ANALYTICAL
CHEMISTRY
·
AUGUST
1956
·
NEWS
r e p r e s e n t a t i v e s of A t l a n t i c Refining, California Research, C o n t i n e n t a l Oil, Monsanto, and Procter & Gamble, m e t informally in t h e spring of 1954 a t t h e K a n s a s C i t y m e e t i n g of t h e A M E R I C A N C H E M I C A L SOCIETY to
Some of the more than 200 registrants sign up for the summer symposium
Analysts Devise IR M e t h o d for A l k y l Benzene Sulfonates faced Tow i tTh Hd eEt earnmailnyitni cga dl e tchemist e r g e n t s in surface w a t e r s , a n i m p o r t a n t i t e m a t t h e 9 t h A n n u a l Conference on A n a l y t i c a l C h e m i s t r y a t t h e U n i v e r s i t y of California a t Los Angeles, J u n e 14 t o 16, was a n e w m e t h o d for d e t e r m i n a t i o n of alkyl benzene sulfonates (ABS) a t low c o n c e n t r a t i o n s in such w a t e r s . I n a d d i t i o n t o t h e s e p a p e r s , which were p a r t of t h e p r o g r a m dealing w i t h analysis of i n d u s t r i a l wastes, t w o o t h e r major sessions were held. T h e s e d e a l t w i t h r a p i d m e t h o d s of a n a l y s i s and analytical problems encountered in biological s y s t e m s . T h e m e e t i n g , which also f e a t u r e d i n s t r u m e n t exhibits, was sponsored j o i n t l y b y t h e A C S Division of Analytical C h e m i s t r y and
ANALYTICAL CHEMISTRY.
It
was
t h e first such m e e t i n g held west of t h e Mississippi. T h e chemical p r o b l e m s involved in t h e movie i n d u s t r y were described b y Herbert Meyer, Motion Picture Research Council, a t t h e b a n q u e t . T h e s e p r o b l e m s e x t e n d far b e y o n d t h o s e of t h e c h e m i s t r y of films a n d include VOLUME
2 8, N O . 8, A U G U S T
such i t e m s a s developing a n d t e s t i n g a wide v a r i e t y of m a t e r i a l s a n d processes used in m a k i n g sets a n d p r o p s a n d those involved in so-called special effects. T h e new m e t h o d for alkyl b e n z e n e sulfonates is n o t a s h o r t m e t h o d a n d e q u i p m e n t needed in t h e p r o c e d u r e is n o t available a t all w a t e r t r e a t m e n t p l a n t s , E u g e n e M . Sallee, P r o c t e r & G a m b l e , p o i n t e d o u t . I t is specific a n d a c c u r a t e , however, a n d gives w a t e r s a n i t a t i o n chemists t h e i r first s u c h t o o l for correctly assessing effect of A B S in w a t e r a n d sewage t r e a t m e n t fields. Briefly, t h e new m e t h o d involves c o n c e n t r a t i o n of A B S in surface wat e r s b y a d s o r p t i o n on a c t i v a t e d carb o n , desorption, r e m o v a l of interfering m a t e r i a l s t h r o u g h several purifications, a n d finally a q u a n t i t a t i v e det e r m i n a t i o n w i t h infrared. I t s t e m s from c o o p e r a t i v e efforts of a s u b c o m m i t t e e on a n a l y t i c a l m e t h o d s of t h e Association of A m e r i c a n Soap & Glycerine P r o d u c e r s , I n c . T h e s u b c o m m i t t e e , which included 1956
dis-
cuss A B S a n a l y t i c a l p r o b l e m s . They were l a t e r joined b y chemists from Colgate-Palmolive, L e v e r B r o t h e r s , N a t i o n a l Aniline, a n d U. S. P u b l i c H e a l t h Service a n d formalized as a n A A S G P subcommittee. Here's t h e procedure the subcomm i t t e e h a s worked o u t a n d cooperat i v e l y t e s t e d in seven l a b o r a t o r i e s . Adsorption. Activated carbon ( N u c h a r C-190, W e s t Virginia P u l p & P a p e r Co., screened t o " o n 30 m e s h " ) is t h e a d s o r b i n g m e