ANALYTICAL
CHEMISTRY
·
ASTM Mass Spectrometer Session Draws Record Attendance N E W O R L E A N S . — A t t e n d a n c e figures here a t t h e J u n g Hotel clearly indicate t h e A S T M E-14 Committee Meeting on Mass Spectrometry has reached t h e s t a t u s of " m e c c a " for national experts in t h e field. F r o m listening to 48 papers in 4 days ( M a y 24 to 28) one gathered t h e impression t h a t there is a definite trend b y manufacturers t o produce smaller, portable units a t lower cost with performance characteristics comparable t o larger laboratory installations. Smaller spectrometers are now being designed specifically for monitoring and control of process gases, with rugged construction capable of continuous service. Although t h e principle of applying combined electrical and magnetic fields for improved ion beam focusing was reported almost 20 years ago, Consolid a t e d Engineering has now introduced a small commercial i n s t r u m e n t to exploit recent advances in techniques. T h e cycloidal analyzer, as described b y C. P . Robinson and L". G. Hall, is free of aberration due to cross-talk, has substantially higher dispersion'than a sectort y p e instrument, and will m a k e a clean separation between two peaks when there is no valley present between them. T o evaluate adequately t h e nonmagnetic radio-frequency principle of m a s s selection, research workers a t Phillips Petroleum h a v e constructed a 5-stage t u b e and h a v e studied t h e operating variables. T . C. W h e r r y and F . W. Karasek said the R F principle appears a t t r a c t i v e because it promises to give a mass spectrometer of simple construction and rugged n a t u r e . D a t a indicate t h e t u b e is capable of sufficient resolution t o handle m a n y hydrocarbon analyses encountered in a petroleum refinery. Suitable accuracy was also obtained during the analysis of a gas mixture containing 6 4 . 8 % hydrogen, 3.0% helium, 9.0% methane, 2 0 . 1 % nitrogen, and 3.7 argon. Beckman I n s t r u m e n t s now has a mass spectrometer ( R F linear decelerator) which features resolution to 100 and a dynamic range of 2000 t o 1, reported W. Donner. Stressing mass spectra and stability data, Donner said the cracking p a t t e r n stability for b o t h w-butane and propane was within 1 % ; t h a t sensitivity stability is in t h e range of 2 % . This performance is obtained without a temperature controlled source. Elimination of a n y m a g n e t gives a compact spect r o m e t e r t u b e especially suited for procVOLUME
2 6, N O . 6, J U N E
1954
ess applications where size is a n import a n t consideration. At Esso Laboratories in B a t o n Rouge, K . P . Lanneau, L. H . Lane, and R . J. Vick h a v e been evaluating the new ion resonance spectrometer manufactured b y General Electric. F r o m a perform-
JUNE
1954
·
NEWS
ance point of view, L a n n e a u said it has excellent sensitivity a n d resolution u p t o mass 100 for application t o gaseous compounds. I t can be used t o reproduce mass spectra on a cathode ray oscillograph, and is well suited for analysis of regenerator v e n t gases in the refinery (CO-2, CO, 0 2 , N 2 ) . T h e i n s t r u m e n t has unusually high resolution in the low mass range, should offer interesting possibilities in t h e field of atomic energy. Spectra show complete resolution between mass peaks for helium a n d D 2 (m = 0.04 atomic m a s s u n i t ) .
Pros a n d Cons of Paper C h r o m a t o g r a p h y W e i g h e d a t N I H Symposium W A S H I N G T O N . — I n s t r u m e n t makers, designers, and users gathered here a t the National Institutes of Health M a y 24 to 26 for the F o u r t h Annual Research E q u i p m e n t Exhibit. I n addition to the exhibit, there were four symposia on instrumentation techniques and t h e latest developments in i n s t r u m e n t research. M o s t heavily a t t e n d e d symposium was on electrophoresis and chromatogr a p h y . Symposium chairman, H e n r y G. Kunkel, opened the session, with a discussion of t h e advantages and disadvantages each technique offered. H e pointed out t h a t for the present he favored reliance on b o u n d a r y electrophoresis for definitive conclusions in most
cases. H e said h e believed t h e m e t h o d was t h e most precise for mobility s t u d ies. Electrophoresis, however, has certain limitations which paper chromatogr a p h y can overcome. F o r instance, Herbert A. Sober told t h a t recent work b y himself and associates indicates t h a t large protein molecules can be separated b y a cellulose ion exchanger developed b y t h e m . I n addition, t h e y find the m e t h o d often aids t h e m to h a v e a higher resolving power t h a n in electrophoresis. Analysts trying t o specialize with either one of the techniques according to William R. Carroll, N I H , should realize t h a t t h e two techniques are complemen-
Dean Burk (seated) and George L. Hobby, both of National Cancer Institute, look over new electrostatic electron microscope produced by Farrand Optical Co.
