analytical chemistry - American Chemical Society

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CONTENTS

ANALYTICAL CHEMISTRY

EDITORIAL ANALYST'S C O L U M N .

867 .

.

NEWS

READERS'

INFORMATION

SERVICE ANALYST'S CALENDAR

.

39 A

20 A NEW PRODUCTS

20 A

42 A

MANUFACTURERS'

LABORATORY OF THE MONTH

33 A

R. H. Müller

11 A 19 A

1

NEW BOOKS Volume 2 7 , N o . 6

INSTRUMENTATION .

29 A

LITERATURE

51 A

Issued June 1 0 , 1 9 5 5 CopyrigKl 1 9 5 5 by the American Chemical Society

EDITOR: WALTER J. MURPHY Executive Editor: JAMES M. CROWE Science Editor: LAWRENCE T. HALLETT Production Manager: JOSEPH H. KUNEY Associate Editors Robert G. Gibbs Stella Anderson, G. Gladys Gordon, Bertha Reynolds, Charlotte C. Sayre, Ruth Cornette Assistant Editor Katherine I. Biggs Editorial Assistants Betty V . Kieffer, Sue Jones, Ruth C. Laubach, Veronica O'Keefe, Fern S. Jackson, Ruth M . Howorth, Lois J. Bennett Contributing Editor R. H. Müller Advisory Board H . F. Beeghly, G. E. Boyd, A . Q . Butler, Harvey Diehl, N. H. Furman, W. W. Hilty, D. N. Hume, Robert Kunin, S. S. Kurtz, Jr., H. A . Liebhafsky, J. J. Lingane, O . D. Shreve, V . A . Stenger, P. W. West, J. H. Yoe

Scientific and Technical Articles MassSpectrometric Analysis of High Molecular Weight, Saturated Hydrocarbons R. J . Clerc, Archie H o o d , and M . J . O ' N e a l , Jr.

868

Analysis of Fluorinated Polyphenyls by Mass Spectrometer Paul Bradt and F. L. Mohler

875

Direct Spectrophotometry Determination of Uranium in Aqueous Solutions R. G . Canning and P. Dixon

877

Emission Spectrochemical Analysis of Vanadium and Iron in Titanium Tetrachloride H. V . Malmstadt and R. G. Scholz

881

Identification of Frozen Liquid Samples with X-Ray Diffractometer. H . N . Smith and H . H . Heady

883

Quantitative X-Ray Determination of Amorphous Phase in Wood Pulps as Related to Physical and Chemical Properties G . L.Clark and H. C. Terford

888

New Polarographic Electrode Employing Controlled Stirring Paul Arthur, J . C. Komyathy, R. F. Maness, and H. W . Vaughan

895

Polarographic Determination of Nitroglycerin in Double-Base Powder G . C. Whitnack, M . M . MayField, and E. St. C. Gantz

899

Polarographic Determination of Traces of Copper, Nickel, Cobalt, Zinc, and Cadmium in Rocks . . . L. E. Smythe and Β. Μ . Gatehouse

901

Polarographic Determination of Palladium R. F. Wilson and R. C. Daniels

904

Polarogrephy with Platinum Microelectrodes in Fused Salts E. D. Black and Thomas De Vries

906

Flame Photometric Determination of Calcium in Sea Water and Marine Organisms T. J . C h o w and T. G . Thompson

910

Flame Photometric Determination of Strontium in Portland Cement J . J . Diamond

913

Chronometric Method of Determining Polyphenol Oxidase Activity L. L. Ingraham and Benjamin Makower

916 918

Determination of Small and Large Amounts of Fluorine in Rocks F. S. Grimaldi, Blanch Ingram, and Frank Cuttitta

921

Absolute Assay of Beta Radioactivity in Thick Solids A . D. Suttle, Jr., and W. F. Libby Chromatography of Organic Acids in Cured Tobacco F. E. Resnik, L A . Lee, and W . A . Powell

•

9S8 931

Determination of Uranium in Uranium Concentrates R. J . Guest and J . B. Zimmerman

936

Radioisotopic Study of Uranium Separations H . P. Raaen and P. F. Thomason

944 Determination of Hydrocortisone C. R. Szalkowski, M . G. O'Brien, and W . J. Mader 947

This Month's Cover.

An a t -

tractive exterior, dictated by its location in Kansas City's cultural center, belies the "ultimate in utility" which is the keynote of Midwest Research Institute's new $1.25 million laboratory. A basic requirement of keeping costs down to $15 a square foot presented a challenge, as normal costs run from $25 to $40. Some of the means by which this goal was attained without sacrificing basic needs are set forth on page 29 A. M R I ' s basic objectives, those of developing a better balance between industry and agriculture in the Midwest and methods of processing locally produced raw materials, have been followed since M R I started operating 10 years ago in four rented rooms with a few scientists.

