INSTRUMENTATION Complete automation of analysis foreseen in decades ahead H E NOVEMBER ISSUE of this j o u r n a l
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several stimulating discussions on t h e role and n a t u r e of analytical chemistry. W e wish t o comment on this question, n o t solely because, as J i m m y D u r a n t e would say, " E v e r y b o d y wants t a get inta da a c t , " b u t because we believe our own experience encompasses t h e entire range of what t h e extremists on both sides of t h e question are modestly claiming a t t h e t o p of their voices. Before chanting our personal Misericordia, m a y we say t h a t t h e E d i t o r of this journal has for years spelled out the definition of analytical chemistry. H e was a pioneer, in this country a t least, of microorganic analysis, t a u g h t analytical chemistry, contributed t o t h e field in original research, a n d finally directed one of t h e finest, best coordinated industrial analytical laboratories in t h e land. Upon invitation, our last issue profited enormously b y t h e observations of R . C. Chirnside, probably t h e most outstanding a n d i m p o r t a n t analyst in G r e a t Britain. Those who are fortunate enough to know Chirnside a n d have h a d t h e privilege of chatting with him know t h a t he only scratched t h e surface of what is t h e real problem in the current appraisal of analytical chemistry. Our own Prof. W . W . B r a n d t h a d reported on t h e relative situation a n d a t titudes toward analytical chemistry in G r e a t Britain a n d t h e United States. Chirnside, with typical British courtesy, tact, a n d diplomacy, preferred t o throw t h e questions toward t h e larger problem of how analysts in general are a p proaching their challenges a n d responsibilities. T h e consequences of this were t r a n s p a r e n t l y obvious. I t is not a question of t h e n u m b e r of professors, n u m b e r of courses in analysis, or n u m ber of endowed chairs in analytical chemistry, b u t r a t h e r t h e a t t i t u d e a n d degree of enlightenment of the incumbents. P e r h a p s our esteemed friend Chirnside might agree t h a t one could say, as of G a l a h a d — " H i s strength was as t h e strength of ten, because his h e a r t was p u r e . " Complete A u t o m a t i o n of Analysis
I n order t o conserve time a n d t h e patience of t h e reader, we wish t o m a k e several flat statements of conviction. This, for a twofold p u r p o s e : First t h a t
it m a y establish our considered opinions and, collaterally, t h a t it m a y spare t h e indignant from reading further. 1. A century or less from now, what used to be called analytical chemistry will be completely automated. There will be n o particular need for chemical experience, "chemischer verstand," or purely chemical justification for its practices. I t will require only a detailed knowledge of physical constants and an explicit definition of t h e information which is required. 2. T h e classical analyst, while hopelessly pleading for a r e t u r n t o fundamentals, will have largely abandoned the early precepts, traditions, and practices of t h e a r t . At this point, having lost an appreciable fraction of our readers, we proceed to our own personal " V i a Dolorosa" in an analytical career. I n this statistical age, our personal experiences have a significance which is 1, 2, 3, 4, or 5 σ · On t h e basis of statistical significance, we r a t e very close t o zero, b u t we would be, statistically, in good com pany with t h e first m a n who landed on the moon a n d got home in time for supper Classical A n a l y s i s
In our early youth a t the University of Pennsylvania, we had t w o years of qualitative analysis. T h e most casehardened classical analyst, if still living, would blanch a t this fact. Even among the classicists it is a moot question whether qualitative analysis should be t a u g h t a t all, or whether it should be introduced as an innocuous ingredient in general chemistry. Our professor, t h e late D r . John Hughes Miiller (no relative) was a slight, cadaverous, chain-smoking savant. H e was currently engaged in a redetermination of t h e atomic weight of germanium. We were always aware t h a t a n y white sulfide obtained in t h e second group must be germanium. Years later we discovered t h a t there is another white sulfide—zinc! W e analyzed dozens of unknowns. N o t those cryptically-labeled neat bottles, with everything in solution as soluble n i trates, b u t minerals with some of t h e dirt still clinging to them. Professor Miiller knew t h a t most of us were concurrently taking mineralogy a n d if we would heft t h e specimen, m a k e scratch tests, a n d t r y t o get a mineralogical