Kent M. Wight, National Cancer Institute, and Lawrence R. Crisp, NIH, discuss compact polarograph made by Patwin Instruments. Precalibrated electrodes are used for faster analyses of routine samples
21 A
NEWS
PROBE i ηt ο
yουr
Robert J. K o e g e l (left), National Cancer In stitute, e x p l a i n s fea tures o f r o t a r y Kjeldahl digestion a p p a r a tus (American Instru ment Co.) he helped design, to Elizabeth G . Frame, NIH, a n d Leon a r d H. B o l z , N a t i o n a l Bureau of Standards. S e v e r a l c h a n g e s in the instrument w e r e incor p o r a t e d at the sugges tion o f the Committee on Microchemical A p paratus of the ACS Division o f Analytical Chemistry
',
p H problems on-the-spot . w i t h the
Analytical
pocket
r e v o l u t i o n a r y [°;t?c£>L®e y n i t
Completely self-contained in waterproof ever-ready case with shoulder strap, Instrument s i z e : 3 χ SYz χ VA inches Case s i z e : 3 % χ bVz χ 4 Va inches Weight w i t h accessories: 3 lbs. Permits.continuous, direct reading pf p H . No buttons to hold down or dials to-,turn!
Analytical Measurements, Inc. 585 M A I N ST.
CHATHAM, N. J.
Analytical Measurements, Inc. 585 Main Street, Chatham, N. J . Please send full information t o : Name Company . Address — City
.State.
Circle No. 22 A on Readers' Service Card, page 41 A
22 A
I
t a r y and should not be divorced from one another. R a t h e r , t h e y should be used to cross reference each other, with each contributing- its obvious advantages t o t h e final conclusion. I n t h e symposium on methodology a n d instrumentation in microanalysis, Alsoph H . Corwin, J o h n s Hopkins, dis cussed the design and construction of a new microbalance. H e hopes t h a t it will eliminate m a n y of t h e previous sources of error which h a v e occurred. I t is housed in a double sheath of alumi num, is free from relative h u m i d i t y a n d t e m p e r a t u r e changes', and has incorpo rated a special device which makes it free from vibration. Balance uses specially fabricated materials and is designed and constructed b y techniques developed b y him over a period of 20 years. H e has t a k e n especial pains in constructing t h e balance t o incorporate strain-relief de vices. An electronic device which can obtain d a t a on the configuration of individual molecules was described b y Raold Wangsness, N a v a l Ordnance Labora tory, W h i t e Oak, M d . Wangsness says he uses the technique of nuclear m a g netic resonance to measure q u a d r u p l e m o m e n t s of molecules. C o m m e n t s b y others after the paper h a d been deliv ered said the a p p a r a t u s was a b o u t "one step removed from visualization of the actual molecule." Some of the instruments on display a t t h e exhibit included a recording spec trophotometer b y B e c k m a n I n s t r u m e n t s . I t automatically records t h e light absorption spectra of a sample a n d enables the operator to m a k e a closer de termination of the chemical composition of the sample. F a r r a n d Optical showed a n improved electron microscope which permits magnification to 200,000-plus diameters, gives high resolution, a n d costs $12,500 to build.
Glycerol Determination T h e Uniform M e t h o d s C o m m i t t e e of the American Oil Chemists' Society h a s recommended t h a t : The acetin method for glycerol, E a 4-38, and the dichromate method for glycerol, E a 5-38, be removed from AOCS official methods. T h e sodium periodate method for glyc erol, Ea 6-51, be retained as the only AOCS official method for glycerol, with minor changes. T h e recommendations were approved b y t h e society a t its April 1954 meeting.
100,000th Scientific Instrument C o m m e m o r a t i n g t h e production of t h e 100,000th i n s t r u m e n t — a recording spectrophotometer—by B e c k m a n in struments, Inc., South Pasadena, Calif., Arnold O. Beckman, president, pre sented a gold nameplate t o R. Francis Faull, m a n a g e r of t h e California Re search Corp.'s La H a b r a Laboratory, where t h e i n s t r u m e n t will be used in research on petroleum hydrocarbons.
