Analytical Chemistry in Great Britain - ACS Publications

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REPORT FOR ANALYTICAL

CHEMISTS

Analytical Chemistry in Great Britain R. C. CHIRNSIDE, F.R.I.C.

The General Electric Co. Ltd., Central Research Hirst Research Centre, Wembley, England

r n i i i s CONTRIBUTION was originally -I intended as a commentary on an earlier article in these columns by Dr. Warren Brandt headed "Analytical Chemistry in Europe'' (December 1958) following a six months' residence at Oxford, during which time he also visited a few of the larger industrial and government laboratories in England. In seeking to comment on and to fill in the picture presented by Brandt, it became evident that after this interval one might more profitably discuss factors common to developments in analysis in Great Britain and the U.S.A. rather than to concentrate on such minor differences as may exist, for example, in the academic curricula. It is my purpose to suggest that, with the advent of new techniques of analysis or examination, many of a physical nature, and with the new kinds of information which some of these techniques provide, a new and broader conception of what constitutes analysis is now both possible and desirable. This new philosophy has been developed, both in Great Britain and the U.S.A., mainly in the context of industrial research. It is here that the inadequacies of conventional chemical analysis have been disclosed and where analysts so often failed to identify and to measure the properties of materials that are of most importance. For too long the analytical chemist, and his client, have been content to believe that figures representing chemical composition could be transmuted by mathematical skill into a satisfying statement of physical properties. It

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is, in my view, against this background that the status of analytical chemistry in the two countries should be examined. In both countries much is written and spoken about analytical chemistry, the analyst, and his training. In both countries these subjects have been discussed intensively only in the last 15 years. Interest has been re-awakened only after a long period of relative neglect, particularly in academic circles. In the U.S.A. the annual Pittsburgh Conference presents accounts of exciting developments in techniques of analytical chemistry to a large audience and the American Chemical Society Division of Analytical Chemistry has before it twice a year about 100 papers on a wide range of analytical topics. In Western Europe there have been major international congresses on analytical chemistry since the war, in Utrecht in 1948, Graz, 1950; Oxford, 1952 ; and on gas chromatography in Amsterdam in 1958. In Britain the Society for Analytical Chemistry sponsored a congress on Modern Analytical Chemistry in Industry at the University of St. Andrews in 1957 and an International Symposium on Microchemistry at the University of Birmingham in 1958. In 1960 the Society organised an international meeting in Edinburgh jointly with the Gas Chromatography Discussion Group, and later in London another symposium, international in character, on the determination of gases in metals. This meeting was organised jointly with the Iron and Steel Institute and the Institute of VOL. 33, NO. 12, NOVEMBER 1961

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Metals. Several well-known chem­ ists from the U.S.A. contributed to the proceedings. In 1956 and 1959 a summer school in analytical chemistry, organised by the Royal Institute of Chemistry and the Society for Analytical Chemistry, took place at the Uni­ versity of London and on each occa­ sion applications greatly exceeded places available. A third summer school is to be held in Manchester in 1962. Analytical Groups in Universities

During his short stay at Oxford in 1958 the extent of these activities not unnaturally escaped the notice of Dr. Brandt. He properly drew attention in his report (1) to the dearth of analytical groups in British universities. Whether his comment that "this undoubtedly has its effect on national thinking about analytical chemistry" is wholly justified, is more open to question. There are now two Chairs of Ana­ lytical Chemistry in Great Britain, one at the University of Birming­ ham and one at Queen's University, Belfast. This compares unfavour­ ably with the relatively larger num­ bers of professors in the universities of the U.S.A., but such informa­ tion as is available suggests that this disparity does not properly rep­ resent the respective healths of ana­ lytical chemistry in the two coun­ tries; indeed, it is rumoured that there is currently some concern in the U.S.A. about the academic situ­ ation. Analytical Groups in Government and Industry

What is the situation in industry and in government service? It is

doubtful if the over-all position differs very greatly in the two coun­ tries. Any attempt at a genuine comparison would immediately in­ volve us in a number of considera­ tions—of what we mean by analysis as distinct from control testing— whether we are talking about works laboratories or research laboratories —the nature and degree of scien­ tific intelligence of the industry con­ cerned. It is my purpose therefore not to compare and contrast the present status of analytical chemistry in the two countries but, instead, its position in either to that of, say, 30 years ago. Status of Analytical Chemistry

