CONTENTS
ANALYTICAL CHEMISTRY
EDITORIALS ANALYST'S C O L U M N .
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.
NEWS
19 A
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. . . . . . ' .
45 A
51 A
34 A
NEW PRODUCTS
54 A
41 A
MANUFACTURERSLITERATURE
63 A
32 A
LABORATORY OF THE MONTH
INSTRUMENTATION . . . . R. H. Muller READERS" INFORMATION SERVICE
28 A
A N A L Y S T S CALENDAR NEW BOOKS
Volume 2 7 , No. 5
691
Issued M a y 2 3 , 1 9 5 5 Copyright 1 9 5 5 by the American Chemical Society
Scientific and Technical Articles Symposium on Analytical Methods and Instrumentation in Air Pollution Introduction Morris Katz
EDITOR: WALTER J. MURPHY Executive Editor: JAMES M. CROWE Science Editor: LAWRENCE T. H A L L E H 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
692
Light-Scattering Studies in Aerosols with New Counter-Photometer C. T. O'Konski and G . J . Doyle
694
Microdetermination of Sulfuric Acid Aerosol E. R. Gerhard and H . F. Johnstone
702
Gas Chamber Microapparatus in Identification of Air-Borne Pollutants J. L. Monkman
704
Instrumental Measurements of Visibility in Air Pollution Studies G. D. Clayton and P. M . Giever
708
Water-Containing Jars and Greased Plates for Dustfall Measurements R. L. Pond and R. R. Paxton
714
Principles of Precision Colorimetry C. N . Reilley and C. M . Crawford
716
Automatic Photometric Titrations of Calcium and Magnesium in Carbonate Rocks Leonard Shapiro and W . W . Brannock
725
Polarographic Determination of Copper, Nickel, Cobalt, Manganese, and Chromium in Titanium Alloys 729 J. J. Mikula and Maurice Codell Elimination of Interferences in Flame Photometry Paul Porter and Garrard Wyld
733
Infrared Evaluation of Sodium Salts of Organic Acids Eugene Childers and G . W . Struthers
737
Automatic Spectrophotometry Titration with Coulometrically Generated Titanous Ion H . V . Malmstadt and C. B. Roberts
741
Determination of Erythromycin by Ultraviolet Spectrophotometry J. B. Tepe and C. V . St. John
744
Use of 50-Cm. Heated Gas Cell in Ultraviolet Spectrophotometry W . F. Hamner, Nina Hadden, and W". M . Padgett II
747
Spectrophotometry Determination of Gluconic Acid and Its Salts L. L A l t
749
Spectrographic Analysis of Briquetted Unashed Plant Material J. H. Muntz and S. W . Melsted
751
Spectrographic Determination of Lead in Oxygen-Free, High-Conductivity Copper S. B. Deal
753
Ultraviolet Determination or Combined Methyl Isopropenyl Ketone in Polymers J. J. Pepe, Irwin Kniel, and Michael Czuha, Jr.
755
Nephelometric Determination of Sulfate Impurity in Certain Reagent-Grade Salts H . J . Keily and L. B. Rogers
759
New Solvent System for Separating Monocarboxylic Acids (C2 to Ge) and Dicarboxylic Acids (C2 to C22) 764 Vladimir Zbinovsky
This Month's Cover.
Automation by that or any other name is a marvel of our age. Actually chemists for some years have used chemical and electronic systems in modern analysis, control, and instrumentation. This month the Fisher Scientific Co. dramatized the opening of its new reagent chemicals plant at Fair Lawn, N. J., by applying a little "automation." As shown on our cover, J . C. Warner, president of Carnegie Tech and President-Elect of the ACS, from his desk in Pittsburgh started an automatic titrimeter. A change in potential actuated a relay starting a vacuum-tube oscillator tied in to a telephone line. The signal started by a chemical reaction set off an 800-cycle audio note in the intercom at Fair Lawn, tripped a relay, and started the automatic filling and labeling of bottles of reagent chemicals.
