Automation analytical chemistry fromrule of thumb fully …downloads.hindawi.com/journals/jamc/1984/425239.pdf · 2019-08-01 · Journal ofAutomatic Chemistry, Volume6, Number (January-March

Journal of Automatic Chemistry, Volume 6, Number (January-March 1984), pages 6-13

Automation in analytical chemistryfrom rule of thumb to fully automatedmethods. Some philosophies and socialconsequencesR. Stanley

Department of History of Science and Technology, University of Manchester Institute of Science and Technology,PO Box 88, Manchester M60 1QD, UK*

Historical brief

It seems a far cry from 1761 when the chemist’s place ofwork wasdefined in the following way: ’Laboratory or Elaboratory, thechemists workhouse or the place where they perform theiroperations, where their furnaces are built, their vessels kept, etc.and in general the term laboratory is applied to any place wherephysical experiments in pharmacy, chemistry, pyrotechny etc.are performed’ [-1]. By 1880 it was pointed out to the AmericanSociety ofMicroscopists that ’the better the instrument the morereliable the results obtained, and the best work cannot be doneeven by the most expert worker except with the best instruments’[2]. Ofcourse we have seen dramatic changes in the appearanceofanalytical instruments since those days, and by the mid 1950sGeorge D. Beal could confidently state that the analyticallaboratory was, in his estimation, ’the Supreme Court of thechemical profession in its relation to industry’ [3].

From early times, equipment for chemical transformationshas been made by man--his machines having been evolvedfrom apparatus of the kitchen, the pharmacy and the forge.Quality and purity measurements became fairly widespread, theonly really qualitative tests being thcse for the assay ofgold andsilver by cupellation. The 17th century witnessed many newinstruments, such as the telescope, microscope, air pump andpneumatic trough for the collection ofgases. Eighteenth-centurypreoccupations with fire paved the way for the introduction ofthe mouth blowpipe, which further extended the range ofanalytical chemistry. Hydrometers, burettes, pipettes, polari-meters, viscometers, bunsen burners, colorimeters, and a wholehost of varied and important instruments became available tothe laboratory during the 18th and 19th centuries.

The 19th century was a period of consolidation. Chemicalanalysis grew into an art, with a sound empirical basis involvingweight relationships and chemical combinations. Techniques ongravimetric analysis were continually refined and there emergednew concepts of physical chemistry towards the turn of thecentury. Techniques in volumetric analysis were graduallyimproved, though it only became effective in industrial appli-cations around the middle of the century, and it matured as anaccurate method of analysis with the advent of sensitiveindicators and the general acceptance of titrimetric procedures.

* Correspondence to 16 Newbury Grove, Hopwood, Heywood, LancashireOLIO 2PL, UK.

The first titrimeric method was probably carried out by ClaudeJoseph Geoffroy in 1729 when he showed that Orleans’ vinegarwas stronger than the Parisian variety [4]. Descroizilles de-scribed a burette for the volumetric determination of alkalinematerials in 1806.

Instrumental methods at the turn of the century were wellreceived. They had an important role to play in industrialresearch and a greater speed and sensitivity in repeated analysesmore than justified initial costs. The theory of analyticalchemistry became more refined towards the end of the 19thcentury, and physical chemistry became popular through scien-tists such as Wilhelm Ostwald (1853-1932), William Gibb (1839-1905) and Wilhelm Pfeffer (1845-1920). Theoretical titrimetrybecame established, as did electrometric analysis--RobertBehrend (1856-1926) performed the first potentiometric tit-ration in 1893.

Twentieth-century analytical chemistry had a firm footing,both theoretical and practical, on which to build techniques inthe future. Theory and practice were becoming cementedtogether with the aids of better laboratories, improved tools ofexperimentation and a more coherent approach to the problemsin analytical chemistry, though analytical methods remainedsimilar to 19th-century techniques until the emergence ofphysical methods in applied electricity. The Laboratory of theGovernment Chemist in Clements Inn Passage, London, wasoriginally equipped in 1895 and it represented a significantlandmark in analytical workshops in Britain because of itsadvanced design. It set a precedent for others and was ashowpiece of the late Victorian age [5]. The benches had gascontrols, sinks and waste-disposal facilities which were plannedfor accessibility when servicing. Other features were a centrally-heated water supply (which served as a hot plate as well as adrying cupboard), a vacuum line, a microscope, a balance, aflash-point apparatus, a refractometer, a polarimeter and acentrifuge for milk analysis. The Government Chemist’s labo-ratory was in no way a reflection of most contemporarylaboratories. From around the turn of the century until aboutthe 1930s, analytical laboratories were furnished with equip-ment typical of that used for traditional analyses and such wetanalytical techniques dominated procedures used in analysingthe materials ofproduction and research well into the 30s whenelectrically powered aids became more commonplace.Analytical chemistry then was ’a rather unspectacular hand-maiden of the other fields of chemistry Some researchersemployed micro methods, particularly in organic analysis, and