That the universities have turned their attention again to analytical chemistry after a long period of neglect is obviously welcome and must give cause for satisfaction, even if in Great Britain it is tem­ pered for some by the fact that this has come, if not too late, certainly at a time when the subject has be­ gun to cross new frontiers. There are other dangers of course. Those in the universities would be un­ wise to assume that the analyst in industry is a benighted creature, steeped in empiricism and sadly in need of theoretical enlightenment. That distinguished figure in analyt­ ical chemistry, G. E. F. Lundell, in his now classic paper on "The Analysis of Things as They Are" (10), pointed out how near Ostwald came to making this mistake. Brandt, in his article, says of Brit­ ish industry—"some supervisors ex­ pressed a hope that some day they would be able to employ men

Mr. R. Clark Chirnside is Chief Chemist and Head of the Chemistry and Technical Services Division at the Central Research Laboratories, Hirst Research Centre of The General Electric Co. Ltd., Wembley, England. He is immediate Past-President of the Society for Analytical Chemistry and was Chairman of Analytical Abstracts from their inception in 1953 to 1959. He has been a Vice-President of the Royal Institute of Chemistry and is an Examiner for their Diploma in General Analytical Chemistry. He has taken a prominent part in the activities of the International Union of Pure and Applied Chemistry and served as Vice-President of Section V from 1953 to 1957. He was Honorary Secretary of the Inter­ national Congress on Analytical Chemistry held at Oxford in 1952. He has been a member of the British National Committee for Chemistry, and is a Governor of Brunei, one of the new Colleges of Advanced Tech­ nology.

trained with the analytical view­ point." This seems a more realistic objective than that implied in his statement—"there is never an ana­ lytical chemist graduated by these (Oxford and Cambridge) universi­ ties." It is only too common for the in­ dustrialist in this country to find that the new graduate's conception of what constitutes analytical chemistry and what an analytical chemist, is 30 years out of date. He will almost certainly declare a wish to engage in research and he will, with equal certainty, eschew the thought of anything that savours of routine, as if there was not an es­ sential element of routine in every aspect of professional, scientific, and artistic life. One is tempted to ask if the universities, turning again to analytical chemistry after a gen­ eration of neglect, may not have overlooked in some degree the fact that in the meantime analytical chemistry itself has not been stand­ ing still. Indeed, there can be no static or permanent conception of what constitutes analytical infor­ mation nor any artificial restriction of the methods or techniques used to obtain that information. Seen in retrospect, the golden age of classical analysis was concerned in large measure with charting the composition of much that goes to make up our material world. The present structures of chemistry, geology, and some other sciences were greatly indebted to the vast collection of basic information thus established. Later, the emphasis shifted to the commercial examina­ tion of materials by analysis or test, to control a process, to fix a price,

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" I n t h e United States during the past 15 years," said D r . Brandt, "analytical chemists have witnessed a revolution which has raised their status so t h a t they are now considered equal to other members of the research team. This situation does not generally prevail in Great Britain." I believe this to be an oversimplification if n o t a misunderstanding of t h e nature of all the issues involved. T o illustrate my point it is necessary to look more closely a t the n a t u r e of this revolution and at some of its consequences. L e t us consider first the effects in the realm of control analysis. T h e outstanding developments have been in spectroscopy. Stemming in large measure from the pioneering work of the Dow Chemical Co. during World W a r I I , direct reading emission spectroscopy can be used in both the ferrous a n d the nonferrous metallurgical industries for rapid, accurate, and comprehensive testing. I n this country, at the Steel Co. of Wales, to take b u t one example, the analytical testing which previously required a number of routine "shift" chemists is now being carried out with great rapidity on direct reading, multichannel, and vacuum spectrographs. I n the chemical a n d petrochemical industries some qualities of a material m a y be continuously monitored by infrared or other techniques and effective automatic control of the process established. I n a sense this renders superfluous not only the analyst b u t also the analytical laboratory. Of more significance is the fact t h a t it m a y actually have made possible a process which by its n a ture could n o t otherwise be operated. I t could not accept the conventional delays between t h e t a k ing of a sample for t h e laboratory and t h e publication of t h e laboratory findings. I n general, these techniques give no new kind of information but, assuming t h a t the conventional analvtical information

