ANALYTICAL CHEMISTRY Volume 24, N o . 8 Issued August 19, 1952 Copyright 1952 by American Chemical Society
EDITOR WALTER J.
James M. Crowe
Gordon
Anderson
Charlotte C. Sayre Assistant
Editors
Katherine I. Biggs Ruth Cornette Gertrude Editorial
McMurray Assistants
M a r y R. Carls Betty V. Kieffer Doris L. Krout Sue Peter Violet Rivlin Contributing
Theory of Chemical Analysis by High-Frequency Methods W . J . Blaedel, H . V . Malmstadt, D. L. Petitjean, and W . K. Anderson
1240
Practical High-Frequency Titration Apparatus for General Laboratory Use J . L. Hall
1244
. . . .
Titration of Sulfates with A i d of High-Frequency Oscillator O . I. M i l n e r
1247
Determination of Water in A l c o h o l s b y Means of High-Frequency Oscillators P. W . West, Paschoal Senise, and T. S. Burkhalter
. .
1250
Infrared Spectra and Characteristic Frequencies of Inorganic Ions F. A . M i l l e r and C. H . Wilkins
1253
Spectrophotometric Determination of O n e Component in Two-Component Mixture Eugene A l l e n and Ε. Μ . Hammaker
1295
Chemical Analysis and Isotopic Assay of Organic Compounds R. C. Anderson, Yvette Delabarre, and A . A . Bothner-By
1298
A c t i v i t y of Silica-Alumina Cracking Catalysts C. J . Plank
1304
Investigation and A p p l i c a t i o n of Zinc-1,10-Phenanthroline Complexes J . M . Kruse and W . W . Brandt
1306
Identification of M a l o n y l Urea Derivatives C. J . Umberger and Grace Adams
1309
Solubility and Freezing Point Depression of Nitrous O x i d e in L i q u i d Nitrogen Dioxide A . W . Rocker
1322
Colorimetric M e t h o d for Estimation of Digitoxin E. L. Pratt
1 324
Classifying Butyl Rubber with Respect to Modulus L. L. Currie
1 327
Editor
R. H. Müller Advisory
1236
Reynolds
G. Gladys Stella
High-Frequency Titration J . l . Hall
Editors
Lawrence T. Hallett Bertha
1235
MURPHY
Executive Editor
Associate
EDITORIALS
Board
S. E. Q . Ashley P. J. Elving N. H. Furman D. M . Hume
Dissociation Temperatures of Urea Complexes of Long-Chain Fatty A c i d s , Esters, and A l c o h o l s 1331 H . B. Knight, L. P. Witnauer, J . E. Coleman, W . R. N o b l e , Jr., and Daniel Swern Streak Reagents for Chromatography A . L. LeRosen, R. T. Moravek, and J . K. Carlton
1335
W . A. Kirklin S. S. Kurtz, Jr. H. A. Laitinen Gordon
MacKinney
C. J. Rodden J. W . Stillman Grant Edward
MICROCHEMISTRy Detection and Estimation of Steroidal Sapogenins in Plant Tissue M . E. W a l l , C. R. Eddy, M . L. McClennan, and M . E. Klumpp
1 337
Mlcrodetermination of Chromium in Blood H . J . Cahnmann and Ruth Bisen
1 341
Chloric A c i d M e t h o d for Determination of Protein-Bound Iodine Bennie Zak, H . H . W i l l a r d , G . B. Myers, and A . J . Boyle
1345
Wernimont Wichers
Progress Report of Committee on Nomenclature, Division of A n a y t i c a l Chemistry, This M o n t h ' s Cover: Although infrared spectroscopy has been widely applied to the analysis of covalent materials, there is at present relatively little published information on its application to inorganic salts. Foil A. Miller and Charles H. Wilkins of Mellon Institute have been engaged over the past two years in surveying the infrared spectra of a wide variety of such salts in an effort to assess the potential value of this technique. By examining over 150 compounds, they have been able to find characteristic frequencies for 33 polyatomic ions. A combination of emission analysis, infrared examination, and x-ray diffraction is especially fruitful for the qualitative analysis of inorganic solids. The results are described on page 1253·
A M E R I C A N C H E M I C A L SOCIETY June 1952
1348
S. E. Q . Ashley et a i . Suggested Nomenclature in A p p l i e d Spectroscopy H . K. Hughes et a/. NOTES O N A N A L Y T I C A L
1 349
PROCEDURES
Volumetric Determination of Hypophosphate Ion Therald M o e l l e r a n d G . H . Q u i n t y
1 354
Determination of Organic Peroxides E. W . Abrahamson and Henry Linschitz
1 355
Conversion of Hydrogenic Materials to Hydrogen for Isotopic Analysis . . . . Jacob Bigeleisen, M . L. Perlman, and H . C. Prosser
1356
Estimation of Pyrethrins on Coated Paper Bags F. I. Edwards and Cipriano Cueto
1357 (Continued
on page 4 A)
ANALYTICAL
4A
CONTENTS,
Moisture in Minutes!