by Ralph H. Müller ^ÈrsÊÈSSk % SOXMMI hunch about t h e n a t u r e of t h e unknown, it was " n o go." H e h a d successfully smuggled prized and priceless specimens out of Mexico in his y o u t h a n d knew all t h e tricks. P e r h a p s we h a d a textbook, or mimeographed notes, b u t our bibles were Prescott a n d Johnson, and Fresenius. N o w if you wanted t o know t h e properties of indium ferrocyanide a n d its behavior toward a dozen reagents, you could find it in Prescott and Johnson. W e learned thousands of empirical facts about the chemical n a t u r e and properties of substances a n d those properties which distinguished t h e m from other substances. W e devised all sorts of short cuts t o outwit the professor, listing all cations which would be insoluble in excess of a m m o mium hydroxide and excess of sodium hydroxide. As fast as we devised short cuts t o t h e identification of an " u n k n o w n , " t h e professor would keep pace with our insolence. W h e n we got too " u p p i t y , " we would receive an " u n known" of red ink. Simple boiling with sodium hydroxide would yield a yellow-green fluorescence from which we would conclude t h a t t h e original was tetraiodo fluorescence or eosin. T h e University of Pennsylvania has never been a sectarian institution b u t it did offer chapel services from 10:30 t o 11:00 A.M. Miiller would emerge from his office, wade through t h e fog of a m monium chloride fumes, a n d announce — " C h a p e l hour, boys, do your praying here." Small wonder t h a t with this group of enthusiastic, students he offered a second year of qualitative analysis dealing with t h e rare elements. Then, shortly afterward, came enlightenment. We entered t h e G r a d u a t e School a t Columbia University. Although we became, after one year, referee analyst t o Professor H a l T r u m a n Beans, we learned t h e modern approach to analytical chemistry. W e learned about thermodynamics, orbitals, solubility products, a n d all t h e theoretical reasons why analysis is essentially impossible. One of our principal responsibilities was t o prove t h a t t h e electrolytic deposition of copper was, a t best, hazardous. Years before a t Pennsylvania we h a d h a d a special course in electrodynamics. O u r mentor was E d g a r F a h s Smith, Provost of t h e university. T h e r e were only t w o people in t h e entire world who really knew VOL. 33, NO. 13, DECEMBER 19«1
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INSTRUMENTATION what was significant in electroanalysis, and the American, Smith, was one of them. As undergraduates, at Pennsylvania, we were inordinately proud of the fact that we were the academic grandsons of his professor, Wohler. In a special laboratory at Pennsylvania, conducted by Smith's brilliant student Hiram Lukens, we used to conduct the complete analysis of a silver coin in 14 minutes flat. This was a result of Smith's innovation of the rotating anode. As we became more and more conversant in the esoteric nuances of thermodynamics and a more receptive attitude toward the limitations of empiricism, we began to get a more enlightened attitude toward analysis. Instrumental Analysis
At this point we concluded that there were numerous physical criteria of a system which had true analytical significance. This was the beginning of our interest in instrumental analysis. After some 20 years in the field, we are compelled at this late date to conclude that it was a complete waste of time and energy. Initially, with the suggestion that analytical information could be obtained instrumentally and more or less automatically, our notions
were received with hilarity. At the present time, analysis is so predominantly instrumental that the debate is almost a poor joke. In essence, it all depends upon whether you teach or work for a living. If the last ditch classicists have any argument, let them return to the real fundamentals of chemistry, however empirical they may be. Editorially speaking, we have run the entire gamut of analysis from the rank empiricism of Liebig, Smith, Fresenius, Treadwell, and Hall and all the rest up through the most recent advances. We are convinced that progress in analytical chemistry is largely in the hands of physicists and instrumentation experts in enlightened industry. It is no secret that analysts still do not enjoy the prestige of their associates in other fields. Some of us seek to ameliorate this situation by loud noises in management circles and with a modicum of success. We, personally, have given up the struggle by finding solace in the far more exciting field of nuclear physics. What may be the most significant contribution of last month's discussion is the simple fact that analysis has earned, throughout the entire world, a prestige and exalted position far greater than the opinions of its dichotomous proponents and practitioners.