they give is useful, they give it quickly enough for maximum use to be made of it. I t is n o t difficult to think of other circumstances where analytical information, obtained a t great cost and considerable labour, is available so late as to be only of post-mortem value. Unless these assumptions about utility are critically examined, we m a y , of course, merely succeed in amassing a large amount of useless analytical data in a very much shorter time. A large contribution to t h e analytical revolution stems from the introduction of more a n d more instrumentation and t h e use of socalled physical methods. I t is well to remember, however, t h a t although all analysis ends in measurement and measurement is a physical process, measurement in itself is not necessarily analysis. This misunderstanding is all too common and it needs to be emphasised t h a t a very great deal of classical analytical work is still required for the solution of our problems. Nevertheless, t h e introduction of physical techniques a n d instruments to the analytical laboratory has been of the greatest value, for m a n y determinations m a y now be made more elegantly and often without recourse to classical separations. Absorptiometry, flame photometry, atomic absorption spectroscopy, polarography, are examples. Where separations have to be made, chromatography in all its forms a n d the use of ion exchange resins have either replaced or supplemented more conventional chemical techniques. W h a t could be the greatest factor of all in t h e analytical revolution is the realisation, by w h a t is still probably a chemical minority in both countries, t h a t these newer techniques can a n d should be used to supplement or to complement, to extend and to replace classical analytical methods in t h e measurement of the things t h a t m a t t e r ; t h e realisation t h a t the object of analysis is to obtain information t h a t offers the greatest possibility of translation into a useful and satisfying statement of the properties of a material system. I n these circles also it is appreciated t h a t t h e 19th century idea t h a t analysis is wholly concerned with a statement of com-

detect and continually r e c o r d . . . 5§ς position, a n d t h a t this can be set down in a list of elements, or of arbitrarily calculated oxides or radicals, is no longer true. I t is in the acceptance of this broader phi­ losophy t h a t t h e fruits of t h e rev­ olution a r e to be gathered and, as a by-product, the distinction, hitherto often obscure, between testing a n d analysis m a y become more clear. With t h e introduction of so m a n y new and exciting techniques it would be surprising if t h e status of "analytical chemistry" h a d n o t risen, b u t until there is wider a c ­ ceptance of this larger conception of what constitutes "analytical chemistry" t h e full realisation of status is likely to be delayed. A more complex situation arises in t h e case of t h e analyst. There are m a n y young scientific workers, both chemists a n d physicists, en­ gaged in the application of these newer techniques of measurement, spectroscopy in all its forms, x-ray techniques, gas chromatography, and t h e like, who do n o t a d m i t to the practice of analysis a n d who would reject t h e label " a n a l y s t . " " L i k e it or n o t , " said Liebhafsky (9) recently, " t h e chemistry is go­ ing out of analytical chemistry," and until both industry a n d aca­ demic circles face up to the fact t h a t "analytical chemistry" now includes such a diversity of disciplines, a n d until t h e t e r m " a n a l y s t " is readily accepted as a worthwhile title b y those w h o practise them, then t h e s t a t u s of t h e analyst will n o t rise.

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effects, polymorphic forms of a sub­ stance, crystal size and shape, lat­ tice strain, inhomogeneity, inclu­ sions, distinction between surface and body composition, impurity levels of p a r t s per one, ten, or a hundred million, gases dissolved in solids. All this is becoming vital to the study of the behaviour and the uses of inorganic materials. The renaissance in inorganic chem­ istry and the growth of knowledge about the solid state demand a cor­ responding change in the analyst's thinking. I t is not uncommon, for example, to find materials which, on the basis of every conventional chemical method of examination, appear to be identical y e t behave quite differently in some modern applications. T h e "simple" com­ pounds ferric oxide and aluminum oxide are two examples t h a t come to mind. Analysis in this wider sense to which I have referred is, of course, an indispensable factor in all intel­ ligent research and it is clear t h a t the scientific disciplines involved in providing this kind of analytical re­ search service are no less in status academically t h a n those demanded of the research worker engaged on other aspects of an investigation. I t is not surprising therefore to find t h a t it is in the research labora­ tories of some of the major com­ panies on both sides of the Atlantic t h a t there exists an analytical di­ vision, or a unit with some other name, whose functions and objec­ tives reflect in greater or lesser measure these modern trends. An indication of the n a t u r e and ex­ tent of these developments has been given from time to time in the American chemical journals. Among the pioneers in the new thinking about the function of the analyst, mention must be made of Beverly Clarke who, while at the Bell Laboratories in 1931, described the role of analytical chemistry in industrial research, (5). More re­ cent outstanding contributions h a v e come from R. T. H a l l (6), who in 1948 discussed the role of analytical research in the Hercules Powder Co., and in 1949 from R. P . C h a p ­ m a n {2), who described the analyti­ cal organisation a t the American C v a n a m i d Co. at Stamford, Conn.

