REPORT FOR A N A L Y T I C A L CHEMISTS
Modern Analytical Chemistry.
A Subjective View
by H. A. Liebhafsky
General Electric Research Laboratory, Schenectady, Ν. Υ.
T
HE growth of instrumental analysis and the making of in struments for analysis chiefly dis tinguish modern analytical chem istry from that of yesterday. The difference is small in time, but revolutionary in character. W h a t Is Modern Analytical Chemistry?
This is to be a subjective look at our common discipline, and I shall take as my keynote Like it or not, the chemistry is going out of analytical chemistry (14). Some may feel that this keynote does not "Ac-cent-tchu-ate the pos-i-tive" or 'Έ-lim-my-nate the neg-a-tive," (20) but at least it does stay away from "Mis-ter In-be-tween." Well, what is this analytical chemistry that "chem istry is going out of," that physics, electronics, and engineering are entering? Today, when rapid change seems slow and revolution is the norm, anyone saddled with the task of defining a scientific discipline is al most driven to saying with Humpty-Dumpty : "When I use a word, it means just what I choose it to mean—neither more nor less." And in defining analytical chem istry, one is tempted to paraphrase Voltaire's remark about a certain celebrated institution, that it was "neither holy, nor Roman, nor Em pire." But even if one agrees that modern analytical chemistry is not necessarily either analytical or chemistry, it is important then to pull up short. For "Roman Em pire" suggests "Decline and Fall," the complete antithesis of what faces analytical chemistry today. In 1950, Kolthoff (13), the dis tinguished recipient of this Award, began his address by saying
chemistry are to determine the compo sition of any complex compound, or mixture of compounds. From a university point of view of 12 years ago, this is an excellent definition. But look now at the 1961 Presidential Address delivered to the Society of Analytical Chem istry by Chirnside (6), whose career somewhat resembles my own. In this address, entitled "The Enlarge ment of Horizons in Analytical Chemistry," which is required read ing for us all, Chirnside quotes Ε. Β. Hughes as having defined our dis cipline to be: "the examination of a material to ascertain its composi tion, its properties, its qualities." Then Chirnside suggests "that the greatest of these is no longer nec essarily composition," which ex plains in part why "the chemistry is going out of analytical chemis try." Merely to drive the point home with an absurd example, let me say that there is less and less tendency in modern analytical chemistry to subject the vermiform appendix to ultimate analysis in order to establish what kind of ap pendicitis caused a particular stom ach ache. Somewhat hesitantly I suggest to you that Hughes' definition also has become too restrictive. Having de cided to take this plunge, I was heartened by much of what Ralph Muller wrote in his Instrumentation
column in the December 1961 issue of our journal (21). I see modern analytical chemistry as the char acterization and control of ma terials—no more, and certainly no less. Characterization (9) is in tended to embrace all three ele ments of Hughes' definition. Con trol includes modifying as neces sary, and usually "in-line," the characteristics of a material. We are much farther on the road to characterization than on the road to control. Control implies sensors, error signals, servo links, computers, and automation. Consider only one sensor, an x-ray detector. Even today, x-ray absorption can be used in the automatic control of steel strip and of the coinage ; x-ray emis sion can serve similarly to control the treatment of minerals and the manufacture of cement. And if you tell me that such characterization and control of materials don't sound like analytical chemistry, then let me remind you of Voltaire and the Holy Roman Empire! Let us leave control to the future and content ourselves today with characterization. To oversimplify: Characterization means more phys ics and less chemistry. More phys ics in turn means more instruments, and more instruments mean a higher proportion of individual determina tions, and a lower proportion of complete analyses.
This Report for Analytical Chemists is the text of the Fisher Award Address given at the recent national ACS meeting in Washington. The recipient, Dr. Herman A. Liebhafsky, in his subjective view of modern analytical chemistry, has presented thoughts which may or may not coincide with those of the majority of analytical chemists. Depending on the nature of the response to this article, the editors will consider summarizing comments received in the form of another Report for Analytical Chemists in a later issue. Any comments should be sent to the Editor, ANALYTICAL CHEMISTRY, 1155 16th St., N.W., Washington 6, D . C .
