New York Meeting's Analytical Program Stresses Techniques

Completely Automated System for the Chemical Determination of Streptomycin and Penicillin ..... Optical Sections, Scientific. Apparatus Makers Associa...
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ANALYTICAL CHEMISTRY A u g u s t

NEWS

1 9 5 7

New York Meeting's Analytical Program Stresses Techniques Four symposia feature thermoanalytical titrimetry, microchemistry, coal research, and gas chromatography i DVANCES in analytical techniques -1 *- will be stressed b y t h e Division of Analytical Chemistry a t t h e 132nd A C S National Meeting in N e w York, Sept. 8 to 13. F o u r symposia a n d a b o u t 50 general papers will provide a diversified program dealing with specialized m e t h ­ ods of separation a n d determination. A one-day Symposium on T h e r m o ­ analytical T i t r i m e t r y will include a round table discussion a n d open forum

on nomenclature. One d a y will also be devoted t o a Symposium in Microchem­ istry. Continually increasing interest in finding new uses for coal products is reflected in t h e S y m p o s i u m on M o d e r n Techniques in Research on Coal a n d Related P r o d u c t s . J o i n t sponsor is t h e Division of G a s a n d Fuel Chemistry. I m p o r t a n c e of t h e techniques of gas c h r o m a t o g r a p h y t o t h e petroleum indus­ t r y is recognized in a symposium spon­

D I V I S I O N OF A N A L Y T I C A L

CHEMISTRY

sored jointly with t h e Division of Petroleum Chemistry. T h e division luncheon will be held on W e d n e s d a y noon, with Victor J . Cabasso speaking on "Problems a n d Prospects of Virus R e s e a r c h . " T h e divisional business meeting will be held on W e d n e s d a y afternoon. General information a b o u t t h e N e w Y o r k meeting appeared in t h e J u n e 17 issue of Chemical and Engineering News.

Analyzer for Acetic Acid in Acetic Anhydride. C. D . LEWIS. Direct Thermometric Methods in Nonaqueous Solutions. L. H. GREATHOUSE.

R. P. CHAPMAN, Chairman WARREN W . BRANDT, Secretary Monday

Monday

Morning

Afternoon

SECTION A GENERAL

SECTION A GENERAL

JOHN H. YOE, Presiding

R. P. CHAPMAN, Presiding Introductory Remarks. R. P . CHAPMAN. Determination of Total T a r Acid Content of T a r Acid Oils bv Use of 2.76-Micron Hydroxyl Band Height. M . F . KRANC, D . J. KADAVY, AND H. M . FASSINGER.

Determination of Long-Chain Sulfonates by Direct Titration with Cetyltrimethylammonium Bromide. Ε . Μ . GINDLER. Completely Automated System for the Chemical Determination of Streptomycin and Penicillin in Fermentation Media. ANDRES F E R R A R I , F . M. R U S S O - A L E S I , AND J. M . K E L L Y .

Separation of a Polyhydric Alcohol Mixture by Nonionic Ex­ clusion.

I. T. CLARK.

Infrared Study of Polynorbornene.

B. A. MONTAGUE, W. L.

T R U E T T , AND D . R. JOHNSON.

Fluorometric Determination of 1- and 2-Naphthol in Mixtures. D . M. H E R C U L E S AND L. B . R O G E R S .

Photometric Determination of Iproniazid and Related Com­

Quantitative Spectrochemical Determination of Barium and Strontium.

R. J. GRABOWSKI AND R. C. U N I C E .

Solution of the Matrix Problem in X - R a y Fluorescent Spectroscopy.

E . J. F E L T E N , J. STEIGMAN, AND I. FANKUCHEN.

Operational Comparison of Four X-Ray Detectors.

P. D.

ZEMANY AND H. A. LIEBHAFSKY.

Determination of Uranium-235 b y Gamma Scintillation Spectrometry.

J. F . COSGROVE AND G. H , MORRISON.

Determination

of Sodium by α-Methoxyphenylacetic

Acid.

WILKINS REEVE.

Separation of Fluoride from Inorganic Compounds by Pyrolysis. R. H. P O W E L L AND OSCAR M E N I S .

Ampcrometric Titration of Traces of Fluoride with Thorium Using a Rotating Palladium Electrode. W. E. HARRIS. Determination of Microgram Quantities of Fluoride by Beryl­ lium-Chrome Azurol S.

L. SILVERMAN AND M . E . SHIDELER.

pounds. R. J . COLARUSSO, MORTON SCHMALL, E . G. WOLLISH, AND E . G. E . SHAFER.

Improved Iodometric Method of Analysis for ieri-Butyl Peresters.

SECTION Β

L. S. SILBBRT AND D A N I E L SWERN.

Nature of Bindschedler's Green and I t s Preparation for Use in Analysis of Hydrazo Compounds. H. J. SHINE, R. L. SNELL, AND J. C. T R I S L E R .

SYMPOSIUM ON THERMOANALYTICAL TITRIMETRY JOSEPH JORDAN, Presiding

SYMPOSIUM ON THERMOANALYTICAL TITRIMETRY DAVID N. HUME, Presiding Introductory Remarks. D . N . H U M E . Thermochcmical Titrations. T. G. ALLEMAN. Enthalpy Titrations Involving Proton Transfer

Processes.

J O S E P H JORDAN AND W. H . DUMBAUGH, J R .

Introductory Remarks.

Instrumental

Aspects

Thermometric Titrations of Lewis Acids.

JOSEPH JORDAN.

of Thermometric

Titrations.

R. H.

MÜLLER.

Use of the Multifunction Thermopile in Thermometric Titrations.

D O R I S C. M Ü L L E R .

Analytical Applications of Thermometric Titrations.

M. P.

Titrimetry

in Continuous

MIR LEIBMANN, J . S. PARSONS, AND J. T . WOODS.

D. N. HUME Analysis. An

Panel. G. W. E W I N G , D A V I D N . H U M E , J O S E P H JORDAN, AND M . G. M E L L O N .

AND H. J. K E I L Y .