Isonicotinic Acid Hydrazide as Reagent for Determination of A4-3-Ketosteroids E. J . Umberger
768
Determination of Carbon in Sodium-Potassium Alloy K. G. StoFferand J . H . Phillips
773
Ferricyanide Titration of Cobalt Using Ethylenediamine Harvey Diehl and J . P. Butler
777
1-(2-Pyridylazo)-2-naphthol as Possible Analytical Reagent K. L. Cheng and R. H . Bray
782
Order of Adsorption Affinities of Polynitrostilbenes A . F. Teague, W . A . Gey, and R. W . Van Dolah
785
Detection of Surface-Active Agents Containing Polyoxyethylene or Polyoxypropylene Group · · - · 787 M . J. Rosen Identification of Petroleum Refinery Wastes in Surface Waters A . A . Rosen and F. M . Middleton
790
Simultaneous Determination of Total Carbon and Carbon-14 Activity J. D. Gabourel, M . J . Baker, and C. W . Koch
795
Detection of Unsubstituted Para Position in Phenols Saul Soloway and Angelo Santoro
798
Colorimetric Determination of Sulfate Ion J. L. Lambert, S. K. Yasuda, and M . P. Grotheer
800
Determination of Traces of Sulfur in Organic Compounds J. A . Hudy and R. D. Mair
802
Continued on page 4 A
CONTENTS, continued
NEW!
Color Reaction for Determination of Some Aromatic Nitro Compounds C. C. Porter
805
Specific-Surface Determination of Nitroguanidine by Microscopic and Air-Permeability Methods . . . A . S. Bass and H . M . Sternberg
808
Activation Analysis of Trace Impurities in Silicon Using Scintillation Spectrometry G . H. Morrison and J . F. Cosgrove
810
Optical-Analytical Studies on Steroids A . S. Meyer and M . C. Lindberg
813
Coulometric Determination of Selenium ' Keith Rowley and Ε. Η. Swift
818
Chromatographic Separation and Determination of Porphyrin Methyl Esters D. A . Rappoport, C. R. Calvert, R. K. Loeffler, and J. H . Gast
820
Determination of Microgram and Submicrogram Quantities of Uranium by Neutron Activation Analysis H . A . Mahlman and G . W . Leddicotte
823
Analysis of Automobile Exhaust Gases by Mass Spectrometry J. K.Walker and C . L O ' H a r a
825
Electrostatic Sampler for Dust-Laden Gases G. L. Rounds and H. J . Matoi
829
Two-Step Mixed Indicator for Kiel da h I Nitrogen Titration I. H.Sher
831
Detection of Gallium with Rhodamine Β Hiroshi Onishi
832
Study of Oxidations Using Copper(III) Reagents D. A . Keyworth and K. G. Stone
833
Determination of Zirconium in Magnesium Alloys Using p-Br ο mo- or p-Chloromandelic Acid R. A . Papucci and J . J . Klingenberg
WACO TITRATOR . . . for Karl Fischer MOISTURES At $ 2 1 0 . 7 0 complete, the new W A C O for Karl Fischer moisture determina tions now features NO-DRIP, BALL JOINT Pyrex g l a s s w a r e . . .plus Drain Flask, W A C O magnetic stirrer.. . f o r every application! Hundreds of users of the original W A C O may also modernize as parts are INTERCHANGEABLE!
(No. AN-5653A) New W A C O reservoir with Ball Joint! Capillary outlet and silk-finish grinding provide positive NO-DRIP Feature! Amberized finish avoid deterioration of Fischer Reagent.
. . . .
835
Ammonia Determination and Sample Preparation for Mass Spectrometer by Micro Diffusion Method. . S. W . Mayer, F. H. Kelly, and M . E. Morton
837
Procedure for Determination of Diffusion Coefficients of Gases and Nongaseous Solutes for Membranes S. G . Johnsen and J . E. Kirk
838
Effect of Particle Size on Characteristics of Silicic Acid Chromatographic Adsorbent E. W . Malmberg
840
Improved Acidimétrie Determination of Fluoride J. M . Chilton and A . D. Horton
842
Determination of Impurity with Melting-Temperature Apparatus of Smit L. T. Carleton
845
Assay of lron-55 and Iron-59 in Biological Samples J. H. Rediske, R. F. Palmer, and J . F. Cline
849
Determination of Low Alkalinity or Acidity in Water T. E. Larson and Laurel Henley
851
Correction Factors for Comparing Activities of Different Carbon-14-Labeled Compounds Assayed in Flow Proportional Counter 852 M . L. Karnovsky, J . M . Foster, L. I. Gidez, D. D. Hagerman, C. V . Robinson, A . K. Solomon, and C. A . Villee Qualitative Determination of Amino Acids in Protein Hydrolyzates by Circular Paper Chromatography Irwin Oreskes and Abraham Saifer
854
Quantitative Determination of Glucose and Galactose Hans Fisher, R. G . Hansen, and H. W . Norton
857
Determination of Soluble Ortho-, Pyro-, and Triphosphate in Presence of Each Other L. E. Netherton, A . R. Wreath, and D. N . Bernhart
860
Corrections CRYSTALLOGRAPHY
8 0 9 , 864 DATA
Identification of Organic Bases by Means of Optical Properties of Diliturates (Nitrobarbiturates) B. T. Dewey and E. M . Plein (No. A N - 5 6 5 1 L and A N 5651R) When preliminary ex traction is not required / use T W O bent tip burettes one for Water Methanol and other for Fischer Reagent, also, when standardizing reagents and for DIRECT titration. (No. A N - 5 6 5 8 ) NEW W A C O Drain Flask has a stoppered opening for intro ducing new samples. N e w sample is added through the side opening and procedure repeated, WITHOUT A G A I N titrating to an end point. Drain through lower stop cock. (No. A N - 5 6 6 0 ) Small W A C O Magnetic Stirrer used instead cf the motor and stirring rod. Par ticularly convenient when using the Drain Flask set-up. May be ordered separately for your present assembly. WRITE FOR New WACO Titretor bulletin AN-5 and new Directions, based on trie latest technics! Laboratory Supplies a n d Equipment
WILKENS-ANDERSON CO.