d i u m . T h i s is placed in a 2 b y 24 inch glass column, w i t h b r a s s or stainless steel screens dividing t h e c a r b o n i n t o sections of 20, 30, 40, a n d 10 g r a m s ( t o p t o b o t t o m ) . T h e s a m p l e is t h e n r u n t h r o u g h t h e column a t t h e r a t e of less t h a n 10 liters p e r h o u r . (If t o t a l s a m p l e v o l u m e necessary t o give 10 t o 25 m g . of A B S is less t h a n 2 liters, it is s h a k e n w i t h a b o u t 10 g r a m s of c a r b o n i n a n e x t r a c t i o n flask i n s t e a d of being r u n t h r o u g h t h e column.) T h i s concent r a t e s t h e A B S a n d also r e m o v e s it from some interfering s u b s t a n c e s . I n checking completeness of a d sorption, t h e s u b c o m m i t t e e found a residual c o n c e n t r a t i o n of 0.1 p . p . b . in 20 liters of 0.1 p . p . m . r a d i o a c t i v e A B S passed t h r o u g h 100 g r a m s of t h e a c t i vated carbon. Elution. C a r b o n sections a r e r e m o v e d from t h e c o l u m n a n d dried s e p a r a t e l y . E a c h is t h e n e x t r a c t e d twice b y boiling in a 1 t o 1 solution of b e n z e n e a n d m e t h a n o l which is 0.047V in p o t a s s i u m h y d r o x i d e . Following filtration of t h e e l u t e d carbon, ext r a c t s from t h e 20-, 30-, a n d 4 0 - g r a m sections are c o m b i n e d a n d e v a p o r a t e d , a n d t h e residue is dissolved in w a t e r . T h e 10-gram section is t r e a t e d separ a t e l y t h r o u g h o u t , absence of A B S in t h e final infrared d e t e r m i n a t i o n indicating c o m p l e t e a d s o r p t i o n of all A B S in t h e original s a m p l e . Purification. S e p a r a t i o n of A B S from r e m a i n i n g interferences consists of t h r e e s t e p s : h y d r o c h l o r i c acid h y drolysis t o d e s t r o y organic sulfates, phosphates, and other hydrolyzable s u b s t a n c e s ; p e t r o l e u m ether e x t r a c t i o n of h y d r o c a r b o n s , alcohols, a n d sterols from t h e A B S ; a n d finally complexing A B S with 1-methylheptyla m i n e a n d e x t r a c t i n g this w i t h chloroform a w a y from inorganic salts a n d water-soluble organics. Chloroform a n d excess a m i n e are t h e n e v a p o r a t e d a n d t h e r e s i d u e is 17 A
NEWS taken up in carbon disulfide or carbon tetrachloride for the IR determination. The infrared absorption curve is run from 9.0 to 10.5 microns. Absorbance of the 9.6- and 9.9-micron peaks measured against appropriate calibration curves from standardized ABS samples (available from AASGP) gives the original ABS concentration. Although lack of an infrared unit may prove a stumbling block for local water works, the method is a start toward eliminating misinterpretations now in the literature based on in-
accurate colorimetric methods, according to Sallee. The colorimetric method involves formation of an ABS salt of a cationic dye such as methylene blue, extracting the salt into an organic solvent, and determining the amount extracted colorimetrically. Interfering material may cause high or low results. Meanwhile, the subcommittee is turning its attention to a suitable method for ABS in sewage, and Sallee notes preliminary results are promising, though no method has been subjected to coopera-