Thermoanalytical

Certain Applications of Automatic Thermometric Titrations in Organic Analysis. J. S. PARSONS. Thermometric Titration of 2-Naphthalenesulfonic Acid. WLADIRpund Table Panel Discussion and Open Forum on Nomenclature of Thermoanalytical Titrimetry. Moderator. L. T . HALLETT.

BEN-YAIR.

Thermometric Titrations in Glacial Acetic Acid.

S. T . ZENCHELSKY

AND P . SEGATTO.

VOL. 29, NO. 8, AUGUST 1957

·

25 A

NEWS Microanalytieal Determination of Sulfur in Organic Compounds.

Tuesday Morning

J. F . ALICINO.

Determination of Fluorine. T . S. M A . Applications of Microanalysis in the Petroleum Industry.

SECTION A GENERAL

Perspectives in Quantitative Organic Microanalysis.

Determination of Residual Elements in Iron and Steel by Flame Photometry. PRINCE.

Determination

G. E .

C. W E A R .

WARREN W . BRANDT, Presiding

J. A.

KUCK.

F . V. COGLIANESE, T . L. COLESS, AND L. A.

of Metallic

Impurities

ill Cathode

Nickel.

P. D . GARN AND H . M . GILROY.

Wednesday

Morning

Analytical Program for Processing Aluminum-Uranium Reactor Fuel Elements.

SECTION A GENERAL

R. C. SHANK AND J. E . R E I N .

Analytical Program for Processing Zirconium-Uranium Reactor Fuel Elements.

J. E . R E I N AND R. C. SHANK.

Oxygen Analysis in Titanium Using a Modified Vacuum Fusion Apparatus and Platinum Bath Technique. S. J . BENNETT

RALPH N. ADAMS, Presiding An Ultramicro Direct Setting Thermoregulator.

ROGER G I L -

MONT.

AND L. C. COVINGTON.

Evaluation of the Inert Gas Fusion Method for Rapid Determina­ tion of Oxygen in Steel. J. I. PETERSON, F. A. MELNICK, AND

Ultramicro Electrode Titration Assembly.

E. P . ARTHUR AND

R O G E R GILMONT.

Polarograph with Direct Recording of Cell Voltage.

J. E . S T E E R S , J R .

Analysis of Ultrapure Silicon b y Neutron Activation.

B . A.

Effect of Surface Active Substances on Polarographic Currents.

THOMPSON, Β . Μ . STRAUSE, AND M. B. L E B O E U F .

Determination of Boron in High Purity Silicon Using the Principle of Hydrothermal Refining.

D . T.

SAWYER, R. L. PECSOK, AND Κ. Κ. J E N S E N .

C. L. L U K E AND S. S. FLASCHEN.

R. W. SCHMID AND C. W. R E I L L E Y .

Polarographic Behavior of Iodinated X-Ray Contrast Agents in Buffered Media. GLOTTEN.

PETER

KABASAKALIAN

Oxidations at Mercury Pool Anodes.

SECTION Β

AND JAMES M C -

THEODORE KUWANA AND

R. N . ADAMS.

SYMPOSIUM ON MICROCHEMISTRY

Titration of Iron with Electrolytically Generated Chlorine, Phosphoric Acid, and Copper(II) as Catalysts. P . S. F A R -

K. B. STREETER, Presiding

Coprecipitation in Some Binary Systems of Rare E a r t h Oxa­

Introductory Remarks. Κ. Β. STREETER. Microgram Techniques. A. A. BENEDETTI-PICHLER. Micromanipulations in Nuclear Chemical Research and Other

Luncheon. Division of Analytical Chemistry. Speaker: V I C ­ TOR J. CABASSO. Problems and Prospects of Virus Research.

RINGTON, J. M. D U N H A M , AND W. J . RAMSEY.

Fields.

lates.

A. M. F E I B U S H , K E I T H ROWLEY, AND L O U I S GORDON.

M . CEFOLA, C. J. UMBERGER, AND L. D A L CORTIVO.

Culture Isolation and Purification by the Hanging Droplet Technique.

F . R. SWIFT.

Micromanipulation in Industrial Research.

H. V. WADLOW.

Wednesday

Afternoon

SECTION A GENERAL Tuesday Afternoon

B. J. HEINRICH, Presiding

SECTION A GENERAL

Solvent Extraction of T i n with Tributyl Phosphate.

A. E .

LEVITT AND E. G. BELTRAN.

Ε. Η. SWIFT, Presiding Sodium Hydrogen Diglycolate, New Primary Standard in Acidimetry.

D . A. K E Y W O R T H AND R. B . H A I I N .

M A N N AND J. C. W H I T E .

Hydrolysis Reactions of Thioacetamide in Alkaline Solutions. F . H.

LOHMAN.

D . W. MARGERUM AND J. O. FROHLIGER.

Selective Titrations of Metal Ions with Triethylenetetramine. C. N . R E I L L E Y AND M . V. SHELDON.

Photometric Determination of Aluminum and Titanium in Poly­ ethylene.

Separation of Metal Ions Utilizing 1,10-Phenanthroline Coordi­ nation Kinetics.

E L I O T B U T L E R , D E N N I S P E T E R S , AND Ε . Η. S W I F T .

Spectrophotometric Determination of Carbonyl Oxygen.

Extraction of Chromium with Trioctylphosphine Oxide from Acidic Solutions of Alkali Metal Salts and I t s Determination in Situ as t h e Chrornium-Diphenylcarbazide Complex. C. K.

W. T. BOLLETER.

Determination of Microgram Quantities of Zirconium in Sulfuric Acid Solutions with Pyrocatechol Violet. J. P . YOUNG, J. R. F R E N C H , AND J. C. W H I T E .

Differential Spectrophotometric Determination of ZirconiumHafnium Ratios. F . HOLBROOK.

HARRY F R E U N D , ARNOLD JOHNSON, AND W.

Spectrophotometric Determination of (Ethylenedinitrilo)tetraacetic Acid, Nitrilotriacetic Acid, and Tartaric Acid. P . F . L O T T AND K. L. C H E N G .

New Titrimetric Determinations of Magnesium and Aluminum Oxinates. WOOD.

R. M . P O W E R S , R. A. D A Y , J R . , AND A. L. U N D E R ­

Business Meeting for members of the Division of Analytical Chemistry.