unusual organic reagents, occasionally were used to detect andestimate trace amounts of particular ions’ [6]. Spectrochemicalanalysis had been developed initially during the latter years ofthe 19th century and the technique began to be used by manyindustrial and research establishments. Colorimetric analysis inparticular was a widespread technique using the now obsoleteDuboscq Colorimeter.

Though classical wet chemical methods were the dominantprocesses used to analyse the materials of commerce, micro-analysis emerged as a branch ofscience through chemists such asFreidrich Emich (1869-1940) and Fritz Pregl (1860-1930).Many techniques appeared or were perfected in the early 20thcentury. Gravimetric analysis, thermal analysis, titrimetricanalysis, non-aqueous acid base titrimetry, non-aqueous redoxtitrimetry, chelometric and complexiometric methods, func-tional group analysis and kinetic methods of analysis allrepresent the kind of impetus that was given in the field ofanalytical chemistry.

The Influences of the World WarsThe First World War ’greatly accelerated the demand for manythings and resulted in a large increase in industrial production’[7]. New and improved products created the need for carefulprocess-control requirements--classical methods of analysiscould hardly cope. At the end of the War there was a furthersteady increase in production. New elements were finding theirway into new products which rendered the older methods ofanalysis inadequate. The improved methods of productionaccentuated the requirements for more trained research chem-ists to undertake more precise and faster analytical techniques.Laws, theories, factual information and instruments gathered inthe fields ofchemistry, physics and other related subjects. Theseconverging ideas enabled analytical chemistry to emerge fromthe era of the burette and balance and into the era of thespectrometer and titrimeter--the instrumental era [8]. 1930marked the first significant use of electronic techniques inanalytical chemistry. Various devices such as photo-electricsystems had been tried, but the recording spectrophotometerwas the first successful instrument. It was invented by A. C.Hardy at Massachusetts Institute of Technology and it in-corporated a thyatron, which energized a pen motor and drove apolarizer, which restored null conditions in a Hiifner-typephotometer. Since 1930, the phenomenal growth in electronicshas resulted in a major revolution in analytical instrumentation.The rapid development of the vacuum-tube amplifier and thephoto-electric tube, and more recently, of transistors and othersemi-conductor devices, has resulted in the establishment ofmany analytical methods based upon them.

The Second World War placed heavy demands on thechemical industry for explosives, light metals, synthetic rubber,quality aviation fuels, synthetic oils, fats, medicinals and purifiedisotopes. In the USA, the chemical industry grew enormously.Despite their subjection to heavy bombing, the Germans hadproduced the V-2 missile which required its own special fuel. Theend of hostilities resulted in a Cold War, which, in turn, createddemands for nuclear research. There were other areas ofresearch such as in jet propulsion and rocket fuels.Investigations into outer space drew attention to elements andcompounds that had formerly been a mere curiosity. In 1957, B.W. Bradford and D. L. Nicholson of Imperial ChemicalIndustries illustrated only too well how the emergence of newand improved materials, which had appeared as a result ofWar-time hostilities, created a demand for improved methods ofanalysis during the period 1947-1957 [9].

R. Stanley Automation in analytical chemistry

The most striking development up to the early 1960s wasconcerned with electro-analytical methods--major facets ofwhich included potentiometry, polarography, voltametry, con-ductiometry and coulometry. With the introduction of themanufacture of spectrometers covering the ultra-violet, visibleand infra-red ranges, spectroscopic methods in analytical chem-istry were promoted to a prestigious level as an analytical tool.Spectrographic methods depending on the measurement of thewavelength and intensity of light emitted by an element orcompound in a flame or an electric arc have replaced some ofthemore conventional methods of qualitative analysis. An in-novatory and revolutionary analytical tool which was widelyused after 1950---chromatography--completely altered the ap-proach to problems associated with the separation and analysisof mixtures of organic and inorganic compounds. Absorption,partition, ion exchange and vapour-phase chromatography allbecame popular techniques. Analysis incorporating the use ofradioactive tracers were exhaustively tried and was implementedfollowing the availability of radioactive isotopes. Micro-chemical methods using milligram quantities produced ex-tremely accurate results and had profound influence on the rateof progress in organic chemistry. Methods of analysis wereavailable in the early 1960s for the determination of mostelements occurring in organic compounds, and determination ofoxygen became possible in 1947. The use ofimproved electronicdevices became popular and resulted in greater sophistication ofanalytical methods: this enabled analytical results to be dis-played by pen-recording devices, which subsequently enabledanalytical methods to be carried out completely automatically.