Exhibit of Physical Society T h e exhibition of t h e Physical Society opened April 8 a t t h e Imperial College of Science a n d Technology, London, England. A m o n g t h e scientific instru m e n t s and a p p a r a t u s was the "flying s p o t " microscope which uses television t o magnify t o a n e x t e n t t h a t rivals t h e electron microscope. T h e pitch indi cator developed b y Kelvin H u g h e s gives t h e pilot an exact reading of the nose elevation of his aircraft during take-off. Photographic representations of t h e electron density in a crystal were shown b y t h e Crystallographic D e p a r t i n e n t of the Cavendish L a b o r a t o r y , C a m b r i d g e . A micro hardness tester for rubber A N A L Y T I C A L
C H E M I S T R Y
For further information, circle number 23 A on Readers' Service Card, page 41 A
>-
NEWS (Nash and Thompson), will test the hardness of a specimen of rubber 3/i6 inch in diameter, a nucleonic weight gage (Electronic Instruments) uses radioisotopes to control the weight of tobacco used in cigarette-making ma chines, and the unit developed by Mullard Ltd., for use with a resistance furnace temperature controller, will automatically control the temperature of the furnace from 1° to 1000° C. over short or long periods. The small analog computer built of standardized component units exhibited by Elliot Brothers (London), Ltd., has an accuracy of 0.1% as against 1% for most existing small analog computers. A direct-reading spectrometer for de termining the composition of an alloy was shown by Hilger and Watts. A number of exhibits were especially concerned with the development of British nuclear industry. The Atomic Energy Authority showed a small scale working model of an electromagnetic pump which may be used for pumping liquid metals such as mercury or sodium through the breeder reactor being built at Dounreay, in order to draw off the heat. Equipment used for surveying for radioactive materials from aircraft was shown by Edison Swan Electric Co.
CARL ZEISS
A range of scintillation phosphors for use in scintillation counters was shown by Isotope Developments, Ltd., and a number of radiation counters of different shapes and sizes have been designed for both industrial and personnel use.
Southwest Regional Meeting The Dallas-Fort Worth Section of the AMERICAN CHEMICAL SOCIETY will
be host to members during the Tenth Southwest Eegional Meeting, to be held in Fort Worth December 2 to 4. The region embraces Texas, Louisiana, Arkansas, Oklahoma, and New Mexico.
Papers are invited for presentation in the fields of analytical chemistry, biochemistry, chemical education, in dustrial and agricultural chemistry, organic chemistry, petroleum chemistry, and physical and inorganic chemistry. Information on title, author's name, and subject matter must be received not later than September 1. Two copies of a 200 word abstract must be re ceived not later than October 1. Gen eral correspondence regarding the tech nical program should be sent to Harold Jeskey, Southern Methodist Univer sity, Dallas, Tex. Chairman Of the section on analytical chemistry is C. T. Kenner, Southern Methodist Univer sity, Dallas, Tex.
ANALYST'S CALENDAR American Chemical Society. 126th Na tional Meeting, New York, Ν . Υ., September 12 to 17. Seventh Annual Analytical Symposium. Minneapolis, Minn., June 18 and 19. Sixth Annual Oak Ridge Summer Sym posium on Modern Analytical Chem istry. Oak Ridge, Tenn., August 23 to 27. Sixteenth Midwest Regional Meeting, American Chemical Society, Omaha, Neb., November 4 to 6, 1954.
ABBE
Microchemistry and Microchemical Instrumentation A symposium on Microchemistry and Microchemical Techniques will be held September 17, 1954, in connection with the Instrument Society of America First International Instrument Exposi tion, at Convention Hall in Philadelphia. The purpose of the symposium is to show that microchemistry has now come of age and supplies a useful and much needed technique. Historical develop-
REFRACTOMETER Made in West Germany
T h e famous ABBE REFRACTOMETER is available incorporating t h e following f e a t u r e s : • Range of measurements: no 1.3 t o RD 1.71 and 0% t o 95%. by transmitted and reflected light.