Spectrophotometric Determination of Molybdenum as the Quercetin Complex in an a-Bcnzoinoxime-Chloroform Medium. MENIS.

GERALD GOLDSTEIN, D . L. M A N N I N G , AND OSCAR

SECTION Β

Extraction and Flame Spectrophotometric Determination of Lanthanum.

OSCAR M E N I S , T. C. R A I N S , AND J. A. D E A N .

Ion Exchange Separation of Beryllium by Elution with Salicylate Analogs. J A C K SCHUBERT, ARTHUR LINDENBAUM, AND W I L ­ LIAM WESTFALL.

Infrared Absorption Studies of Sulfamic Acid and I t s Platinum ( I I ) Complexes. A. J. SARACENO, SAN-ICHIRO MIZUSHIMA, T. J. L A N E , AND J. V. QUACLIANO.

SECTION Β SYMPOSIUM ON MICROCHEMISTRY H. K. ALBER, Presiding

SYMPOSIUM ON MODERN TECHNIQUES IN RESEARCH ON COAL AND RELATED PRODUCTS Joint with Division of Gas and Fuel Chemistry R. A. GLENN, Presiding X-ray Studies of Coals and Coal Derivatives.

SABRI ERGUN

AND V. H. T I E N S U U .

Application of Thermoanalytical Techniques to a Study of t h e Pyrolysis of Coals.

C L E M E N T CAMPBELL AND SAUL GORDON.

Infrared Spectra of Fulvenes.

J. C. WOOD, R. M . ELOFSON, AND

D. M. SAUNDERS.

Introductory Remarks. Η . K. ALBER. Review of Microchemistrv. A. STEYERMARK.

Specific Volume-Composition Relations in t h e Study of Coal Structure.

W. R. K. W u AND H . C. HOWARD. VOL. 29, NO. 8, AUGUST 1957 ·

27 A

NEWS Analysis of Nitrogen Dioxide by Gas-Solid Chromatography.

Thursday Morning

S. A. GREENE AND H. PUST.

SECTION A SYMPOSIUM O N A D V A N C E S I N G A S CHROMATOGRAPHY Joint with Division of Petroleum Chemistry EMIL F. WILLIAMS, Presiding Introductory Remarks. E. F. WILLIAMS. Some Fundamental Aspects of Gas Chromatography.

A. I. M.

KEULEMANS.

Nonideal Effects upon Elution Curve Shape in Vapor Partition Chromatography.

Thursday Afternoon SECTION Β SYMPOSIUM O N M O D E R N TECHNIQUES IN RESEARCH O N C O A L A N D RELATED PRODUCTS Joint with Division of Gas and Fuel Chemistry

T. G. NORRIS AND Ο. Κ. CROSSER.

WILLIAM H. ODE, Presiding

Selectivity of Various Liquid Substrates Used in Gas Chromatog­ raph}'.

H. M. TENNEY.

Design Parameters for Process Gas Chromatographs.

W. J.

BAKER, H. L. NORLIN, T. L. ZINN, AND R. F. WALL.

Sampling and Gas-Liquid Chromatographic Analysis of Organic Air Pollutants. GIBSON.

P. W. WEST, BUDDHADEV SEN, AND N. A.

Infrared Spectroscopy as a Means for Evaluating Pitches for Use as Binders in the Preparation of Electrodes for the Alumi­ num Industry.

D. S. MONTGOMERY AND F. E. GOODSPEED.

Improved Method for Determination of Coking Value of Binders Used in Carbon Electrode Manufacture. L. GIROLAMI AND L. P. CHARETTE.

Structures of the Acids Obtained by Oxidation of Bituminous Coal. Thermal Decarboxylation of the Copper Salts. R. S. MONTGOMERY AND E. D. HOLLY.

SECTION Β

Comparison of the Thermal Decomposition of the Copper Salts with the Copper-Quinoline Decarboxylation Method. R. S. MONTGOMERY AND E. D. HOLLY.

SYMPOSIUM O N M O D E R N TECHNIQUES IN RESEARCH O N C O A L A N D RELATED PRODUCTS Joint with Division of Gas and Fuel Chemistry R. S. MONTGOMERY, Presiding Interaction of Organic Vapors with Coal. Irreversible Sorption of Amines.

RUTH TRAMMELL AND PAUL FUGASSI.

Determination of Total Pyridines and Total Quinolines in Low Temperature Coal Tar Distillates by Ultraviolet Spectro­

Chemistry and Properties of Humic Acids from Lignitic Mate­ rials. Source and Some General Properties. C. M. FROST, J. J. HOEPPNER, AND W. W. FOWKES.

Friday Morning SYMPOSIUM O N A D V A N C E S I N G A S CHROMATOGRAPHY Joint with Division of Petroleum Chemistry

photometry. ΤΑ-CHUANG LO CHANG AND CLARENCE KARR, JR.

JOHN E. WILLARD, Presiding

Identification and Determination of Low Boiling Phenols in Low Temperature Coal Tar.

CLARENCE KARR, JR., P. M. BROWN,

P. A. ESTEP, AND G. L. HUMPHREY.

Differential Infra Spectrometry Technique Used for Study of Coals.

R. V. SMITH, M. E. WADSWORTH, AND G. R. HILL.

Determination of Hydroxyl Content of Coals by the Formation of Trimethylsilyl Ethers.

SIDNEY FRIEDMAN, W. A. STEINER,

Quantitative and Qualitative Analj-sis of Fatty Acids in the Range Ci to C2o.

WILLIAM INSULL, JR., AND A. T. JAMES.

Gas-Liquid Chromatography of the Volatile Components of Onions.

J. F. CARSON AND F. F. WONG.

Analysis of C6--C9 Aromatics b}' Gas-Liquid Partition Chromatog­ raphy.

W. C. JONES, JR.

RAPHAEL RAYMOND, AND IRVING WENDER.

Resolution of Isomeric Hexanes b3" Gas-Liquid Chromatograph3·.

HOLMES AND D. C. HILLS.

Gas Chromatography. Analysis of the Crude Reaction Product from the H}'droform}dation of Isobutene. J. F. HASKIN, G.