The aims and objectives of analytical VOL. 34, NO. 7, JUNE 1962
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There is another way of looking at the situation. Mellon (18) described the older analytical chemistry as consisting of separation preceding determination: separation usually involving chemistry, determination being based on physics. If we adopt characterization as the essence of modern analytical chemistry, then separation needs replacing by the broader preparation, a change made necessary by the decreasing emphasis on ascertaining composition. Two trends are noticeable: toward less chemistry in the preparation, and toward less preparation prior to the determination, determinations being made more and more upon the original sample. These trends are nothing new—witness the characterization of polymers. Separations involve less and less the actual handling of welldefined chemical compounds—witness chromatography of all kinds, and the use of ion-exchange resins. The 1962 review of x-ray methods (15) contains 81 references to the determination of iron by x-ray emission spectrography. In almost three fourths of these cases, sample preparation did not involve chemical treatment. Elving (8) has indicated that organic analysis will not escape the revolution in analytical chemistry. Organic analysis carried out on a large scale may be the first to feel the impact of a new concept the computer has made possible (22). This is the concept of an "analytical spectrum," which is a new name for a set of determinations intended to characterize a sample. The computer lets us choose such a set relatively unhampered by considerations such as cumbersomeness in calculating results, lack of specificity in the determinations, added cost of redundant measurements, and absence of linear response. I t is good to know that our 1962 Summer Symposium will deal with applications of computers in analytical chemistry. Analytical Chemistry as a Services Activity
Analytical chemistry enjoyed a golden age when chemistry was young. But let us listen to W. F.
REPORT FOR ANALYTICAL CHEMISTS
Hillebrand
(12), an old master:
In the early days of chemistry there was needed a vast accumulation of observations to serve as foundations for the development of the science. At the very basis lay the need for knowledge of the composition of all kinds of matter. Hence, it came about that many, if not most, of the great chemists of the time were of necessity analysts, and the analytical branch of chemistry stood in high repute. That this condition did not maintain itself, that chemical analysis during the latter half of the past century fell from its high estate and came to be looked upon more or less as a handy tool for ulterior ends, a tool, moreover, which need not for most purposes be of the sharpest or the best or entrusted only to the most careful and skilled operators—all this has been recognized and lamented by many. It is clear in retrospect that a decline in prestige had to come. Once methods of ascertaining composition had been developed and applied to show in rough outline of what the world is made, familiarity began to take its toll. The finding that Iceland spar is calcite is calcium carbonate came tô be less celebrated than Gertrude Stein's discovery about the rose. The decline was accelerated in industry by a tendency to continue ascertaining composition in cases where other information would have been a better basis for action (6). I think
the decline was accelerated further by a tendency to worship high precision, to use it as an opiate that induced a feeling of security, and to disregard the difficult and embarrassing question of accuracy. Nowhere is this situation presented better than in the memorable address, "The Chemical Analysis of Things as They Are," given by the 1949 Award Winner at a Washington meeting of our Society 29 years ago almost to the day. In this address, Lundell (16) also mentioned that an analyst "must be an expert manufacturer of pure chemicals," which points up the close relationship between analytical chemistry and standards, and between analytical chemistry and atomic weights. Although the revolution in analytical chemistry affects the demand for standards, standards will continue to be important if only because most of the instrumental methods are merely comparative. Atomic weights are another story. Anyone who reads Scott's recent critique of the Harvard method for determining atomic weights (23) must agree that these atomic weights resulted from superlative scientific work. Yet these atomic weights are going the way of much of the older analytical
chemistry. Atomic weight determinations now belong to physics, to chemistry no more. For. me, the 1961 Table of Atomic Weights, in which oxygen is listed as 15.9994, marks the end of an era (5). A decrease of 6 parts in 160,000 is not much, yet as Mercutio says, 'tis not so deep as a well, nor so wide as a church-door; But 'tis enough, 'twill serve. We are confronted by a paradox. If we can believe our elders, the prestige of analytical chemistry is now lower than in its golden age, but the discipline is more important than ever before. This importance is taken for granted in industry, but it extends beyond industry into many fields of research. For example, the characterization of materials is an indispensable part of the life sciences (17) and of nuclear chemistry. Analytical chemistry as we have defined it scored perhaps the greatest success of its history in 1939 when Hahn and Strassmann (10) identified the alkaline earth they had produced upon bombarding uranium with neutrons. When Hahn was asked at Berkeley whether he realized that their work had brought on the atomic age, I heard him reply about like this: "Absolutely not. We only wanted
Herman A. Liebhafsky, recipient of the 1962 Fisher Award in Analytical Chemistry, is the first industrial scientist to receive this award. Dr. Liebhafsky is manager of the physical chemistry section of the General Electric Research Laboratory, the Knolls, Schenectady, Ν. Υ. He was born in Zwittau, AustriaHungary, and was educated at Texas A&M, University of Nebraska, and the University of California. He re ceived his Ph.D. from the last in 1929. He also taught there for several years before joining GE. He has published many papers in all phases of physical, analytical, and inorganic chemistry and has been is sued five patents.