The processing and interpretation of analytical data

The most dramatic growth in signal processing and control overthe past quarter ofa century has come about in the field ofdigitalelectronics. By 1948, experiments were already in hand inconnection with stored program digital computers, but by thetime these first-generation computers were completed in theearly 1950s, they were already obsolete. Advanced knowledgeabout the subject of discrete solid-state electronics progressedrapidly; and, by the late 1950s, specialization in large digitalcomputers was such that they could be used in scientificapplications. Initially such machines were used to handlemassive numerical calculations. By the mid 1960s, chemists werebecoming enthusiastic about the application of the dedicatedcomputer. In the UK the situation appeared to be very similar tothat in the USA, and dramatic changes in analytical procedureswere very apparent between the years 1954 and 1957 in the fieldof process control [10]. In 1954, Walter J. Murphy (editor ofAnalytical Chemistry)prophesied the way ahead in analyticalchemistry with a fair degree ofaccuracy as to what it might havepromised to society at large [ 11]. In contemplating the future interms ofthe instrumental regime ofanalytical chemistry MagnusPyke noted:

Traditionally the analyst has prized his technical dexterityat the bench. Yet there are today clear signs for all who areprepared to read them that increasingly we shall findanalytical techniques being carried out automatically.Already there are automatic spectrographs for steelanalysis, automatic analysis assemblies for determiningdissolved oxygen designed by the Water Pollution Board,and even general purpose automatic analysis equipmentcommercially available for those who wish to arrange forroutine operations to be done by machine rather than byshift chemist. As this kind of apparatus becomes more


common, clearly skill and dexterity in the laboratory artswill be less in demand [12].

The signs were there for all to see, the classical chemist was tofeature less and less in the field of analytical control as the artand science of analytical control by instrumentation advanced.The chemist trained in the rigours of classical analyticalchemistry would have to change his whole outlook towardsthese newer procedures ofanalysis, or become obsolete during aperiod when the economic growth ofan industrial (or otherwise)organization was becoming largely dependent upon paying lowwages to its employees. Fully automatic procedures would, ofcourse, increasingly feature in analytical procedures, eventhough it was appreciated that these systems had a high initialcost. In the long term they can be proved to be less labourintensive and capable of being used in a profitable manner. Theimpact of instrumental techniques upon industry was perhapsbest described by G. F. Smith in 1957:

Fantastic applications and accompanying instrumen-tation as applied to analytical operations have served amajor role in glamourising the field. This is the majorinfluence in the ascendancy of analytical research androutine industrial control in the last quarter century. Theclick of the Geiger counter, the flick of the neon,button

indicators, the whine of the centrifuge, the graphicrecording of the Brown chart and the fabulous simplicityof the operations of gas-phase chromatography are butcasual examples. The multiplicity of electronically oper-ated instrumentation devices has been the basis of arapidly growing industry devoted exclusively to supplyingthe necessary equipment. The requisite monetary outlayinvolved seems to be no deterrent. From the electronmicroscope to the mass spectrometer, and all the inter-mediate installations, instrumentation serves the fieldwithout noticeable retardation [13].

From about the end of the Second World War to the mid1950s, three factors appear to have been operating which gaveadded impetus to the growth and popularity ofinstrumentationand automation of analytical processes. These factors may beseen as antecedents of the complex factors operating today:

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A decline in manpower available for analytical work.A rapid increase in the volume of analytical workrequired for the control of new plants.A very marked increase in the complexity of newanalytical problems arising from the development ofnew products, particularly in the organic field.