Circle No. 4 A on Readers' Service Card, page 51 A
4A
· .
862
MEETING REPORT Microchemical Symposium
864
AIDS FOR THE A N A L Y S T Automatic Cut-Off Valve for fon Exchange Columns C. A . Hewitt
865
Plastic Dry Box A . J . Franklin and S. E. Voltz
865
Stable Starch Solutions for lodometry A . C. Holler
866
G U I D E FOR A U T H O R S , published in December 1954 issue, page 2032, gives copy requirements w h i c h should be observed in preparing manuscripts for editorial consideration. Manuscript ( 2 copies) should be submitted t o t h e E d i t o r , 1155 Sixteenth S t . , N . W . , W a s h i n g t o n 6, D . C. The American Chemical Society assumes n o responsibility for t h e statements and opinions advanced by c o n t r i b u t o r s t o its publications. Views expressed in t h e editorials arc t h o s e of t h e editors and d o n o t necessarily represent t h e official position of the American Chemical Society. Published m o n t h l y by t h e American Chemical Society, from 20th and N o r t h a m p t o n Sts., Easton, Pa. Executive Offices, Editorial H e a d q u a r t e r s , and Circulation D e p a r t m e n t , 1155 Sixteenth St., N . W . , W a s h i n g t o n 6, D . C. Advertising Office: 430 Park A v e . , N e w Y o r k 2 2 , N . Y. Branch Editorial Offices: 86 East R a n d o l p h S t . , Chicago 1, 111.; 623 West B l d g . , H o u s t o n 2 , T e x . ; 2 Park Ave., N e w York 16, N . Y . ; 703 Mechanics' Institute B l d g . , San Francisco 4 , Calif.; Bush H o u s e , A l d w y c h , L o n d o n . Entered as second-class m a t t e r a t t h e Post Office at E a s t o n , P a . , U.S.A., February 1 8 , 1 9 4 8 , under t h e Act of M a r c h 3 , 1 8 7 9 . Annual subscriptions: members $4.00, n o n m e m b c r s $ 5 . 0 0 . Postage t o countries n o t in t h e Pan-American Union $1.20. Canadian p o s t a g e $0.35. Single copies: current issues, $1.00 ( A p r i l , issued in t w o p a r t s , priced a t $2.00). Claims for missing numbers will n o t be allowed if received more t h a n 60 days from date of mailing plus time normally required for postal delivery of journal and claim. N o claims allowed from subscribers in Central E u r o p e , Asia, o r t h e Paci6c Islands o t h e r t h a n H a w a i i , o r because of failure t o notify t h e Circulation D e p a r t m e n t of a change of address, o r because copy is " m i s s i n g from files." C H A N G E O F ADDRESS: Notify Circulation D e p a r t m e n t , American Chemical Society, 1155 Sixteenth St., N . W . , W a s h i n g t o n 6 , D. C. Such notification should include b o t h o l d and n e w addresses and postal zone number, if any. T h e American Chemical Society also publishes : Industrial and Engineering Chemistry t Chemical and Engineering Newt, Chemical Abstractly Journal of the American Chemical Society, Journal of Physical Chemistry, Journal of Agricultural and Food Chemistry, and t h e Journal of Organic Chemistry. Rates on request.
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