VOL. 34, NO. 7, JUNE 1962
REPORT
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to prove to the physicists that what we had was barium and not ra dium." Had it been radium, Hahn and Strassmann's work would have been far, far less significant. The actual curtain raiser for the atomic age was thus the identification of barium, an operation not unknown to analytical chemists. But, back to our paradox. I sug gest that the paradox disappears when one takes into account the profound change that has occurred in the character of analytical chem istry. In the golden age of the last century, our discipline was, to a much greater extent than now, a research activity; in those days, great prestige accrued even if the activity produced no more than new knowledge of analytical meth ods. Nowadays, our discipline is mainly what in General Electric is called a Services activity (7)—an activity that can be justified only if it makes its major contribution to an activity outside itself. Few of us do analytical chemistry just for fun! The paradox is explained as fol lows: Analytical chemistry has lost prestige as a research activity and has not yet gained prestige commen surate with its great and growing importance as a service in industry. To gain this prestige, we must ac cept its status as a service, we must envision modern analytical chem istry as the characterization and control of materials, we must lay claim to most ways of accomplish ing this broad and indispensable function, and we must let those out side our field know what we are doing. It is easy to gain the impression that those performing a Services function are somehow below the salt. This is nonsense, as the Four Horsemen in the Notre Dame backfield soon learned when the Seven Mules in the line decided to demon strate the value of Services by simply getting out of the way. The General Electric Co. has a threepart structure (7) consisting of the Executives, the Services, and the Operating components. Those of us engaged in analytical chemistry in Research Services thus provide a service for a Service, and yet we have no difficulty in holding up our
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REPORT FOR ANALYTICAL CHEMISTS
Table I. Contributions to Analytical Chemistry from Nobel Prize Researches Laureates Marie Curie T. W. Richards F. Pregl T. Svedberg P. Debye G. de Hevesy A. Tiselius A. J. P . Martin and R. M. Synge J. Heyrovsky W. F . Libby M. Calvin W. K. Roentgen A. H. Becquerel and the Curies M. von Laue W. H. Bragg and W. L. Bragg C. G. Barkla K. Siegbahn C. V. Raman C. J. Davisson and G. P . Thomson F. Bloch and E. M. Purcell F. Zernike
Contributions Chemistry Radioactivity as a means of characterization Refinement of classical methods Microanalysis of organic substances The ultracentrifuge Dipole moment as a means of characteriza tion Radioactive tracer techniques Electrophoresis and chromatography as means of characterization Partition chromatography Polarography Radiocarbon dating Refinement of paper chromatography Physics X-rays. X-ray detection. X-ray absorptiom etry Discovery of radioactivity Discovery of x-ray diffraction" The x-ray spectrometer Discovery of characteristic x-ray spectra 1 ' Advancement of x-ray techniques Discovery of the Raman effect Discovery of electron diffraction Nuclear magnetic resonance methods Development of phase contrast microscopy
° A. W. Hull, a physicist, first used x-ray diffraction for the characterization of ma terials. 6 Moseley, a physicist, first envisioned x-ray emission spectrography as a useful analytical method.