The trends towards automation

As instruments and systems became more sophisticated, theywere further refined as a result of advances made in com-puterized techniques and data handling. Different systemsbegan to be interfaced and miniaturization of electronic gad-getry allowed such systems to be featured in more compactforms. The revolution in the field ofelectronics has perhaps hadthe most far-reaching consequences for automated analysis. Adivisional chief analyst [14] of a research department of a largeindustrial chemical complex isolated some ofthe growth areas ininstrumentation within his company during the period 1955-1980. This particular research department then dealt with some15 000 samples per annum. The period between 1960 and 1965was thought to be the rapid growth time which resulted from theuse of mechanical means of automation such as syringe pumps,crozet motors, cam timers, syringe dispensers and analogue

displays. Between 1968 and 1975 was thought to be the periodwhen the newer techniques ofanalysis were appearing and it wasthe start of the laboratory computing era. Analytical problemswere becoming more complex. These years represent the era ofthe microprocessor. Although there is now a proliferation offairly sophisticated equipment and computers, their use dependson the number ofsamples and the frequency ofpresentation andwhether the analysis of batches is possible. Much can be gainedfrom partial automation and very often a demand for analysisgrows with analytical capability. As the employment of anal-ytical manpower has become more and more expensive, thedecline in the number of analytical chemists has been a directfunction of the use of analysis instruments. There has been atransitional phase from bench analysis to laboratory instrumen-tation [ 15]. The ultimate in laboratory automation, which hasin some cases already been achieved, can be thought of as theextensive replacement of laboratory analytical control by con-tinuously operating process stream quality-control instrumentswhich are used to direct integrated automatic-control systems.The use ofsemi- and fully automated techniques went a long wayto solving problems associated with the limited manpowerproblems--problems that J. Craik had noted in 1957 when hewas Chairman of the ICI Nobel Division [15].

Where have all the chemists gone?The period 1950-1960s witnessed the decline of the chemist[16J--where before older instruments had been used by ex-perienced analysts almost as a sideline, newer generationanalysts took over, all too often with very little or no knowledgeof chemistry. The classical chemist was to feature less and less inindustrial laboratories, and this situation was to deterioraterapidly to the point where there was an acute shortage of suchpeople. Wartime experiences had made the government re-evaluate education in Britain because hostilities had made thecountry even more aware of the fact that it depended uponscientifically and technologically trained staff. If Britain was toachieve its manpower targets set in science and technology asoutlined by the Percy Report on Higher TechnologicalEducation, and the Barlow Report of 1946, it was thought thatuniversity output would have to double [-17]. This doubling ofthe number of scientists and technologists did in fact comeabout. Consistent with such expansion, a trend of studentsstaying on for sixth form education prior to university entrancecame about. Many further-education institutions acquired fullstatus of universities. The expansion in scientific subjects wasalso stimulated by interests in jet propulsion. Industry could notget the requisite number of such trained scientists to work intheir laboratories. The economy was running at almost fullemployment, and demands for industrial scientists, chemists,electrical and mechanical engineers remained in excess ofsupplyfrom about the late 1940s to the middle 1950s. Such factorscontributed in no small way to the shortage of suitably qualifiedanalysts. Moreover, subjects such as mathematics and statistics,electronics and physics were beginning to attract students whootherwise might have become analytical chemists. With incent-ives in other academic disciplines, with analytical chemistrybeing held in poor esteem, and a ’creaming off’ to university ofgood practical and academic laboratory staff, the use of semi-and fully automated systems in analytical quality controlbecame a vital necessity. Another deleterious factor aggravatedthis situation during the 1960s, which must have been workingcontrary to trends that would otherwise have been beneficial toindustry in Britain. There was a serious drift abroad of scientists

and technologists which gave rise to the catch phrase--’TheBrain Drain’ [18]. It is now more than apparent that the era ofthe classical chemist is over, and events have justified theprophecies made in the past. Heavy investment in Americanspace programmes has resulted in the emergence of specializedanalytical equipment that is capable of sampling and analysingon the surfaces of far-off planets. Indeed, it has been some ofthese kinds of ventures in the USA that have lured British topscientists and technologists abroad. The skills of the analyst cannever be totally superseded for his knowledge and applicationswere and are still needed for the analysis ofstandards used in thesetting up, calibration and control ofinstruments. The qualifiedchemist still retains a vital role as the arbiter between customerand supplier, and this role is governed by procedures which useestablished, standardized classical methods of analysis whichwere developed over many years. Albeit, certainly in the UK, itmight be fair comment to state that analytical chemistry as aprofession has become downgraded by a complex matrix offactors outlined above and possibly some others not mentionedhere. Objectively, the analyst became regarded by many asrepresenting an overhead charge to production, and his skills,accuracy, reproducibility, efficiency and fatigue effects could, inmany cases, be bettered by instruments of this ever-expanding’black-box’ era.