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tive testing yet. And still to be worked out, of course, is a short chemical method suitable for use in any water treatment plant. Air Pollution The study of air pollution in the Southern California area has settled down to a methodical collecting of data from which action may be taken to help correct conditions. M. D. Thomas, Stanford Research Institute, reviewed techniques and instruments used and described an automatic recorder for total oxidants using potassium iodide reagents and measuring liberated iodine. Ozone is determined separately by a continuous ultraviolet method. Ferrous thiocyanate reagent is sensitive and reasonably specific for oxides of nitrogen. Unfortunately, the agreement is not good between the ultraviolet method for ozone and the chemical methods, but further study, it is hoped, will reconcile the different methods. Carbon monoxide is determined best by infrared and olefins by electrolytically generated bromine using the Titrilog instrument to do this automatically. Research is proceeding at the Stanford Research Institute on the development of an instrument for recording hydrogen fluoride content of air. Sufficient progress has been made on the method, and the laboratory instrument is far enough along to guarantee the instrument will give precise data. J. W. Kemp, Applied Research Laboratories, speaking about rapid methods of analysis, said that optical spectrographic analysis has been recognized as a high-speed routine control method for 20 years and direct reading techniques have been added to this approach for the past 10 years. At present x-ray fluorescence technique is going through its acceptance period as a highspeed method. It is restricted in general usefulness to those elements with atomic number greater than 19. While these methods are faster than conventional wet methods, they require considerable outlay of capital, the speaker said, so that a large volume of work must be handled to justify money involved. Drug Assay An interesting discussion of the problems involved in the assaying of drugs in biological material was presented by Bernard B. Brodie, National Institutes of Health, Bethesda, Md. Early in their research they recognized that many drugs could be determined by fluorescence in the ultraviolet. The early sources, of course, were restricted as to wave length and so the method was not of wide application. ANALYTICAL
CHEMISTRY
NEWS With the development of the xenon high intensity lamp, which could pro duce fluorescence at all wave lengths, they set to work to build an instrument which could utilize this new source and thus extend the method. The speaker described the early instrument and the useful application which it now makes possible in their studies on biological materials where the determination of drugs is necessary. As a result of their basic instrument research, commercial spectrofluorometers are now manufac tured by American Instrument Co. and Farrand Optical Co. Instrument Exhibits A wide variety of analytical instru ments were exhibited by Applied Physics, Arnold 0 . Beckman, Beckman Instruments, Braun, Central Scientific, Consolidated Electrody namics, Harold Kruger, Nuclear In strument & Chemical, and PerkinElmer.
SE Texas Analytical Group Officers The Southeastern Texas Analytical Group has elected the following officers: J. H. Karchmer, Humble Oil Co., Bav-
town, chairman; E. R. Wright, Dow Chemical Co., Freeport, chairman-elect; W. F. Hamner, Monsanto Chemical Co., secretary; Gordon 0. Guerrant, Shell Development Co., treasurer. Directors are C. H. Beckworth, M. L. Owens, T. J. Eobichaux, and L. C. Shepard.
tary Engineering Center. The U. S. Geological Survey has been elected to membership. F. W. Gilcreas is chair man, A. Thurn vice chairman, and C. K. Rice, Refinery Technology Laboratory, Gulf Oil Corp., P.O. Box 7409, Phila delphia 1, Pa., secretary.