heads in the presence of colleagues from any part of the Company structure. Analytical Chemistry and Other Sciences
Once we accept Services status for analytical chemistry, we need feel no chagrin because it feeds on other sciences. If our main job is the characterization and control of ma terials, we cannot be expected to do much of the kind of research that turns up, often by accident, new phenomena that can be used in get ting this job done. We must cheerfully acknowledge our debt to those who do discover these new phenomena. To get an inkling of this debt, I have listed contributions accruing to analytical chemistry from Nobel prize re searches. Table I shows 11 such contributions from chemistry and 10 from physics. I should not classify a single Nobel laureate as primarily an analytical chemist. The devel opment of our important new tool, the x-ray emission electron microprobe, tells the same story. We owe this microprobe almost en
tirely to physicists, among whom I need mention only Hillier, Castaing, Cosslett, Wittry, and Birks in order to make my point. Drawbacks of Modern Analytical Chemistry
Modern analytical chemistry has some obvious and serious disad vantages, such as: ( 1 ) High capital investment (2) Rapid obsolescence (3) Complex maintenance prob lems (4) Relative inflexibility Automated systems in general tend to suffer from these disadvantages, which are consequently attracting widespread attention. A moderately instrumented labo ratory handling some 5000 diversi fied samples annually could easily have $250,000 invested in equip ment, and face write-off charges near $25,000 (or $5 a sample) for instruments alone. Rapid obsoles cence wrould make this a continuing charge. The relative inflexibility of electronic robots makes one shudder at what might happen if weak
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aqueous hydrogen peroxide were given as an unknown to a completely instrumented laboratory. There are less tangible drawbacks also. Unreasonable or uninformed customers are more likely to insist on unnecessary determinations if the laboratory is instrumented. I t will be tempting to agree with such customers in order to keep idle equipment at work. There will be a tendency for analytical chemists to maintain and repair equipment when they might be better occupied. In sum, the instruments m a y t a k e over unless they are kept where they belong. Our situation has much in common with t h a t of the laboratories in our modern large hospitals. The problem of the unreasonable customer is highlighted by the following quotation from an article by a Chief of Hospital Laboratory Service {24): But the ultimate request has just come to hand. It was written by a new and inspired resident. . . .
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His supreme gift to the laboratory was a beaker containing enough blood to fill a beer can, with a laboratory slip demanding 'Complete laboratory workup.' This would call for some 250 tests worth about $1200. I intend to frame this laboratory slip and hang it among my precious mementos. Fully instrumented laboratories are going to be formidable organizations t h a t must have a large and diversified work load if they are to live and prosper. I t would seem to follow t h a t not m a n y institutions can support such laboratories, and t h a t we m a y expect to see commercial laboratories in increasing n u m ber selling the services of the more costly instruments. Also, it will be long before all laboratories are fully instrumented, and longer yet before all one-of-a-kind samples are done without recourse to chemical methods. Chemistry is not about to disappear from analytical chemistry (11), and the ascertaining of composition will be with us for a long time to come.
Determinators, Analysts, and Analytical Chemists More important t h a n analytical chemistry are the people who practice it. They are described by Lun-
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dell {16) as determinators and ana lysts, and this description is a logi cal point of departure. In modern analytical chemistry, determinators are more likely to push buttons and handle chart paper than to read burets, and they will yield ground to maintenance men as automation in creases. For my purposes, I should like to describe analysts as top flight scientists who in their work rely heavily upon books such as those of Noyes and Bray, or Hillebrand, Lundell, Bright, and Hoff man. I respect and admire these two books, and I cite them because I wish to classify as an analytical chemist anyone who places greater reliance upon instruments than these books require. This distinc tion between analyst and analyti cal chemist is as subjective as any one could wish, but it is safely in definite and gratifyingly convenient. In these terms, the character of modern analytical chemistry dic tates a gradual replacement of the analyst by the analytical chemist. The cost of modern instruments, their need for determinators, and the alternative approaches they offer, all put management content into the analytical chemist's job. The analyst is always a functional individual contributor, a term I have borrowed to describe an em ployee of great ability, training, and experience who, in contrast to the professional manager, does not work primarily through others. The ana lytical chemist will come closer to being a professional manager the larger the laboratory he heads. When he works alone, he is of course a functional individual con tributor. Fortunately, we are not called upon to specif}^ at what point he becomes a manager—a delicate and difficult matter.