CHEMISTRY
continued
NOTES, Contd. A n A n o m a l y in Zeisel M e t h o x y Determination R. L. Huang and Francis Morsingh
1359
Volumetric Determination of Hydroxylamine with Ceric Sulfate S. R. Cooper and J . B. Morris
1 360
Isotopic M e t h o d for Direct Determination of O x y g e n in Fluorocarbon Derivatives A . D. Kirshenbaum, A . G . Streng, and A . V . Grosse
1361
Rapid Analysis of Viscose Coagulating Liquor Using Schwarzenbach M e t h o d Keihei Ueno
1 363
Polarographic Study of Inosose D. H . Couch and Ward Pigman
1 364
END POINT TITRATOR
Separation of Vanillic and Protocatechuic A c i d s by Chromatography I. A . Pearl and D. L. Beyer
1 366
MOISTURE d e t e r m i n a t i o n s are m a d e in a f e w MINUTES using the W A C O . The K a r l Fischer R e a g e n t m e t h o d is a CHEMICAL technic f o r t h e d e t e r m i n a t i o n o f w a t e r content . . . . e l i m i n a t i n g oven drying!
Colorimetric Determination of A m i d e s as Hydroxamic A c i d s Felix Bergmann
1367
Amperometric Determination of Fluoride C. R. Castor and J . H . Saylor
1 369
Benzidine Reagent in Paper Chromatography H o w a r d M i l l e r and D. M . Kraemer
1 371
Microdetermination of Phosphorus G. R. Nakamura
1372
Wide range is i n d i c a t e d
Determination of Hexaphenylethane G. S. Hammond, Abraham Rawe, and F. J. M o d i c
1 373
by partial list of users
Polarographic Determination of Iron in Nonferrous A l l o y s Louis Meites
1374
Determination of Iron in Water in Presence of Heavy Metals R. L. Morris
1376
WACO
Dead Stop
American Cyanimid (2) The Dow Chemi cal Co. Standard Oil Co. (14) E. I. du Ponl de Nemours Lever Bros. (2) Cannon Mills Pabst Brewing Co. Crown Can Co. Schweitzer Paper Co. C o r n Products Refg. (2) Bristol-Meyers Co. U. S. Naval Pow der Chemical Special ties U. S. Dept. of Agric. (3) Phoenix Chem. Lab. McGill Univ. Washington Univ. Ohio State Univ. (2) Michigan State Univ. N. C. State Univ. Celanese Corp. (2) Nuodex Products Co.