REPORT FOR ANALYTICAL CHEMISTS Charles Rosenblum of Merck and Co. w a s responsible for a masterly exposition of t h e subject of the industrial analytical chemist in 1950 (11) a n d the variety of professional services available from a centralised unit a t the Westinghouse R e search Laboratories was described by J o h n C. R. Kelly, J r . (8), in 1958. T h e broad p a t t e r n of organisation is no doubt different in every case a n d shaped to suit t h e special needs of each particular company, b u t t h e general philosophical background appears to have much in common. I n this country during t h e same period much h a s been spoken about this subject b u t it would be difficult to m a t c h this list with a similar number of published contributions to t h e subject b y British chemists. Nevertheless, comparable activities do exist in the research laboratories of some of the larger organisations —for example, in t h e various divisions of Imperial Chemical I n d u s tries, Ltd., t h e British Petroleum Co., Ltd., and T h e General Electric Co., Ltd., to n a m e only a few. I n the light of this it seems surprising to find how little notice has been taken of these developments in academic circles on both sides of t h e Atlantic.

Current Developments W e t a k e comfort in T h e General Electric Co., Ltd., from t h e fact t h a t there appears t o be growing a wider acceptance of t h e views t o which we have subscribed more a n d more over the last 30 years. Some account of this w a s given in 1950 under t h e heading of " T h e Co-ordination of Analytical Techniques in Industrial Research" (4) a n d again in the Svensk Kemisk Tidskrift this y e a r (S), b u t a brief reference to t h e n a t u r e of t h e organisation t h a t h a s evolved more recently a t t h e H i r s t Research Centre of T h e General Electric Co., Ltd., m a y best serve to illustrate some of t h e comments made earlier about t h e health of "analytical chemistry" in Britain. T h e company is in fact a collection of industries ranging from t h e very old to t h e very new, from glass and ceramics a n d metals t o telecommunications a n d nuclear power.

Interest extends therefore over a very wide range of materials a n d the properties a n d t h e behaviour of materials depend very largely on their chemical constitution and their physical structure. W e have for long believed t h a t " a n a l y s i s " can a n d should embrace all those techniques of investigation a n d measurement t h a t will contribute t o our knowledge of t h e structure and composition a n d properties of a m a terial—its n a t u r e a n d its " q u a l i t y . " T h e picture of our analytical facilities as they existed in our early days showed chemical analysis in its rightful place as t h e keystone of the whole analytical structure with some support from a spectroscopy group, concerned primarily with t h e measurement of radiation, a n d from an x - r a y diffraction group whose principal interest was in t h e crystal structure of materials. I n course of time, a n d with t h e stimulus of t h e developments of t h e last fifteen years, there h a s evolved a unit, t h e Chemistry a n d Technical Services Division, the efforts of a n y p a r t or all of which can be brought to bear on w h a t m a y broadly be called analytical problems. • T h e facilities within the division comprise classical techniques of chemical analysis and t h e newer techniques of separation by ion exchange and chromatography, including gas chromatogr a p h y ; instrumental absorptiometry a n d spectrophotometry, flame photometry, flame spectrometry and atomic absorption techniques, emission spectroscopy including directreading equipment, polarography, radiochemical techniques, vacuum fusion equipment for the determination of gases in metals, a n d conductimetric techniques for t h e microdetermination of carbon in metals or other material. I n addition, there are groups concerned with x-ray diffraction, electron diffraction by reflection a n d by t r a n s m i s sion, electron microscopy, radiology, and autoradiography. All this could bring its own p r o b lems, chief among them t h e selection of t h e right analytical technique, b u t our early decision to use the physical techniques then available complementarily a n d not competitively has facilitated t h e a b sorption a n d integration in t h e scheme of things each of t h e newer