Trends towards full automation

In the USA there appears to have been a more dynamic attitudeto the full utilization ofautomation in analytical chemistry whencontrasted against the situation in the UK. By 1958, the analystwas becoming more challenged by the advancement of tech-nology with the inherent advantages offered by mechanizedinstruments [ 19]. As noted already, the analyst was regarded asrepresenting a high overhead charge to production. It becamemore important for the chemist to think in terms of cost/man-hour or pennies/test. Analysis for its own sake was seen as anobjective that was no longer valid. Ultimate precision inanalytical processes was seen not to be a prime requirement ofthe chemist, as in most cases an error of +_5 would notnormally be of too much significance. Analytical speed becamean important criterion in analytical control, and completeanalysis in many ways was seen as giving a pointer to the efficientoperation of a process. As instrumental procedures began to beapplied to analytical control, their operators were not alwaysrequired to have a knowledge of the chemistry of a particularprocess or to know the chemistry ofthe reactions involved whichdictated the choice of technique for analysis, and hence theinstrumentation being utilized. Only when analytical resultsbecame abnormal were questions asked about their impli-cations, The overriding factors which prescribed the analyticalprocedures used was the time occupied in each control test, andthe wage of the individual worker. Such a situation was wellillustrated by L. H. Lampitt ofthe Lyons Laboratories, London,in 1952 at the International Congress on Analytical Chemistry[20]. More unquali.fied labour began to be used in analyticalcontrol as instrumentation and automation began to featuremore in production laboratories. However, it was well ap-preciated that, when operated by the most careful oftechnicians,such sophisticated instruments could not replace the experienceof the analytical chemist. Such chemists qualified in the moretraditional techniques were becoming more of a rarity by 1960[21]. As a consequence, the use ofcontinuous analysers for plantcontrol was in many cases thought to be of paramountimportance. The situation was much the same in the USA in1963, and attempts were being made to attract qualified


graduates into instrument-development groups. Such a short-age of qualified personnel was a problem apparently shared bythe whole instrument industry [22].

More and more literature on instrumental techniques ap-peared in textbooks as analysts grappled with the bewilderingproliferation ofnew machines. The preface to A. I. Vogel’s thirdedition of Qualitative Inorganic Analysis (1961) indicated theimportance that he thought should be placed upon the extendeduse of instrumental analysis: ’It is generally accepted that thetraining in at least some of the instrumental methods is highlydesirable’ [23]. Included in the text are detailed descriptions andapplications of various instruments. This standard referencework presents a balance between classical and instrumentaltechniques and also gives due emphasis to the requirementsof older techniques needed for standardizing instrumentalprocedures. By today’s standards many of the instrumentsillustrated by Vogel could be ’relegated to the attic or the cellar’,but the theoretical principles upon which many of theseinstruments operated (or perhaps still do operate) still apply tothe more streamlined machines of today with their multifunc-tional capabilities. Vogel’s book in many ways reflects thetransitional stage from the truly classical procedures to thoseinstrumental methods which would ultimately merge into fullyautomated techniques. At the time ofprinting, Vogel noted that,due to limitations on space, topics such as X-ray methods, massspectroscopy, gas chromatography, radiochemical methods,nuclear magnetic resonance spectroscopy, polarimetry andrefractometry had to be omitted from the book. These omissionsalone illustrate the vast number of instruments that could thenbe acquired.

Naturally enough, with such increases in the use of,physicalmethods of analysis, problems did arise in connection withtraining in instrumental methods [24]. Many of the inter-connected problems associated with recruitment are still with us,and it remains fashionable for companies to recruit laboratoryassistants with minimal or no qualifications at all, which can be afinancial advantage in the long term.

Changing economies

The 1950s witnessed increasing demands in ’money wages’following the events of the Second World War. In the USA, realcompensation per man-hour in the private economy has risenfaster than productivity since 1940. During the early 1960s, realhourly earnings increased less than productivity, and unit costswere stable for the period. Between 1966 and 1971, real earningsand money earnings had exceeded pi’oductivity gains, and thisresulted in a sharp rise in unit labour costs--especially in the1970s. Between 1947 and 1970, the output per man-hour in thetotal private economy showed an annual increase of 3.2%compared with the average increase of 5" 1% in the compensationper man-hour, in 1970, annual increases in productivity fell to0"9%, whilst compensation per man-hour rose by 7%.