Effect of Side Wall Friction on Coal Expansion Tests. C. R.

ALBERT ZLATKIS.

W. WARREN, R. E. KOUREY, AND V. A. YARBOROUGH.

Gas Chromatograph}-. Analysis of Constituents in the Study of Azeotropes. J. F. HASKIN, G. W. WARREN, L. J. PRIESTLEY, AND V. A. YARBOROUGH.

Thursday Afternoon SECTION A SYMPOSIUM O N A D V A N C E S I N G A S CHROMATOGRAPHY Joint with Division of Petroleum Chemistry

Friday Afternoon SYMPOSIUM O N A D V A N C E S I N G A S CHROMATOGRAPHY

D. H. LICHTENFELS, Presiding

Joint with Division of Petroleum Chemistry

Low Pressure Electric Discharge Detectors. R. C. PITKETHLY. Use of Time of Flight Mass Spectrometry and Vapor Phase Chromatography in Identification of Unknown Mixtures.

PAUL Η. ΕΜΜΕΤΤ, Presiding

R. S. GOHLKE.

High Temperature Gas Chromatography Apparatus. 3. S. FAWCETT AND B. W. TAYLOR.

Double Column Gas Chromatography. Analysis of Noncondensable and Light Hydrocarbon Gases by a Combined Gas-Liquid, Gas-Solid Chromatograph. R. T. DAVIS AND R . A . SCHREIBER.

Analysis of Fixed and Condensable Gases by Two-Stage Gas Chromatography.

JOHN MADISON.

Separation of the Rare Gases 03' Gas-Solid Chromatograph3'. S. A. GREENE. 28 A

·

ANALYTICAL CHEMISTRY

Presentation of Gas Chromatographic Data.

D. AMBROSE, A

I. M. KEULEMANS, AND J. H. PURNELL.

Gas Absorption Chromatographic Determination of Some Oxygenated Products in Cool-Flame Combustion. H. R. MENAPACE, GEORGE KYRYACOS, AND C. E. BOORD.

Evaluation of a Commercial Alk3-1 Ar3rl Sulfonate Detergent as a Column Packing for Gas Chromatography. D. H. DESTY AND C. L. A. HARBOURN.

Applications of Gas Chromatography to Petroleum Processes. W . A . DlETZ AND B . F . DUDENBOSTEL, J R .

Gas Chromatograpli3r for Plant Stream Analysis, DENBOSTEL, J R . , AND G W . ScARSTROM.

B. F. Du-

AT

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NEWS

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Both models offer an easy-reading angled index and pointer, and smart gray-and-black corrosion-resistant finish. Nickel-silver or stainless steel scoops for bulk weighing of dry chemicals are optional accessories, THESE NEW BALANCES will find constant use in the busy industrial or research laboratory. They are part of the complete Troemner line of quality balances and weights of every class, for every need. See your laboratory supply dealer, or drop us a card for Bulletin C.

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·

ANALYTICAL CHEMISTRY

Some o f the s p e a k e r s a t the a n a l y t i c a l sessions o f the N o r t h w e s t Regional m e e t ­ ing. (Left t o right) C. B. Kincannon, Shell O i l C o . ; Loyd Johnson, H o o k e r Electro­ chemical C o . ; W i l l i a m I n g r a m , O r e g o n S t a t e D e p a r t m e n t o f A g r i c u l t u r e ; Arthur Petrey (session c h a i r m a n ) . Aluminum C o . o f A m e r i c a ; J. W . M o n t z h e i m e r , C e n t e n ­ nial Flouring M i l l s ; Rex J . Robinson, University o f W a s h i n g t o n ; John L. S h a c k l e f o r d , Boeing A i r p l a n e Co.

N W Regional M e e t i n g Spotlights Analyst's Role in Industry SPOKANE, Wash. The role of the analytical chemist in those industries which are of major importance in the northwest area highlighted papers on analytical chemistry presented at the Northwest Regional ACS Meeting held here, June 13 and 14. Petroleum Refining. Vanadium, nickel, copper, and iron all have a detrimental effect on catalysts used in petroleum cracking processes. Tech­ niques used at Shell Oil's Anacortes, Wash., refinery for determining trace amounts of these elements were de­ scribed by C. T. Magnin and C. B. Kincannon. Fresh catalyst is added to the system daily and careful analy­ tical control exercised to determine optimum addition rate. Analytical methods developed by Shell for these elements involve reaction of each metal with a specific reagent and subsequent measurement of absorbance with a spectrophotometer. Impurities in Hydrogen. Trace im­ purities in hydrogen used for ammonia synthesis will poison the catalyst used as well as carry over into the final product. Methods used in Hooker ElectrochemicaFs Tacoma, Wash., plant for determining trace impurities in hydrogen were described by Loyd Johnson of that company.

Organic chlorides are determined by decomposing them to HC1 over a hot platinum wire and precipitating the chloride with silver nitrate. AgCl is then determined turbidimetrically. Carbon dioxide presents a particu­ larly difficult problem, since it is present only to the extent of 0 to 10 p.p.m. Hooker developed a conduc­ tivity method which proved satisfac­ tory. The C 0 2 is absorbed in 0.01ΛΓ Ba(OH)j in a special cell. The test cell and a standard cell are made arms of a Wheatstone bridge. Difference in the conductivities of the B a ( 0 H ) 2 solutions is determined as a measure of the C 0 2 content. Aircraft Manufacturing. The an­ alytical chemistry group at Boeing Airplane has two prime responsibilities, according to J. I. Campbell of that company. For engineering the an­ alysts must develop parameters which will be of assistance in writing speci­ fications for purchased materials. Also, for manufacturing, they must ensure that purchased materials meet these specifications. As a result, work of the analyst covers a wide range—literally from A to Ζ—from the examination of anaero­ bic molds to the determination of zinc in die metals. The analytical re-

NEWS

' W h y is t e m p e r a t u r e control so important in G a s C h r o m a t o g r a p h y ? " Because the reliability of analysis depends upon establishing, maintaining, and reproducing precise temperatures in the chromatographic column through which the samples are passed. Variations of 1°C. produce changes of 5% in retention times—may make component identification impossible. The Beckman GC-2 Gas Chromatograph (with a control range from 40°C. to 240°C.) can handle gases and liquids with boiling points up to 350°C. and maintain precise column temperatures closer than ±0.5°C. This precision control is accomplished by the unique GC-2 proportional control system*. The heating element is continuously regulated and sensitive to changes as small as 0.01 °C. The GC-2 metal-to-metal conduction system completely equilibrates column temperature in 10 minutes after a 30° increase on the range control. Columns can be changed readily... more samples can be run with less time lost between analyses. By comparison, air-transfer heat systems normally take several hours to stabilize column temperature. The unequalled stability and reproducibility of the Beckman GC-2 is absolutely necessary for accurate, consistent qualitative analysis and for quantitative measurements in the order of one part per million. "IS A HIGH TEMPERATURE INSTRUMENT ALWAYS NEEDED?"