Separation and Determination of Thorium and Aluminum C V . Banks and R. E. Edwards 949 Determination of Total Sulfur Content of Sedimentary Rocks by Combustion Method . M . E. Coller and R. K. Leininger 951 Test for Vicinal Dithiol Group D. H . Rosenblatt and G . N . Jean

954

Quantitative Elution of Morphine from Ion Exchange Resins C. H . Van Etten

957

Test for Establishing Residual Safe Life of Stabilized Solid Propellents Carl Boyars and W . G. Gough

961

Fluorimetric Determinations of Aluminum and Gallium in Mixtures of Their Oxinates J. W . Collât and L. B. Rogers Adsorption-Dialysis, Extraction Technique I. R. Hunter, D. F. Houston, and E. B. Kester Improved Plastometer for Studying Agglutinating Behavior of Caking Coals G. L. Barthauer One-Phase Solvent Mixtures for Separation of Amino Acids T. L. Hardy, D. O . Holland, and J . H . C. Nayler Continued on page 4 A

965 969

. . . . 971

Three Great Waco MAGNETIC STIRRERS

the

JUMBO

Five gallon bottles or 1 2 inch jars can be sup­ ported easily on this 11 " diameter 8 " high stirrer. By f a r , the most powerful magnetic stirrer . . . used for agitating large volumes in closed systems, under vacuum or pressure, for stirring through heating mantles and for viscous solutions. W A C O J U M B O M A G N E T I C STIRRER. Complete w i t h 2 teflon-covered stirrer bars, one %" χ l 3 ^ f f , a n a one %" x lY%. F o r 115 volts, 5-60 cycle AC. $69.50 each.

the Standard Convenient round shape, 6 " diameter, only AVi" high for agitating liquids in closed or open systems, under vacuum or pressure. W A C O S T A N D A R D M A G N E T I C STIRRER. Complete w i t h t w o teflon coated stirring bars, JHi* x %" and % χ 1 } ^ * , m o u n t i n g r o d . F o r 115 volts 5 0 / 6 0 cycles A C . Each $28.50

the Junior Titration stirrer is only 3 V 4 " diameter χ 3 " high . . . ideal size for all titration assemblies. Ideal for micro and semi-micro systems. WACO J U N I O R T I T R A T I O N STIRRER. Complete w i t h monel cased magnetic stirrer w i t h %" plastic m o u n t i n g r o d , teflon b a r "A " ι % ". Each $30.00.

CONTENTS, continued Twenty-Stage Molecular Distillation Unit F. W . Melpolder, T. A . Washall, end J . A . Alexander

974

Determination of Traces of Nickel and Zinc in Copper and Its Salts Louis Meites

977

Microscopic Fusion Study of 2,4,5-Trichlorophenoxyacetic Acid and Related Compounds C. J . Arceneaux

979

Mierodetermination of Chromium in Small Samples of Various Biological Media *C. H . Grogan, H. J . Cahnmann, and Elizabeth Lethco

983

Determination of Organic Sulfur in Nonvolatile Materials by Rapid Open-Tube Oxidation E. W . McChesney and W. F. Banks, Jr.

987

Distillation Micromethods for Analysis of Petroleum A . R. Javes, Christian Liddell. and W . H. Thomas

991

Quantitative Determination of Certain Sulfenyl Haiides Norman Kharasch and Μ . Μ . Wald

996

Volumetric Determination of Fluorine Involving Distillation from Sulfuric Acid Solution O . D. Smith and T. D. Parks

998

Spectrophotometry Technique for Calcium Leonard Aconsky and Motoko Mori

1001

Determination of Thorium by Fluorescent X-Ray Spectrometry Isidore Adler and J . M . Axelrod

1002

Determination of Organic Nitrogen by Kjeldahl Method without Distillation C. t. Adams and G . H . Spaulding

1003

Application of Zero Grid Current Vacuum Tube Voltmeter to Measurement of pH with Glass Electrode 1004 Samuel Natelson Rapid Determination of Perch I orates N . L. Crump and N . C. Johnson

1007

Rapid Polarographic Determination of Tetraethyllead in Gasoline Walter Hubis and R. O . Clark

1009

Quantitative Spectrographic Analysis of Rare Earth Elements V . A . Fasse!, Beverly Quinney, L. C. Krotz , and C. F. Lentz

1010

Method for Direct Col or i metric Determination of Oxalic Acid Julio Bergerman and J. S. Elliot

1014

Microscopic Identification of Microgram Quantities of D-Fructose L M . W h i t e and G . E. Secor

1016

Continuous Determination of Oxygen in Gases J. T. Corcoran

1018

Colorimetric Determination of N-Phcnyl-1-naphthylamine in New and Used Oils W. S. Levine and W . A . Marshall

1019

Polarographic Determination of Lead in Beryllium R. W . Bane

1022

Determination of Acetylenic Hydrogen by Means of Concentrated Silver Solutions Lucien Barnes, Jr., and L. J . Molintni

1025

Infrared Characterization of Side-Chain Substitution of Monoalkyl Benzenes W. J . Potts, Jr.

1027

Anomalous Behavior of Certain Tetraalkylbibenzyls in Zeisel Methoxy Determination R. L. Huang and Lee Kum-Tatt

1030

Performance of Interference Filters in Simple Flame Photometer W . G . Schrenk and B. L. Gendening

1031

Corrections W A C O S W I N G ARM AS­ SEMBLY. Permits swinging stirrer aside for SPEEDY re­ moval of beaker. With porcelain base support.

CRYSTALLOGRAPHY

986,1024 DATA

Triphenylacetic Acid O . W . Adams and W . C. McCrone

1033

MEETING REPORTS

Each $ 1 5 . 5 0

SATISFACTION

Air Pollution Symposium

1034

Society for Analytical Chemistry

1035

AIDS FOR THE A N A L Y S T

GUARANTEED ORDER T O D A Y

New Ceramic Buckboard and Muller Harold Bloom and P. R. Barnett

1037

Write for

Graphite-and Aluminum-Block Solution Evaporators C. D. Susano

1038

complete IMagnetic Stirrer Bulletin A C - 6

Laboratory Supplies and Equipment

WILKENS-ANDERSON CO. 4525 W . Division St.

Chicago 5 1 , III

Circle No. 4 A an Readers' Service Card, page 39 A

4A

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ANALYTICAL

CHEMISTRY