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REPORT FOR ANALYTICAL CHEMISTS techniques as they have come along. We have indeed anticipated the ex­ cellent advice given by L. T. H a l l e t t in these columns a few years ago under t h e heading "Selecting t h e Right Analytical M e t h o d " ( 7 ) : " T h e answer," he said, "which is gradually being recognised, is to or­ ganise the analytical d e p a r t m e n t so t h a t it h a s both t h e chemical a n d instrumental to offer as service and so obviates t h e wasteful process of customers shopping around to get their analytical problems solved." Every problem submitted can be considered against this background and the n a t u r e of t h e examination planned in such a way as to give t h e information required, a n d not a l ­ ways t h a t initially requested for, as R. P . C h a p m a n p u t it, " a t a n y point along the line . . . . questions m a y be raised as to the propriety of t h e request, the possibility t h a t d a t a not specified might be more useful, or the addition of background in­ formation which might be more helpful." By co-ordination a n d integration of these m a n y techniques of exami­ nation, in particular in the case of inorganic materials, it is possible to give the quantitative composition in terms of major, minor, and trace elements ; t h e state of combination ; the concentration a n d distribution of impurity phases: evidence of inhomogeneity or nonstoichiometry ; the ultimate crystal size; t h e exist­ ence of polymorphic forms; t h e n a ­ ture of the surface layers where these differ from the body structure of t h e material. I t is perhaps not so i m p o r t a n t to stress, with Liebhafsky, t h a t t h e chemistry is going o u t of analytical chemistry b u t rather to emphasize t h a t physics is coming i n ; our a n a ­ lytical division has for long in­ cluded a substantial proportion of physicists. Indeed, to match u p to the requirements of a modern ana­ lytical unit the analyst m a y have to be something of a chemist, physicist, metallurgist, mineralogist, bacteri­ ologist, and electronics engineer, all in one. I n some circumstances t h e place of the analyst is t a k e n by a team of specialists, some of whom would formerly have h a d no place in the traditional analytical labora­ tory-,

While t h e a n a l y s t h a s therefore an i m p o r t a n t a n d essential p a r t to play in industrial research, his r e ­ sponsibilities are heavy, for besides his specialist knowledge a n d skills he must also become so knowledge­ able as to be able to discuss intelli­ gently the problems of t h e other r e ­ search groups t o whom he has a service to offer. H e must also be prepared to explain a n d to interpret the significance of his own contribu­ tion.

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TUBING

Summary To sum u p , i t is not only t h e techniques of analysis t h a t have been affected by t h e revolution of the last 15 y e a r s ; it is more particu­ larly t h e objects a n d t h e purpose of analysis a n d above all t h e concep­ tion of w h a t analysis comprises. Against this background it is per­ haps not very profitable to discuss the s t a t u s of t h e a n a l y s t on either side of t h e Atlantic until there is a clearer recognition as to w h a t con­ stitutes an analyst a n d what is now included in t h e obsolescent term "analytical chemistry." Above all, it is urgently necessary t h a t this re-appraisal should be made and understood in academic circles everywhere, so t h a t it m a y be real­ ised t h a t it is t h e best and not the second-rate m a n t h a t is needed for analytical work and t h a t a worth­ while, if demanding, career is open to him.

LITERATURE (1) Brandt,

W.

W.,

because set-ups are so fast and easy with Tygon Tubing's rub­ ber-like flexibility (yet Tygon is clear as glass, permitting visual examination of flow at any point);

... and SAVES because one tubing can be used to handle all chemicals found in the laboratory, thanks to Tygon's extremely broad range of chemical resistance (it's quick and easy to flushclean, too);

...

and

SAVES

because non-aging, tough Ty­ gon Tubing retains its unique characteristics throughout an amazingly long service life.

CITED ANAL.

SAVES

CHEM.

30,

39 A (December 1958). (2) Chapman, R. P., Chem. Indus. 1949. (3) Chirnside, R. C., Svensk Kemisk Tidsk. 73, 255 1961. (4) Chirnside, R. C , Cooper, B . S., Rooksby, H . P.. G.E.C. Journal 17, N o . 4 (October 1950). (5) Clarke, Beverlv, Ind. Eng. Chem. 23, 1301 (1931). (6) Hall, R. T., Chem. Eng. News 26, 3340 (1948). (7) Hallett, L. T., ANAL. C H E M . 27, 1509

(1955). (8) Kelly, J. C. R., Jr., Industrial R e ­ search Conference, Columbia Univer­ sity, 1958. (9) Liebhafsky, Η . Α., Pfeiffer, H . G., Winslow, E . H., Zemany, P . D., "X-Ray Absorption and Emission in Analytical Chemistry," New York and London, 1960 (J. Wiley). (10) Lundell, G. E . F., I N D . E N G . C H E M . , ANAL. E D . 5, 221 (1933).

(11) Rosenblum, Charles, Chem. News 28, 3578 (1950).

Eng.

Insist on genuine Tygon Tubing . . . no other tubing is "just as g o o d . " For your protection, every foot is branded with the n a m e " T Y G O N " a n d the formulation number. Ty­ gon Tubing is a v a i l a b l e at Labora­ tory Supply houses everywhere.

For complete technical information, write to­ day for free 28-page Bulletin T-100. 97-G

PLASTIC & SYNTHETICS DIVISION

U.S. STONEWARE AKRON 9, OHIO Circle No. 173 on Readers' Service Card VOL. 3 3 , N O . 1 2 , NOVEMBER 1 9 6 1

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