Not when working with fixed gases or liquids with low boiling points. The Beckman GC-1 —designed especially for routine gas and vapor analysis—will handle gases with boiling points up to 80°C. Although selling for only half the price of any instrument of its kind, the GC-1 accurately solves almost any fixed gas problem. For the rest of the story on gas chromatography and a full description of the two Beckman Gas Chromatographs, see your Beckman Dealer or write for Data File L-28-15.

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For further information, circle number 32 A on Readers' Service Card, page 73 A 32 A

· ANALYTICAL CHEMISTRY

•Patent Pending

search group at Boeing has been active in many fields in addition to developing methods of analysis. It has, for example, aided the manufacturing department directly through the formulation of pH-sensitive paint for fuel tank testing. The outside of the tank under test is coated with this paint, ammonia placed in the tank, and air pressure applied. The color change shows quickly the location of any leaks. Food Industry. Services of the analytical chemist in the flour industry have increased greatly in recent years. This was pointed out by J. W. Montzheimer, Centennial Flouring Mills. He said that new activities include analysis of bleaches, softeners, and vitamin enrichments. Sanitation, both in mills and in country elevators, is receiving increasing attention and this alone has almost doubled the work of the analytical laboratory. A problem of considerable importance in the fruit and bean extract industry is detection of adulterants in vanilla extract. Previous analytical methods provided no qualitative distinction between vanilla bean extract and the extract of many other plant materials, according to Raymond Way, Crescent Manufacturing Co. This, of course, left the way open for undetectable adulteration. Way has found that if the organic acids of vanilla extract are separated by paper chromatography, a distinctive pattern is produced which is not duplicated by other plant extracts.

Automatic Analyses Changing Analyst's Role ST. ANDREWS, Scotland. Analysts are not taking enough responsibility in seeing that what they do is useful and properly applied. New techniques have revolutionized chemical analysis, but the attitude towards analysis in industry has not changed apace. This was the thesis offered by R. C. Chirnside, General Electric Co., Ltd., at the Congress on Modern Analytical Chemistry in Industry. The congress was held by the Society for Analytical Chemistry at St. Andrews, Scotland, June 24 to 28. Too much useless analysis goes on in many industries, Chirnside said. Often the people requesting an analysis are not capable of formulating the request or interpreting the results properly. At one time analysis was confined chiefly to obtaining a mere statement of percentage composition of samples submitted. Today it is much more

NEWS

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ANALYSTS

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Send me your latest Carbon-Sulfur Determinator catalog. NAME COMPANY ADDRESS CITY STATE Circle No. 34 A on Readers' Service Card, page 73 A 34 A

·

ANALYTICAL CHEMISTRY

|

Sixth Annual Conference on Industrial Applications of X-Ray Analysis, Denver Research Institute, University of Denver, Denver, Colo. Contact: J. P . Blackledge, Denver Research Institute, University of Denver. See page 37 A.

Aug. 20 to 22 ;

Conference on Liquid Scintillation Counting, Northwestern University, Evanston, 111. Contact: F . Newton Hayes, Program Chairman, Los Alamos, Ν. Μ .

Aug. 26 to 301

Eighth Annual Infrared Spectroscopy Institute, Fisk University, Nash­ ville, Tenn. Contact: Nelson Fuson, Infrared Spectroscopy I n ­ stitute, Fisk University, Nashville, Tenn.

Aug. 28 to 301

International Symposium on Gas Chromatography, Instrument Society of America, Michigan State University, East Lansing, Mich. Contact: Henry J. Noebels, general chairman, IGC Symposium, Instrument Society of America, 313 6th Ave., Pittsburgh, Pa.

Aug. 7 to 9

Sept. 8 to 13

with a

CALENDAR

132nd National Meeting, ACS, New York, Ν . Υ. See page 25 A.

Sept. 9 to 13

12th Annual Instrument Automation Conference and Exhibit, Instru­ ment Society of America, Cleveland Auditorium, Cleveland, Ohio. Contact: Herbert S. Kindler, director of technical programs, Instru­ ment Society of America, 313 Sixth Ave., Pittsburgh, P a .

Sept. 11 to 13

Fourth Ottawa Symposium on Applied Spectroscopy, Canadian Associa­ tion for Applied Spectroscopy, Victoria Museum, Ottawa. Contact: J. H . D . Howarth, Canada Metal Co., Ltd., 721 Eastern Ave., Toronto, Ont.

Oct. 14 to 16—Association of Official Agricultural Chemists, Annual Meeting, Shoreham Hotel, Washington, D . C. Coming Events · 1 S t 0 1 8 —Midyear Meeting of Recorder-Controller Section, Scientific Apparatus Makers Association, Seaview Country Club, Absecon, N. J . Nov. 2 to 10—International Congress and Exhibition of Measuring Instrumentation and Automation, Nordwestdeutsche Ausstellungs-Gesellschaft m. b . H., Ehrenhof 4, Dusseldorf, Germany. Nov. 6 to 8—Midyear Meeting of Laboratory Apparatus and Optical Sections, Scientific Apparatus Makers Association, Edgewater Beach Hotel, Chicago, 111. Nov. 14 to 16—Southeastern Regional Meeting, ACS, Durham, N. C. Dec. 26 to 31—National Meeting, American Association for the Advancement of Science, Indianapolis, Ind. Apr. 13 to 18, 1958—133rd National Meeting, ACS, San Francisco, Calif. 0ct