Following the War, Great Britain evolved an incomes policywith a view to restraining wages and prices, which, it was hoped,would compensate for the relatively slow growth in produc-tivity. It was thought necessary to maintain a viable inter-national trade balance. Both Labour and Conservative govern-ments inaugurated incomes policies--Labour’s ’wage freeze’between 1948 and 1950, and the Tory ’wage pause’ between 1961and 1962. Other measures were implemented to resolve theworsening economic situation. The National Board of Pricesand Incomes was terminated in 1971. A wages explosionoccurred in early 1970 before elections returned theConservatives to power, with earnings increasing by 15% during


the year. Other developments up to 1973 occurred to aggravatethe British economy [25]. The economic boom of 1973 wasbrought to an abrupt halt in 1974 by the oil crisis, which causedrecession and accelerated inflation. The effects on wages andemployment were dramatic and this was reflected in a decreasein the hours of working [26].

Consistent with such inflationary trends in the cost ofmaterials, professionally trained and well-qualified analyticalchemists became expensive commodities at a time when lowpaid and unskilled technicians could achieve better and fasteranalytical results by using sophisticated instrumentation. Suchset-ups offered greater flexibility, were less prone to fatigueeffects and were found to be more cost-effective than humanbeings. The trend began when instrumental techniques began tobe applied to analytical processes, and it has carried onunabated since with the effect that laboratories ofthe future maywell be operated by neon-flashing robots that do not in-corporate the instinctive correction facilities that were so oftenfound inherently in the dedicated and experienced analyst.

The changing face of industrial analyticallaboratories

Analysis is fundamental to chemical operations. A chemicalsynthesis can only be considered to be complete when theproduct has been fully analysed and its component partsdetermined. Analysis is the common language of the chemist inindustry. As effective analysis has become more important in theface of economic constraint and a requirement for closespecification control, it has come to rely even more on in-strumentation and automation. Analysis is the basis ofnationaland international commercial agreements which must dependon internationally agreed methods and interpretations. Analysisin industry embraces overlapping aspects of the overall object-ives of analytical control: research, process development andprocess control. As increased demands were placed on analystsin industry, central laboratories introduced instruments thatsaved on mundane laboratory tasks and improved speed.Simpler analytical instruments were available for use on theplant so that shop-floor personnel could undertake their owndeterminations to get stream composition values. This elim-inated the sample ’lag time’ existing between the laboratory andthe plant. Monitoring instruments were introduced, whichdirectly recorded various critical compositions from plantstreams. Manual analysis was becoming replaced more bymechanical aids or the use ofdevices that could measure directlya physical property related to chemical composition.Mechanized machines included automatic and semi-automatictitrimeters, automatic apparatus to determine thermal arrestpoints for such purposes as crystallizing and freezing, automaticdistillation apparatus for determining the Reid vapour pressureof petrol. Techniques used for measurement of a physicalproperty included absorption and emission spectrophotometry,mass spectrometry, gas chromatography and an assortment ofnow household names in the field of such sophisticated tech-niques. Even by 1957 analysts were confronted by a bewilderingchoice ofinstruments that were available for off-line and in-lineapplications. Many systems that were commercially availablewere ofAmerican origin, and this is still the case today. Thoughthere was a proliferation of machines to control operatingplants, in many cases there was a scarcity of reliable, quality-controlled instruments. This was in part due to a lack ofconfidence at the interface between the instrument user and theinstrument manufacturerha situation that seemed to be more

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pronounced in Britain than it was in the USA. A comprehensivereview of the instruments available for industry was given in1964 [27]; American machines were particularly featured. Thesituation with regard to the instrument business in the UK haschanged little from the early 1960s to date [28]. Such instru-ments were so sophisticated that in many cases they werecapable of performing the majority of analyses that could bemade in the plant-control laboratory in suitable circumstances.Most on-line analysers around in the mid 1960s wereexpensive--typically between about 1000 and 3500. Not onlywere more American instruments available, but they were usedmore extensively in the USA [31J--one American firm with 20chromatographs thought itself to be ’lagging behind’; another.was apparently using 100 on-line chromatographs (half forautomatic control) in petrochemical applications. A similarsituation existed in German firms. It seems ironical that by 1950the British instrument business had apparently established itselfwith high standards and it was apparently well advanced [32].Many parameters seem to have contributed to Britain’s declin-ing role in this industry--a less flamboyant attitude, a poorattention to communications and applications at the interface ofanalytical science and production technique, ill-documentedliterature, a lack of suitably trained staff, a cynical attitude tooverall instrument credibility, poor investment in laboratoryequipment [33], a poor awareness ofthe technical developmentsof mechanical aids for research and development, poor appli-cations engineering, poor salesmanship as a result of lack oftechnical knowledge, unfavourable tax incentives, the ’BrainDrain’, the effects of industrial and government secrecy as alegacy of War [34, 35 and 36], and a lack of desire to interfacedifferent technologies that contribute to the instrumentbusiness.