Analytical Section of International Union of Pure and A p p l i e d Chemistry Congress of Practical Polarography CRySTALLOGRAPHIC
1378
R. L. Clark and John Krc, Jr. B O O K REVIEWS
1379
ANALYST'S CALENDAR
1381
A I D S FOR THE A N A L Y S T Shaft Seal for Vacuum Apparatus D. J . Trevoy and W . A . Torpey Directional Cold-Finger Condenser D. J . Trevoy
1 382
Simple Peak Current Recorder for Pen Recording Polarograph Β. Ε. G o r d o n
1383
M e t h o d of A d d i n g Sample to Closed Systems M . J . Bergin and A . H . A . Heyn
1 383
Stability Tube with Foam Breaker G. S. Fisher and N . J. Morris Simple Flask for Titrations under Inert Atmosphere J . L. Myers and Percy Fainer THE A N A L Y S T ' S C O L U M N INSTRUMENTATION
1 384
1382
1 384 9 A 15 A
R. H . M u l l e r
Write for Bibliography and Bulletin AC8 SUPPLIES
1380 1 331
DATA
L 3 -Threonine (Threo-a-amino-/3-hydroxy-n-butyric A c i d )
O N L Y t h e W A C O shows a s h a r p a n d reproducible end point . . . the needle of the microammeter d r o p s across t h e e n t i r e scale a t t h e e n d p o i n t . Technic is s i m p l e a n d electronic a m p l i f i c a t i o n is n o t necessary. It is a s t u r d y equipment and costs but $180.00.
ΙΑΒ0ΡΛΤΟΒ-.
. . . .
AND
CHEMICALS
WILKENS ANDERSON CO. Γ4Μ5 W . O I V I S I O N / ^ % CHICAGO SI,ILL m ^ H
I
N E W PRODUCTS
19 A
M A N U F A C T U R E R S ' LITERATURE
22 A
The American Chemical Society assumes no responsibility for the statements and opinions advanced by contribu tors to its publications. Views expressed in the editorials are those of the editors and do not necessarily represent the official position of the American Chemical Society. Published by the American Chemical Society, from 20th and Northampton Sts., Easton, Pa. Executive Offices, Editorial Headquarters, and Circulation Department, 1155 Six teenth St., N.W., Washington 6, D. C. Advertising Office: 330 West 42nd St., New York 18, Ν. Υ. Branch Editorial Offices: Chicago 1, III., 86 East Randolph St.; Houston 2, Tex., 623 West Bldg.; New York 17, Ν. Y., 60 East 42nd St.,- San Francisco 2, Calif., 760 Market St.; London, Bush House, Aldwych. Entered as secondclass matter at the Post Office at Easton, Pa., U.S.A., February 18, 1948, under the Act of March 3, 1879, as 12 times a year monthly on the 15th. Acceptance for mailing at special rate of postage provided for in Section 1103, Act of Oct. 3, 1917, authorized July 13, 1918. Annual subscriptions: members $3.50, nonmembers $4.00. Postage to countries not in the Pan-American Union $1.20. Canadian postage $0.35. Combination rate for Analytical Chemistry and Industrial and Engineering Chemistry: members $7.00, nonmembers $8.00. Postage for the combination: countries not in the Pan-American Union $3.90, Canadian postage $1.10. Single copies: current issues, members $0.40, nonmembers $0.50; back numbers, prices on request, special rates to members. Claims for missing numbers w i l l not be allowed if received more than 60 days from date of mailing plus time normally re quired for postal delivery of journal and claim. No claims allowed from subscribers in Central Europe, Asia. or the Pacific islands other than Hawaii, or because of failure to notify the Circulation Department of a change of address, or because copy is "missing from files.*' C H A N G E OF ADDRESS: Notify Circulation Department, American Chemical Society, 1155 Sixteenth St., N.W., Washington 6, D. C. Such notification should include both old and new addresses and postal zone number, if any. The American Chemical Society also publishes: Chemical and Engineering News, Industrial and Engineering Chemistry, Chemical Abstracts, Journal of the American Chemical Society, and the Journal of Physical Chemistry. Rates on request.