Analytical Chemistry, Management, and Consulting
We all have something to gain by learning about management as a profession. As such, it has grown in importance until it is recognized even by research-minded institu tions (3). Also, or so it seems to me, a career in modern analytical chemistry could well prepare one to become a professional manager.
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This follows from the management content of almost every analytical chemist's job, but it becomes clearer when we consider, as I was taught 5 years ago, that managing consists of planning, organizing, integrating, and measuring. There is no need to speak of planning and organizing: modern analytical chemistry could not exist without them. Integrating (19) is a process, more mystic than mathematical, by which a manager produces a whole that is greater than the sum of its parts. Let me illustrate with an example from analytical chemistry. The customer wants elements A, B, C determined in a sample by methods he prescribes because he is certain that only these results thus obtained will enable him to understand an unexpected useful discovery—one that Kipling might call "the undoctored incident that actually occurred." The analytical chemist knows that the methods suggested are unsuitable and unloved by his staff, and he suspects that element X may be the key to the problem. If he is able to establish that X is indeed responsible and to suggest that Y might be even better than X, and if he can reach this point at minimum cost, without antagonizing his own staff or the customer, why then he has been integrating ! Surely, analytical chemists need not be told much about measuring, and I shall dismiss it with an analogy drawn from our experience. A manager might make a model of his business, base his decisions on the model, then correct his decisions (and his model) on the basis of experience. In principle, this process resembles controlling the thickness of steel strip on the basis of an error signal supplied by a sensor. Of course, analytical chemistry is simpler than most business, but let us remember that business is accustomed to larger standard deviations. Modern analytical chemistry is closely related also to consulting, which is another service function. The relationship grows out of this: when things go unexpectedly right (as in the "undoctored incident" just mentioned) or unexpectedly wrong (as happens from time to
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time), there has usually been some change in a material, and establishing the nature of this change is the analytical chemist's business. Furthermore, by training, temperament, and experience, the analytical chemist is likely to become the kind of expert upon whom Robert Graves looks with favor in the quotation : Experts ranked in serried rows Fill the enormous plaza full. But only one there is who knows, And he's the man who fights the bull. Training and Status
I am reluctant to touch upon training and status, two subjects about which, to borrow an old quotation {!), "many (have said) much, everyone something, none enough." I do not expect to change the situation. I think the analytical chemist should have broader training than the analyst. Additions to the modern undergraduate curriculum have become impossible, and displacements virtually so. I am afraid, therefore, that methods for the ascertaining of composition will have to be taught primarily for their general educational value, which means that the analytical chemist would spend little more time upon them than other undergraduate scientists or engineers. Modern analytical chemistry would be well served by a closer identity of the undergraduate curricula in science and engineering (4), for the characterization and control of materials cut across many disciplines. What about status? As the scope of modern analytical chemistry continues to broaden owing to the annexation of methods for characterization and control, its prestige will grow. Anything we do to promote this process will improve, though slowly, the status of the analytical chemist. As an individual, he can take action more directly. If he takes advantage of his position to develop as a manager or as a consultant, if he concerns himself with the end toward which his determinations are the means, he will be prepared to change careers if he thinks his status unsatisfactory. Or, always provided he stays scientifically alive, he can find solace in other fields for example,
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* Ref. Analytical Chemistry, 3 3 , 1138 (August 1961).