Such factors have all played their part, and some universitiesin the UK have recently set up departments that bring togetherseparate skills and disciplines and interface theoretical mattersderived from other areas, such as physics, mathematics, com-puter science and management science. From this has emerged arecognizable discipline ofanalytical science, which embraces thesociological implications brought about by the use of micro-electronics. By becoming involved in the multi-disciplinaryapproach this newly recognized analytical format the analystideally becomes an integral part of a team who take collectiveresponsibility for a production process, and his new technologyshould provide the automated means of finding meaningfulresults. P. B..Stockwell succinctly defines automation as ’amultifaceted and multidimensional problem, the various aspectsof which are fully interlocking a multidisciplinary problem’[37]hthe total systems approach. The skills required to achieveeffective automation include electronics, statistics, computerexpertise, with an associated knowledge ofbusiness and organiz-ational skills. Perhaps Britain is at last ’getting it together’.

The 1974 oil crisis escalated the costs oflabour generally andthe costs associated with employing analytical staff began totake an even greater slice of company profits. With theemergence of multi-processor technology, computer facilitiescame to be adopted more in analytical control, particularlybecause they could be applied to dedicated and flexible ana-lytical systems. Such machines had the ability to handle evenmore complex analytical data. Computerization is now anecessity in the field of analytical instrumentation and it hascome of age in being able to interface modularized analyticalsystems. This in turn has extended nalytical capabilities andhas led to many improvements in economic performance on theindustrial front. From communications [38] with a largenumber ofchemical firms and allied manufacturing industries inthe UK, it was apparent that many ofthese organizations beganto adopt analytical facilities with ’state-of-the-art’ electronics

from about the mid 1970s--particularly those large competitiveindustries that could afford them. It is interesting to note thatfrom analysis ofsuch communications with a variety ofchemicalcompanies, that the period between about 1964-1973 was a timewhen companies were buying even fewer instruments than theyhad been in the decade 1950-1960 when labour costs were notwhat they were to become during the 1970s. The worseningeconomic situation from about 1974 became more apparent toindustrialists who quickly realized that computer-interfacedsystems could realistically become very economical and thereforehelp to cut down labour costs. This trend of upgradinganalytical facilities has become widespread, although the use ofsuch modern instrumentation does not necessarily apply to allanalytical strategies--particularly where a batch operation isused as the normal production mode.

Automation of continuous processes has led to the formu-lation of generalized theories, philosophies, definitions and newapplications appertaining to chemical processes at the control,and research and development stage. An overview ofthe state of’Instrumentation and control in process industries’ in 1973 [39]indicated that the adoption of computer-controlled processeswas delayed by a lack of knowledge about particular processesand the theoretical variables involved, and the lack of in-strumentation for continuously monitoring some of the processvariables.