t h a n t h a t . I n t h e electrical industry, for example, n a t u r e a n d quality of m a ­ terials are usually of more interest. T o continue t o r u n analyses merely t o see t h a t various substances meet outmoded specifications is a waste of effort. Assay, of course, is still usually neces­ sary. T h e total cost of analytical control services in salaries, wages, a n d labora­ tory overhead probably a m o u n t s t o 1 % of cost of production in t h e chemical and allied industries, according t o B . W. Bradford, Imperial Chemical I n d u s ­ tries. This is a very large expenditure •—not only in money, b u t in scientific personnel. Besides t h e problem of training senior analytical chemists, t h e problem of s u p ­ plying large numbers of junior analysts

and assistants has been serious for some time. I t is one of t h e chief reasons for the development of analytical instru­ mentation. T h e present phase in t h e chemical industry is a transition from manual bench analysis t o laboratory in­ strumentation. T h e next stage, which is only beginning, is t h e extensive r e ­ placement of laboratory analytical con­ trol b y continuously operating processstream instruments which will ulti­ mately direct integrated automatic control systems. These t w o phases cannot b e sharply distinguished, since t h e y use t h e same types 0 f instruments t o a large extent. I n Bradford's own organization—the Billingham Division of I C I — o v e r 300 analytical control personnel of all grades are employed. During t h e past ten

NEWS

Α. I. M. Keulemans, Koninklijke Shell Laboratorium, checks his program at St. Andrews.

years t h e works has increased its pro­ duction in both volume a n d variety. B u t b y early introduction of dispersive optical spectrometry and mass spectrom­ etry as routine laboratory methods, greater control with less manpower has been obtained. Simultaneously, intro­ duction of simple types of process stream analyzers, such as katharometers and p H meters, has lightened the load of sample taking and laboratory analysis. Nevertheless, a b o u t three years ago it became necessary to increase t h e speed a n d productivity of analytical control methods. A survey revealed t h a t as far as manpower was concerned the major analytical operations in order of importance were titration, gas chro-

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DIVISION OF

An exhibition of analytical apparatus was held along with the meeting at St. Andrews.

FISHER SCIENTIFIC COMPANY 633 GREENWICH STREET · N E W YORK, Ν . Υ . For further Information, circle nwraoers 35 A-1, 35 A-2 on Readers' Service Card, page 73 A VOL

2 9 , N O . 8 , AUGUST 1 9 5 7



35

A

NEWS matography, spectrophotometry, colorimetry, vapor pressure measurement, analytical distillation, specific gravity measurement, and crystallizing point measurement. Substitution of semiautomatic titrators in the laboratory for skilled tech­ nicians is not economically significant for titrations where a marked end point can be obtained with an indicator. Where the visual end point is not defi­ nite, an automatic t i t r a t o r gives more reproducible results b y eliminating h u m a n judgment. Semiautomatic ti­ tration has been used very successfully a t Billingham for two years with Fisher's reagent in determining water in organic compounds. Fully automatic titrators have been developed for plant streams. One of these determines t h e ammonia content of the wash water in an ammonia scrub­ ber for control of water rate. Formerly sampling and determination took 20 minutes and were carried o u t once an hour. Now results are automatically available in 4 minutes and are made every 4 minutes. Gas chromatography has been a p ­ plied directly for some time to process streams b y an automatic sampler. Now I C I is attacking the more difficult problem of sampling liquid streams automatically. Introduction of optical and mass spec­ troscopic equipment into the Billingham laboratories (originally to increase t h e speed of hydrocarbon analyses) cut manpower requirements about 5 0 % . F u r t h e r improvements on the tech­ niques listed above will probably make another 3 0 % cut possible. This is probably the limit of increasing labora­ tory efficiency, because time and cost of collecting and transporting samples then achieve a much greater relative position. Continuous G a s Chromatography. Virtually the only difficulty in develop­ ing gas chromatographic analyzers t o take samples periodically from t h e plant and record results on the control room panel is constructing a sampling device, according to A. I. M. Keulemans of Koninklijke Shell Laboratorium at Amsterdam. " T o t h e best of our knowl­ edge the; entirely automatic introduc­ tion of liquid samples over long periods without attention, usually in environ­ ments t h a t are bad as compared to the laboratory, constitutes a problem which is still unsolved." T h e sample must be extremely small —a few microliters—and this q u a n t i t y must be k e p t constant to within 1 or 2 % . Also, contamination of sample with material from previous sampling cannot be tolerated, he said. Gases are easier to handle. Volumes

are about a thousand times as large, and risk of contamination is much less. I n s t r u m e n t s announced so far have been restricted to gas analysis, although one can deal with products boiling below 50° C. However, gas analysis seems to be more important generally t h a n liquid analysis in t h e petroleum refining and petrochemical fields, so the technique is not seriously limited. While gas chromatography is being adopted rapidly in a variety of indus­ tries, analytical techniques using radio­ active or stable isotopes are not being used in m a n y places where they might be very advantageous, says D . J. Ferrett, U. K. Atomic Energy Research E s t a b ­ lishment, Harwell. Evaluation of new techniques now available should not be confined to considering the traditional problem of the analyst confronted with a sample on his bench when he arrives in the morning. Proper design of re­ search experiments can make it unneces­ sary for t h e samples t o arrive a t t h e analytical laboratory a t all. Tracer techniques, for example, make it possible to follow the passage of an clement or product through a complex industrial or analytical process by ob­ serving a few atoms of added tracer. Obviously, there are difficulties in using radioactive isotopes in following a prod­ uct to be used for external consumption. B u t there are many isotopes with short half lives, so t h a t the product might be perfectly safe if stored for a month or so before use. Using stable, nonradioactive isotopes m a y be economical for following an in­ dustrial process only in very small plants, because t h e m a x i m u m allowable dilution factor is usually not more than 1000 if t h e isotope is to be detected. Besides t h e numerous variations of tracer techniques, radiation can be used t o analyze inactive samples in a number of ways: b e t a particle, x-ray, neutron, and g a m m a radiation absorption, and radioactivation analysis. These meth­ ods can "be especially valuable in re­ search to achieve accurate results often not obtainable b y other means. Initia­ tive for application of these techniques can come from t h e analyst himself. H e can point out to the research man­ ager t h a t any experiment is worthless if the final analysis is inadequate or faulty.