For liquids and solids
• Compensator for dispersion measurements. • Measuring surface of index prism always at horizontal position. • Observation telescope mounted stationary at an inclined posi tion t o carry out measurements at a relaxed posture. • Line of total reflection and scales are observed simultaneously in telescope. • Index prism in heating mount can be easily interchanged. • Special index prism in heating mount available for measurements up to no 1.85. (On special order only) • For highest-accuracy-measurements an Ultra-Thermostat with constancy of temperature ± 0 . 0 0 5 ° is available. Free detailed literature sent upon request
CARL· ZEISS, INC.,
485 F i f t h Ave., N e w York 17, Ν . Υ .
Guaranteed uninterrupted repair service For further information, circle number 26 A on Readers' Service Card, page 41 A
26 A
ANALYTICAL
CHEMISTRY
m e n t a n d newest progress in various phases will b e presented with emphasis on instrumentation. T h e symposium should serve a s a review of p a s t a n d present accomplishments as well as a n idea of w h a t m a y b e expected in t h e future.
INTRODUCING A NEW CONCEPT
SEPARATORY FUNNELS
Opening of Symposium and Introductory Remarks. H. K. ALBER, Chairman, Arthur H. Thomas Co., Philadelphia, Pa. Microchemical Techniques. A. A. BENEDETTI-PICHLER, Honorary Chairman, Queens College, Flushing, Ν. Υ. Quantitative Organic Microanalysis. A L STEYERMARK, Hoffmann-La Roche Inc., Nutley, N. J. Physicochemical Methods in Microanaly sis.
EMPLOYING
The
KONTES SEPARATORY FUNNELS Provide Practical Benefits to A l l Segments of the Chemical Industry
HARRY LEVIN, Texas Oil Co., Beacon, Ν. Υ.
Chemical Microscopy (Fusion Methods). Armour Research
Foundation, Chicago, 111. Discussion and showing of moving pictures depicting microchemical techniques.
R
egardless of t h e specialized chemical field in which you are engaged, t h e ULTRAMAX TEFLON VALVE, embodying in principle a sharp departure from conventional stopcocks, will provide you w i t h a host of exceptional values.
T h e committee for t h e symposium consists of A r t h u r H . Hale representing t h e Affiliated Analytical Group, Dela w a r e Section, A M E R I C A N C H E M I C A L S O C I
ETY; J o s . Alicino, representing t h e Metropolitan Microchemical Society, New Y o r k ; Win. C . Ellenbogen repre senting t h e Analytical a n d Microchemi cal Group, Philadelphia Section, A M E R I
N o lubricants, for instance, are required in these Separatory Funnels. This means that you can now handle any material heretofore sensitive t o this substance. Acids, alkalies and other reagents will not cause them to stick. Without lubricants t o dissolve, there is also freedom from troublesome leakage.
CAN CHEMICAL SOCIETY ; R i c h a r d Z a h n e r
representing t h e South Jersey Section, AMERICAN CHEMICAL SOCIETY;
Teflon
VALVE...
JOHN MITCHELL, J R . , Experiment Sta
tion, E. I. du Pont de Nemours & Co., Wilmington, Del. Microanalysis in the Petroleum Industry. WALTER C. MCCRONE,
Ultramax
The smaller sizes of funnels (30 t o 125 m l ) are especially adaptable for centrifuging to speed up separations, and t h e valve is so designed t h a t it is completely locked in during this process. The K-4525 series, cylindrical type, 30 m l . , is ideal for vitamin analysis.
Herbert
K. Alber, Chairman. Members of t h e sponsoring groups or sections m a y obtain free preregistration tickets from their representatives on t h e committee.
It 'will pay you well to investigate KONTES' FUNNELS today.
Summer Courses at University of Padua
SEPARATORY
TYPES NOW AVAILABLE
T h e University of P a d u a will hold summer courses a t Bressanone (Dolo mites zone), Italy, including a series of lectures a t t h e Center of Polarography. July 26 to 30. Production and Use of Radioactive Isotopes. August 2 to 6. Theoretical and Practical Polarography. August 9 and 10. Chromatography. August 11. Electrophoresis. August 12. Spectrophotometry. August 13. Electronics. Information is available from t h e University of P a d u a , Via L . Loredan, Padua, Italy.