Methods of Water Examination
X-Ray Applications Scheduled for Denver Meeting
The Joint Committee on Uniformity of Methods of Water Examination has been formed to secure uniformity of con tent of methods by providing a mecha nism for exchanging information among members, securing uniformity of termi nology, and reviewing methods for natural water, potable water, industrial water, industrial waste water, and sew age. Charter members are : Committee on Disposal of Refinery Wastes, American Petroleum Institute; American Public Health Association; American Society for Testing Materials; Association of Official Agricultural Chemists; Federa tion of Sewage and Industrial Waste Associations; Manufacturing Chemists' Association; Technical Association of the Pulp and Paper Industry; and TJ. S. Public Health Service, R. A. Taft Sani
A wide variety of industrial applica tions of x-ray analysis will be presented at the 5th annual symposium on this subject to be held at Denver, August 9 to 10. Sponsor is the Metallurgy Divi sion, Denver Research Institute, Uni versity of Denver. Thursday morning the papers deal mainly with x-ray spectroscopy, three being given by makers of equipment and three by research laboratories. This subject is receiving a great deal of at tention because it is specific for the ele ments present. It will prove of value in the metallurgical field and permits under carefully controlled conditions the determination of trace elements. In the afternoon the theme is mainly de voted to x-ray diffraction. Friday morning is devoted to com-
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mereial computers and counters applied to the general x-ray field. In the after noon the general papers cover x-ray fluorescent analysis and x-ray spectros copy, the program closing with a paper on x-ray anah-sis with proportion counters. For those who want a concentrated evaluation of x-ray analysis, this is the best conference of the year. The equip ment manufacturers are presenting one quarter of the 24 papers. There is a strong representation of government laboratories and research foundations, all of which are doing pioneering work in this field. The Bureau of Mines is strongly represented at the conference, as would be expected because chemical wet methods for mineral analysis are slow and cumbersome. The registration fee of $10 includes the dinner on August 9. Subject of the dinner address will be "World Affairs and Their Effect on the Scientific World." Abstracts of papers will be available at the meeting. Special events include a ladies' pro gram and several sight-seeing tours. Further details, including copies of the program, are available from the Metallurgy Division, Denver Research Institute, University of Denver. Denver 10, Colo.
Symposium on Combustion The Sixth International Symposium on Combustion, to be held at Yale University, New Haven, Conn., August 19 through 24, will hold a session on experimental and analytical techniques in combustion, including an invited paper by I. I. Warshawsky on "Meas urements of High Temperatures."
toria Museum Building, Ottawa, On tario, Canada.
Nerve Gas Analyses on Atlantic City Program A series of papers on the detection and analyses of "nerve gases" will be in cluded in the Symposium on Air Pollu tion at the Atlantic City meeting of the AMERICAN CHEMICAL SOCIETY.
Symposium on Applied Spectroscopy The Third Ottawa Symposium on Applied Spectroscopy, sponsored by the Ottawa Valley Section of the Canadian Association for Mines and Technical Surveys, will be held in Ottawa Septem ber 12, 13, and 14. Papers are invited on applied emission spectroscopy and closely related fields of instrumental analysis. Papers on problems of stand ardization and standard samples are particularly welcome. Information as to title, author's name and address, approximate time for presentation, and a short abstract should be sent by July 27 to W. H. Champ, Geological Survey Branch, Department of Mines and Technical Surveys, Vic
This symposium, sponsored jointly by the Divisions of Analytical Chemistry and Industrial and Engineering Chemis try, and the ACS Committee on Air Pollution, will cover a four-day period, September 17 to 20. The symposium will cover field studies of air pollutants, kinetics and related fundamental studies, biologic effects and techniques, and detection and analyses of pollutants. The chairman is Joseph W. E. Harrisson, LaWall and Harrisson; cochairmen are Kingsley Kay, Depart ment of National Health and Welfare (Canada) ; and Solomon A. Love, Army Chemical Center, Md. Other programs of interest to analysts will be a Symposium on New Methods for Analytical Characterization of Cel lulose, sponsored by the Division of Cellulose Chemistry, on September 18
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Pittsburgh Diffraction Conference The Fourteenth Annual Pittsburgh Diffraction Conference will be held October 31, to November 2 at Mellon Institute, Pittsburgh, Pa. The con ference will emphasize small-angle scat tering, high and low temperature dif fraction studies, structural aspects of solid state physics, instrumentation
ANALYST'S CALENDAR
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is simultaneously cooled by a stream of
and 19. In this connection there will be meetings on September 17 of the Com mittee for International Analytical Methods for Cellulose, Section Chair men of ASTM Committee D-23, and the Subcommittees of the ACS Committee on Standards and Methods of Testing Cellulose. The final program of the Analytical Division will be published in ANALYTICAL CHEMISTRY prior to the meeting.
· N h W YORK 10, Ν. Υ.
