferric iron lias been applied to determine trace amounts of inorganic chloride in glycols and water-soluble alcohols. The absorbanee of the reagent blank is regulated to a threshold value with mercuric acetate or hydrochloric acid to obtain maximum sensitivity and accuracy. ROLAND P. MARQUARDT, The Dow Chemical Company, Midland, Mich. 48640 Anal. Chem., 43, 277 (1971)

Fluorescence of 8-Quinolinol in Strongly Basic Solutions. A Defense of the Excited State Prototropic Equilibrium Hypothesis S. G. SCHULMAN, Department of Pharmaceutical Chem­ istry, College of Pharmacy, University of Florida, Gaines­ ville, Fla. 32601 Anal. Chem., 43, 285 (1971)

ANALYTICAL CHEMISTRY, VOL. 43, NO. 2, FEBRUARY 1971

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A C BRIEFS Role of Solvating Agents in Promoting Ion Pair Extraction T A K E R U HIGUCHI, ARTHUR MICHAEUS, and J. HOWARD RYTTING, Department o f Analytical Pharmaceutical Chem­ istry and Pharmaceutics, The University of Kansas, Law­ rence, Kan. 66044 Anal. Chem.,

43, 287

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(1971)

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(1971)

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ANALYTICAL CHEMISTRY, VOL. 43, NO. 2, FEBRUARY 1971 .

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