Zeitschrift fur Physikalische Chemie T h e M a y 1954 issue of t h e Zeiisckrift fur Physikalische Chemie, Neue Folge (Volume 1, Nos. 1/2) contains papers b y Abel, Bandow, Block, Bonhoeffer, Gonser, Hauffe, Kahlweit, Rahmel, Schulz, Schwab, Strehlow, a n d S u h r m a n n . I t VOLUME
2 6, N O . 6, J U N E 1 9 5 4
K-4535
K-4545 K-4525 Write for Literature on Complete Series of Separatory Funnels. Ask also for Complete Catalog on Kontes* High Quality Standard and Specially-Designed Labora tory Glassware.
*Ultramax—Reg. T.M. of Fischer & Porter Co.—*Tef)on—Reg. T.M. of E.I. DuPont Co.
KONTES
GLASS
COMPANY
V I N E L A N D , N E W JERSEY For further information, circle number 27 A on Readers' Service Card, page 41 A
27 A
NEWS is published by Akademische Verlagsgesellschaft m. b. H., Holbeinstrasse 25-27, Frankfurt-am-Main, Germany.
NEW BOOKS Chemistry
of
the
Lanthanons.
R.
C.
Vickery, vii + 280 pages. Aca demic Press, Inc., 125 East 23rd St., New York, Ν. Υ., 1953. $6.00. Reviewed
by
CHARLES
V.
BANKS,
Iowa State College, Ames, Iowa. The material presented was taken pri marily from the literature prior to 1952, although several references are included to work published during 1952. After four short chapters entitled "Historical Development," "Modes of Occurrence," "Structure, Spectroscopy and Paramagnetism," and "Isotopic Constitution, Radioactivity and Va lency," the author discusses at great length (8 chapters, 132 pages) the sub ject of separational techniques. The older separational techniques are dis cussed in great detail, while only 4 or 5 pages are devoted to each of the newer techniques of ion exchange and solvent extraction methods. Chapter 13 gives a rather complete discussion of the properties of the lighter
lanthanons, which includes a discussion of the oxides, hydroxides, carbonates, oxalates, halides, nitrates, sulfates, sul fides, phosphates, cyanides, perchlorates and complex compounds. Chapter 14 is devoted to a brief discussion (5 pages) of the properties of the heavy lan thanons. Analytical methods for the rare earths which are based on oxidationreduction, average atomic weight, neu tralization, magnetic susceptibility, ab sorption spectroscopy, emission spec troscopy, luminescence, fluorescence, flame photometry, polarography, ion exchange, and radioactivity are dis cussed in Chapter 15. Uses and applications of the lan thanons are briefly discussed in Chapter 16 and yttrium is discussed in the ap pendix. The book is well written, but has several typographical errors. Chromatographic Methods of Inorganic Analysis. F._ H. Pollard and J". F. W. McOmie. viii + 192pages. 26 figures. Academic Press, Inc., 125 East 23rd St., New York 10, Ν. Υ., 1953. $5.50. Reviewed by Louis B. ROCKLAND, Fruit and Vegetable Chemistry Lab oratory, Western Utilization Research
Branch, U. S. Department of Agricul ture, Pasadena, Calif. Ostensibly a coverage of general chro matographic methods for inorganic anal ysis, the book is concerned largely with the paper chromatography of inorganic ions. The emphasis on paper chroma tography is not necessarily objection able, because of the great utility of these techniques for both qualitative and quantitative inorganic analysis. The authors have presented an excellent summary of procedures for the estima tion of inorganic ions based on their own work as well as contributions from other groups in the field. The text is well or ganized and written in a manner that should be acceptable to students as well as research workers. A brief but adequate history of the development of chromatography is pre sented, although the reviewer was dis appointed not to find reference to the paper by H. W. Hermance [Bell Labs. Record, 16, 370 (1938) J describing the use of paper as a medium for micro analysis of inorganic ions. As several other very recent books on paper chromatography have developed con siderable space to literature reviews, it is creditable that the authors have minimized extraneous material and have
GLASS ABSORPTION CELLS OF FINE MADE BY
QUALITY
KLETT
Complete Electrophoresis Apparatus SCIENTIFIC APPARATUS Klett-Summerson Photoelectric Colorimeters Colorimeters - Nephelometers - Fluorimeters Bio-Calorimeters - Comparators - Glass Stand ards - Glass Cells - Klett Reagents
KLETT
M A N U F A C T U R I N G CO. 177 E A S T 8 7 T H S T R E E T NEW YORK Ν. Υ.
For further Information, circle number 28 A on Readers' Service Card, page 41 A
28 A
ANALYTICAL
CHEMISTRY