Ν
Tt.i-rpt Y 1-3444
Sixth Annual Infrared Spectroscopy In stitute. Nashville, Term., August 29 to September 2. Eleventh Annual Instrument-Automation Conference and Exhibit. I n s t r u m e n t Society of America. N e w York, Sep t e m b e r 17 t o 2 1 . Fifteenth International Congress of Pure and Applied Chemistry. Analytical Chemistry. I n t e r n a t i o n a l Union of P u r e a n d Applied Chemistry, Lisbon, Portugal. September 9 t o 16. Eleventh Annual Calorimetry Conference. J o h n s H o p k i n s University, Baltimore, M d . . September 14 and 15. American Chemical Society. 130th meeting, Atlantic City, N . J., Septem ber 16 t o 2 1 . American Society for Testing Materials. Second Pacific Coast n a t i o n a l meeting, H o t e l Statler, Los Angeles, Calif., September 16 to 22. American Society for Quality Control, New E n g l a n d Sections. Springfield, Mass., October 3 t o 5. Fourteenth Annual Pittsburgh Diffraction Conference. Mellon I n s t i t u t e , P i t t s burgh, Pa., October 31 t o N o v e m b e r 2. Society for Experimental Stress Analysis. Columbus, Ohio, N o v e m b e r 1 a n d 2.
For further Information, circle numbers 24A-1, 24 A-2, 24 A-3 on Readers' Service Card, page 53 A
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ANALYTICAL
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NEWS and methods, and neutron diffraction. Program chairman is A. Taylor, Westinghouse Research Laboratories, Beulah Road, Pittsburgh 35, Pa.
Southwide Conference in December The Southwide Chemical Conference to be held in Memphis, December 6 to 8, will include papers in analytical chem istry. Rules governing presentation of pa pers at ACS meetings will prevail. These require that the author or coauthor be an ACS member. Papers will be limited to 15 to 20 minutes. Five copies of a 100-word abstract must be submitted by September 21 to E . C. Markham, University of North Carolina, Chapel Hill, N . C. Any additional details are available from Dr. Markham.
Microchemical Journal The Metropolitan Microchemical So ciety plans to issue the first number of its proceedings (Microchemical Journal) about Oct. 1, 1956. Eventually four numbers of the journal will be issued per
year. The society invites contributions in all phases of microchemistry, includ ing critical review articles. Articles should be sent to Editorial Committee, Microchemical Journal, Department of Chemistry, Brooklyn College, Brooklyn 10, Ν . Υ. The editorial committee con sists of A. A. Benedetti-Pichler, T. S. Ma, John A. Means, A. G. Mistretta, and Bella Rosenfeld. Interscience Pub lishers, 250 Fifth Ave., New York, Ν. Υ., will handle distribution and pro motion.
NEW BOOKS Spectroscopy at Radio and Microwave Frequencies. D. J. E. Ingram, xii + 331 pp. Butterworth Publications, London, England, 1955. 45s. Re viewed by DONALD K. COLES, West-
inghouse Research Pittsburgh, Pa.
Laboratories,
This book outlines developments in gaseous microwave spectroscopy, elec tron paramagnetic resonance, and nu clear resonance since their inception about 10 years ago. Ingram stresses the similarity and interrelation of these three parts of spectroscopy, as well as
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their general setting in spectroscopy as a whole. While the chief equations of each subject are set forth and explained, detailed mathematical treatment is avoided. Thus interpretation of the results should be clear to those without specialized knowledge of quantum me chanics. Those wishing to set up spec troscopes will find much useful informa tion, since the design of experimental apparatus is discussed in detail. The various applications of micro wave and radiofrequency spectroscopy are considered in the last chapter, in relation to both fundamental research and determinations of a more practical nature. While the discussions on chemi cal analysis by radiofrequency and gase ous microwave spectroscopy are very brief, the discussion on chemical analy sis by paramagnetic resonance is excel lent. In addition to the section on analysis of elements and compounds which possess an unpaired electron, sec tions are included on the detection of free radicals, the study of photochemical reactions, irradiation damage, and gas discharges. In conclusion Ingram sug gests that if any physical or chemical system possesses unpaired electron spins, then sooner or later the techniques of electron resonance will be applied to obtain exact and detailed information. References on experimental appa ratus, theory, and results are liberal except, perhaps, to other books in this field. The book is well written and appears to be relatively free of errors. Its broad approach should appeal to many research workers and students who would like to obtain a general pic ture of the methods and applications of this part of spectroscopy.