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ANALYTICAL CHEMISTRY
Modern analytical chemistry, viewed as the characterization and control of materials, and managed by broadly trained men and women, could be a unifying force to counter act the splintering and specializa tion t h a t burden science today. As another unifying force, M a terials Science comes immediately to mind. A perceptive analysis of this newly created field says in part (β) : To one who moves around Washington today in the quest for funds to support University research, or indeed to those who visit the metallurgy and ceramics departments of our foremost universities and institutes of technology, the term 'materials science' is an O.K. word. Of course, not even government fi nancing can make the Fermi level significant for polymers or the mo lecular weight distribution impor t a n t for alloys. B u t any a t t e m p t at unification is welcome, and es pecially an a t t e m p t t h a t rests es sentially upon characterization of materials. In accord with the times, we may someday be calling analytical chem istry "materials characterization and control/' but I am too fond of the present name, and of adjectives where they belong, to suggest t h a t now. Conclusion
Let me be really subjective in closing. As a reserve officer, I lived through the mechanization of the field artillery. With this painful but necessary process, the current revolution in analytical chemistry has much in common, emotionally and factually, for mechanization re sembles instrumentation or automa tion. I believe it is foolish to resist such revolutions and sensible to turn them to good account. If modern analytical chemistry suffers at all, it suffers because the charac terization and control of materials is too big an assignment for a single discipline. If this is so, we m a y surely say of analytical chemistry what the National Archives Build-
REPORT
ing says of the nation: "What is past is prologue!" Literature Cited (1) Adams, F . D., "The Birth and D e velopment of the Geological Sciences," p. 124, Dover Publishers, New York, 1954. (The inscription "De hoc multi multa, omnes aliquid, nemo satis" is said to have been engraved on a meteorite subsequent to its fall in 1492.) (2) Bell, M. E., Mineral Ind. (Coll. Min eral Ind., Penn. State Univ.) 31, 1 (October, 1961). (3) Bull. California Institute of Tech nology 70, No. 3, 105 (1961). (4) Ibid., pp. 117, 126, 219, 224, and 225. (For undergraduate curricula showing a welcome degree of identity for engi neering and the sciences.) (5) Chem. Eng. News 39, 43 (Novem ber 20, 1961). (6) Chirnside, R. C , Analyst 86, 314 (1961). (7) Cordiner, R. J., "New Frontiers for Professional Managers," pp. 64, 69, Mc Graw-Hill, New York, 1956. (8)
Elvmg,
P.
J.,
ANAL.
CHEM.
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1538 (1960). (One must agree with Elving that "instrumental analysis" ought not to mean all things to all chemists—in particular, it cannot be regarded as synonymous with "analyti cal chemistry.") (9) Gould, C. W., Ibid., 28, 777 (1956). ("Characterization" as used here is un fortunately too broad for precise defi nition, and t h e word has become closely associated with organic chemis try. But the author could find no good alternative.) (10) Hahn, O., Strassmann, F., Naturwissenschaften 27, 11, 89 (1939). (11) H a l l e t t ,
L.
T.,
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CHEM.
33,
1633 (1961). (12) Hillebrand, W. F., Ind. Eng. Chem. 9, 170 (1917). (13) Kolthoff, I . M., Chem. Eng. News 28, 2882 (1950). (14) Liebhafsky, H . A , Pfeiffer, H . G., Winslow, E . H., Zemany, P . D., " X Ray Absorption and Emission in Analvtical Chemistry," p . vii, Wiley, New York, 1960. (15) Liebhafsky, H . A , Winslow, Ε . Η , Pfeiffer,
H.
G.,
ANAL.
CHEM.
34,
282 R (1962). (16) Lundell, G. E . F., I N D . E N G . C H E M . , ANAL. E D . 5, 222 (1933). (17) Mason,
W.
B.,
ANAL.
CHEM.
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23 A (March, 1962). (18) Mellon, M . G , Ibid., 24, 924 (1952). (19) Meltcalf, H . C., Urwick, L , e d s , "Dynamic Administration: T h e Col lected Papers of Mary Parker Follett," Harper, New York, 1940. (20) Mercer, Johnny, Arlen, Harold, Song "Ac-cent-tchu-ate T h e Positive," Edwin H . Morris & Co., New York, 1944. (21) Millier,
R.
H.,
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CHEM.
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123 A (December, 1961). (22) Savitzky, Α., Ibid., p. 25 A. (23) Scott, À. F., Ibid., p . 23 A, (August, 1961). (24) Wilens, S. L., Harper's Magazine 244, 78 (February, 1962).
CEC
RECEIVED for review April 2, 1962. Accepted April 2, 1962. Fisher Award Address. Division of Analytical Chemistrv, 141st Meeting, ACS, Washington D . C., March 1962. Circle No. 34 on Readers' Service Card VOL. 34, NO. 7, JUNE 1962
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