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X-Ray Metal Analysis Meeting Program Given T h e Sixth Annual Conference on Industrial Applications of X - R a y An­ alysis, to be held a t Denver Research Institute, Aug. 7 to 9, will present 28 papers dealing with x-ray analysis of

Barnstead

Egal M STILL & DEMINERALIHR CO.

34 Lanesville Terrace, Boston 31. Mass. Circle No. 37 A on Readers' Service Card, page 73 λ VOL. 2 9 , N O . 8, AUGUST 1 9 5 7

·

37

A

NEWS

New Stronger More Durable AGILE POLYETHYLENE CUP SINK DRAIN

metals. T h e papers represent a wide range of interests in instrumentation, methods of analysis, and applications t o process control. A. E . Ruehle, Mallinckrodt Chemical Works, is general chairman of t h e pro­ gram committee. F u r t h e r information may be obtained from J . P . Blackledge, Denver Research Institute, University of Denver. T h e program for t h e meeting is given below. August 7 New Hilger Microfocus X-Ray Genera­ tor

and

its

Applications.

FREDERICK

BRECH, Jarrell Ash Co. AND J. R.

STANS-

FIELD, Hilger & Watts, Ltd. Simplified Procedure for Calculating Peak Position in X-Ray Residual Stress Measurements on Hardened Steel. D . R. KOISTINEN, R. E. MARBTJRGBR, AND R. P.

MITCHELL, General Motors Corp. Quantitative Phase Analysis in Titanium by X-Ray Diffraction.

RALPH H. HILTZ,

JR., Water-town Arsenal. Quantitative Determination of Kyanite in Kyanite Ores by X-Ray Diffraction. T h i s new addition to the AGILE line of corrosionresistant laboratory ware is the low cost answer to d r i p p i n g sink drains and costly maintenance. Molded as one piece in natural color polyethylene, the drain is strong, resilient, impermeable and non-oxidizing. It resists the corrosion attacks of virtually a l l a c i d s a n d a l k a l i s and to a large variety of solvents. T h e drain is immediately available in 3 " χ 6 " standard oval shape w i t h the u p p e r r e t a i n i n g lip designed to fit any standard size laboratory bench top. Its 1 Vi" p i p e threaded tail piece permits fast, easy installation. A v a i l a b l e at y o u r laboratory ware dealer — Price $15.00.

Agilene chemical resistant and unbreakable labora­ tory ware now available for immediate delivery.

G. M. FAULRING AND R. D . CARPENTER,

Electro Metallurgical Co. Amorphous Solids, Small Particles, and Thin Surface Films. F . SCHOSSBERGER, Armour Research Foundation. August 8 Electrolytic Isolation and the X-Ray Study of Microconstituents in Steels. KENNETH

W.

ANDREWS,

United

Steel

Companies, Ltd. Effect of Penetration on Quantitative X-Ray Diffraction Measurements. R. E. MAHBURGER

AND

D.

R.

KOISTINEN,

General Motors Corp. Method for Obtaining a Quantitative Pole Figure of Stretched Rubber. OTTO RENIUS, Detroit Arsenal. Early Aging Effects in Copper—1.76% Beryllium Single Crystals. DORIS EVANS, Rutgers Univ. Structure of the Solid Oxidation Prod­ ucts of Carbon Black and Graphite as Revealed by X-Ray Diffraction. LUTHER LYON, D . HARVEY, B. STEWART, AND D . R.

WALLACE, Univ. of Wichita. Counting Method for Measuring Single Crystal Diffraction Intensities Using a Weissenberg Camera.

DAVID T. P E T E R ­

SON AND C L. VOLD, Iowa State College. New Microemission X-Ray Spectro­ graph Design and Operation of the Direct Emission Curved Crystal Instrument. E R W I N C. BUSCHMANN, General Electric

Co. Write for your laboratory w a r e brochure A . A . - 6

Application of t h e Microemission X-Ray Spectrograph. Comparison of Analyses from Small Areas. J. F . NORTON, General Electric Co. X-Ray Fluorescent Analysis of Powders by the Method of Mixtures.

AMERICAN AGILE CORPORATION Plant and General Offices . 5461 Dunham Rd. · Maple Heights, 0 . Mailing Address, P. 0. Box 168 · Bedford, 0 . For further information, circle number 38 A on Readers' Service Card, page 73 A ANALYTICAL CHEMISTRY •

38 A

·

JACOB SHER­

MAN, Philadelphia Naval Shipyard. X-Ray Spectrographs Determination of Tantalum, Columbium, Iron, and Titanium Oxide Mixtures Using Simple Arithmetic

NEWS

MORATORY ifflC/MOY

CM€M

Corrections

for

Interelement

Effects.

BETTY J. MITCHELL, Electro Metallurgical

Co. Determination of Uranium Dioxide in Stainless Steelsby the X-Ray FluorescenceSolution Method.

WILLIAM H O U K , LOUIS

SILVERMAN, AND LAVADA MOUDY, Atomics

MiNI-lAB

International. Results Obtained with the Modified

SAVES T I M E - S P A C E - M O N E Y

Philips Electronics, Inc.

Originally introduced by Ace in 1:950 with $ 1 4 / 3 5 jojnts* Additional assemblies and ' compo­ nents added in 1954, and joints con­ verted to $ 1 4 / 2 0 size.

Now, in 195 7, Ace makes an­ other advancement with many new components, and many items equipped with :?1 8 / 1 9 joints; truly the most versatile line small-scale gltisswti-e_ available.

Norelco Autrometer.

DAVID C. MILLER,

N e w Systems Division Formed b y Beck m a η Instruments

August 9 Nondispersive X-Ray Fluorescence Unit for the Analysis of Biological Tissue Sec­ tions.

THEODORE HALL, Sloan-Kettering

Institute for Cancer Research. Rock Analysis by X-Ray Fluorescence Spectroscopy. ARTHUR A. CHODOS, J. J. BRANCO, AND C. G. ENGEL, California

Institute of Technology. Micro-Analysis with Ultra Fine X-Ray Sources.