Introductory
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Quantitative
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A. R. Olson, C. W. Koch, and G. C. Pimentel. χ + 442 pp. W. H. Free man & Co., San Francisco, Calif., 1956. $5.00. Reviewed by ROY A. WHITEKER, Massachusetts Institute of Technology, Cambridge, Mass. This new textbook of quantitative analysis differs in both style and ap proach from most of the current texts. It includes the contents of Olson, Orlemann, and Koch's "Introductory Quan titative Analysis," and retains their emphasis on fundamental principles and techniques but with a considerably broader scope. In addition to covering conventional quantitative topics, chap ters on the evaluation of data, separa tion principles, and physicochemical methods, principally colorimetiy, are included. As this book is designed as a teaching aid rather than as a reference book, only a limited number of experiments are included. These are planned to inANALYTICAL
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No. 2070
Designed for the rapid and accurate determina tion of thiamin, riboflavin, and other substances which fluoresce in solution. The sensitivity and stability are such t h a t it has been found particularly useful in determining very small amounts of these substances.
KLETT SCIENTIFIC PRODUCTS ELECTROPHORESIS APPARATUS · BIO-COLORIMETERS GLASS ABSORPTION CELLS> COLORIMETER NEPHELOMETERS · GLASS STANDARDS · KLETT REAGENTS
Klett
Manufacturing Co.
179 EAST 87TH STREET, NEW YORK, Ν. Υ. For further information, circle numbers 28 A-1, 28 A-2 on Readers' Service Card, page S3 A
28 A
volve the student in the actual design of quantitative experiments. In all cases the requisite principles and techniques are discussed first. The detailed direc tions of the early experiments are inter spersed with questions to point out the application of these principles. Later, more and more discretion is left to the student, until finally, he may work out every phase and detail of his procedures. This approach necessitates a rather rigid adherence to the topical order of the text, but it does appear to be a worth while teaching technique, unless the student becomes too bogged down in the minutiae of determining satisfactory ex perimental conditions. In general, the treatment of principles is excellent; the discussion of polybasic acids is outstanding. The procedure for the ion exchange separation of copper and cobalt, however, is somewhat con fusing. The chapter on "Volumetric Techniques" might be presented more logically by including experimental procedures with the appropriate discus sions. Explicit experimental directions should not be necessary for determining the Kip of silver thiocyanate, but it seems doubtful that the student can treat his data appropriately, under standing the assumptions and approxi mations involved, from the limited dis cussion given. The inclusion of witty comments and analogies throughout the text may not be appealing to some, but this style may be justified, as the product is well written, extremely readable, and en joyable. This text is certainly a worth-while addition to the literature of analytical chemistry, and its approach should be carefully considered by everyone en gaged in the teaching of "quantitative chemistry."
Chemisorption. B. M. W. Trapnell. vii + 265 pages. Academic Press, 125 East 23rd St., New York 10, Ν. Υ., 1955. $6.80. This book is designed to give a bal anced presentation of the subject of chemisorption, in particular of discover ies made over the past 15 years, but hitherto available only as original pa pers scattered over many journals. The main part of the book, concerned with chemisorption itself, treats veloci ties of adsorption and desorption, equi librium at surfaces, heats and mecha nism of adsorption, and the mobility of adsorbed layers. In the last two chap ters the causes of catalytic specificity are discussed, together with the mecha nisms of some simple catalytic reactions, including olefin hydrogénation and the cracking of hydrocarbons. ANALYTICAL
CHEMISTRY