V. E. COSSLETT, P. DUNCUMB,

AND J. V. P. LONG, Univ. of Cambridge. Applications of the Electron Probe Microanalyzer.

L. S. BIRKS AND E. J.

BROOKS, U. S. Naval Research Laboratory. X-Ray Spectrographic Analysis of Nickel Containing Alloys with Varied Sample Forms.

C. MANNING DAVIS AND GEORGE

R. CLARK, International Nickel Co., Inc. X-Ray Emission Spectrographic Analysis of Bastnaesite Rare Earths. FARRELL W. LYTLE,

JAMES

I.

BOTSFORD,

AND

H.

HELLER, U. S. Bureau of Mines. Applications of X-Ray Spectrography to Continuous Analysis for Process Control. ROBERT A. M C C U N E , WILLIAM M. M U E L ­

LER, AND PAULINE J. DUNTON, Denver Re­

search Institute. Comments on a Beta-Excited X-Ray Source.

LUTHER E. PREUSS, Edsel

B.

Ford Institute for Medical Research. Analysis of Diffusion Couples by X-Ray Absorption.

ROBERT E. OGILVIE, Massa­

chusetts Institute of Technology. Principles and Applications of Propor­ tional Counters for X-Ray Spectrographs. IRWIN I. BESSEN, Philips Electronics, Inc.

Components for X-Ray Polychromators. J. L. JONES, K. W. PASCHEN, AND H. H .

SWAIN, Applied Research Laboratories. Recent Applications with the X-Ray Microscope.

Electric Co.

sions of t h e meeting will be held in rooms provided b y General Electric in its Schenectady plant, a n d a banquet, with featured speaker, is planned. N o r m a n Nachtrieb, University of Chicago, has been chosen as general chairman of t h e 1958 symposium.

A new systems division has been or­ ganized by Beckman Instruments, with headquarters a t Anaheim, Calif., a n d manufacturing facilities a t Anaheim and Richmond, Calif. Arnold O. Beckman, president, said t h a t t h e expansion would help meet growing demand for automatic process monitoring a n d con­ trol systems. T h e new division will consolidate various groups formerly a p a r t of t h e company's Berkeley a n d Scientific Instruments divisions. T h e combined operations will be housed in buildings now under construction a t t h e two cities. J o h n F . Bishop, general manager of the Berkeley and Process Instruments divisions, will head t h e new Systems Division.

L. C. Mitchell W i n s First AOAC-Wiley Award Lloyd C. Mitchell, research chemist, Food a n d D r u g Administration, has been announced as t h e first winner of t h e annual H a r v e y W. Wiley Award of t h e Association of Official Agricultural Chemists. T h e award of $500 was es­ tablished last year t o honor t h e father of t h e original P u r e Food a n d D r u g Act. I t will go each year t o t h e scientist who makes an outstanding contribution t o

S E L B Y E . SUMMERS, General

Locales of Summer Symposia Decided

Send f o r N e w Supplement A— F describing

t h e A l l - N e w ACE " M i n i - L o b "

A l s o i n i i o e V a t o u r M i d w e s t e r n Division,

ACE GLASS I N C O R P O R A T E D VINELAND •

N E W JERSEY

Midwestern Division

LOUISVILLE, KY.—Box 9 9 6

Specialists to Industry and Research Circle No. 40 A on Readers' Service Card, page 73 A 40 A · ANALYTICAL CHEMISTRY

Location of summer symposia for t h e next three years has been announced b y the Division of Analytical Chemistry. T h e 1958 meeting is to be held a t Schen­ ectady, Ν . Υ., J u n e 20 and 21. I n 1959 and 1960 t h e meetings will be a t t h e Universities of Illinois a n d Houston, respectively. Cosponsors^of t h e 1958 meeting are General Electric Corp.. a n d Union Col­ lege. T h e day-and-a-half series will feature reactions in fused media. Ses­

L. C. Mitchell

NEWS

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AOAC Meeting Will Feature MicroscopicAnalytical Methods

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ΛΛ M Q C ψ ΐ J | Ov

STANDARD SCIENTIFIC SctftfcÙf @&lfr. 42 A

·

the development of methods for the analysis of foods, drugs, cosmetics, feeds, fertilizers, pesticides, and soils. Mitchell, since the beginning of his career in 1909, has developed many methods of analysis for spices, cereals, dairy products, and eggs. More recently he has been active in the development of techniques of paper chromatography. A native of Morrisonville, 111., he received his bachelor of science degree at Oklahoma A & M College.

808 BROADWAY N E W YORK 3 , N Y .

For further information, circle number 42 A-2 on Readers' Service Card, paie 73 A ANALYTICAL CHEMISTRY

EACH

A symposium on microscopic-analytical methods for product control in the food and drug industries will be offered at the 71st annual meeting of the Association of Official Agricultural Chemists in Washington on Oct. 15, 1957. Ten papers on plant sanitation and laborator}^ methods are planned. Of particular interest to analysts will be those on the role of the laboratory in quality control, radiographic examination of cereal grains, and integrated quality control. Kenton L. Harris, Food and Drug Administration, is general chairman of the symposium. Further information may be obtained from William Horwitz, Secretary-Treasurer, Association of Official Agricultural Chemists, Box 540, Benjamin Franklin Station, Washington 4, D. C.

SE Regional Meeting to Be Held at Durham in November The

1957 Southeastern

Regional

Meeting of the AMERICAN CHEMICAL

SOCIETY will be held in Durham, N. C , November 14 to 16, 1957. Symposia are planned dealing with organic reaction mechanisms, electrolytic solutions, new developments in analytical chemistry, organic fluorine chemistry, and tobacco chemistry. Papers are invited on organic, inorganic, physical, analytical, and biological chemistry, chemical education, and chemical engineering. Pelham Wilder, Jr., Duke University, is general chairman. C K. Ingold, University of London, will address the general session. Members wishing to present papers at the meeting should send titles, names of authors, and an abstract of not more than 200 words to J. C. Morrow, Department of Chemistry, University of North Carolina, Chapel Hill, N. C , before Aug. 15.