D. S. Harder in 1936being employed by General MotorsCorporation defined automation as ’the automatic handling ofparts between progressive production processes’. A definition ofautomation given in Encyclopaedia Britannica in 1973 [40] wasa little more comprehensive: the term ’automation’ evolvedoutside the disciplines of analytical chemistry and may notalways be appropriate in that context. In a 1968 thesis [-41], D.G. Porter of the Laboratory of the Government Chemistsurveyed the various definitions that have been put forward inrelation to laboratory automation by workers such as R.Jonnard (1960) who defined it as ’the science concerned with thetechniques, methods and principles involved in each phase ofqualitative data acquisition, reduction, conversion, transmis-sion, storage, retrieving, handling and computation by auto-matic instrumentation’. Porter outlined the distinction betweenmechanization, instrumentation and automation in laboratoryapplications. The term ’automation’, accepted in 1958, wasconsidered to be a ’relatively new word in the lexicon ofanalysts’[42]. A generalized definition of automation was given by R.Kuzel et al. [43] in 1969; as early as 1957, Gorden D. PattersonJr. had suggested a broader definition ofautomation that wouldnot only be applicable in process or manufacturing operations[44]. A rationalized definition of automatic analysis whichembraces most of the techniques available to analytical chem-istry was given by Foreman and Stockwell in 1975 [45] whoquoted from the Commission ofAnalytical Nomenclature oftheAnalytical Division of the International Union of Pure andApplied Chemistry. They also gave a definition for mechaniz-ation. Whatever definition is used to describe fast analyticalmethods, it is clear that they have a vital part to play in chemicalindustries. Foreman and Stockwell note that expansion in thefield of automated analysis is characterized in our standards ofliving and general well-being [-46], and that such instrumen-tation provides an important analytical service to industrywhere analytical information can be produced quickly andevaluated rapidly. In industry, such analytical procedures maybe accomplished off-line, on-line, or in-line with a relatively lowtotal analysis time. Continuous-flow and discrete sample-processing systems have been exploited successfully in a varietyof configuations in both research and industrial laboratories. Areview in 1969 by Kuzel et al. [47] gives details of the variousautomated and semi-automated systems then available, and


they also give extensive references to other work in the field atthat time. The paper also highlights the advantages of usingautomated uniformity, a greater optimization of analyst’s time,labour savings, increased laboratory throughput, an earlywarning of production and process difficulties, and a speediertransfer from research and development programmes to full-scale production. On the negative side, automation can beineffective on a small number of samples where a variety ofproducts is processed, where the method does not comply withofficial compendia, where the technique does not lend itself toautomation, or, perhaps more important, where the costing ofautomatic equipment may be greater than any anticipatedsaving. There are now well-established philosophies concerningautomation and there are also some futuristic ideas as to whereautomation and computing are leading to [48]. Whether justmechanized, partly automated or fully automated, a prolifer-ation of sophisticated instrumentation is described in scientificliterature. The changes that have occurred as a result of themicroprocessor revolution have been dramatic in the very recentpast. A complete world-wide listing of scientific equipmentmanufacturers, dealers and distributors appeared in theLaboratory Buyer’s Guide Edition of International Laboratory in1980 and it contains a great deal of information that cannot begained elsewhere. Its objectives are to aid laboratory researchersin obtaining information about products available--highlighting an awareness of the need to communicate ideasacross a multitude of disciplines which lend themselves to someform ofinterfacing in the broadest sense ofthe word. The editionhas since appeared annually. An analysis of the internationalcompanies listed in the 1980 edition illustrates that the USA stillhas by far the largest commitment to laboratory management[49].

The present status of automation inanalytical chemistry

It has become increasingly apparent that automated procedureshave become an essential element of analytical control in thelaboratory, and their use is not restricted to clinical laboratoriesand process control. Automation can involve all stages of ananalytical procedure including sampling, sample preparation,separation, standardization, calibration, data collection andprocessing, reporting results and data storage and retrieval. Overthe past 30 or more years chemistry has expanded tremendously,as witnessed by the logarithmic increase in the associatedjournals. In no small measure, it has been due to the innovationand adaptation for common use of instrumental techniques.Like other branches of the subject, chemical analysis hasbenefited and the subject has been transformed from that basedon chemical technique to one based on physical methods.Consequently, concepts and philosophies have been introducedinto analysis which even a few years ago might have been purelyassociated with other disciplines. The modern-day analyst needsto develop skills and familiarize himself with the theoreticalmatters derived from physics, mathematics, electronics, com-puter science, and technology and management science.Crystallizing out from the interfacing of these multidisciplineshas been a recognizable discipline of analytical science whichfurther embraces wider horizons other than those bounded byanalytical chemistry. In recognizing the importance and impli-cations ofanalytical science, the Department ofChemistry at theUniversity College of Swansea, introduced a BSc in the subject,and the Swansea Summer School of Automatic ChemicalAnalysis was conceived within this framework. First given in

11


1979, the Summer School was received with enthusiasm. In 1980the School was equally, if not more successful, and like theprevious and all subsequent meetings, it drew lecturers ofinternational repute who detailed the latest thinking on allaspects of chemical analysis. Like the analytical department atSwansea, a similar department has been established at theUniversity of Manchester Institute of Science and Technologyto look into the applications ofautomated analytical techniquesat a high academic level under the guidance of three appointedprofessors.

There is now a wealth of information scattered in theliterature which describes automatic equipment and its as-sociated gadgetry which can be used in analytical control andresearch. The appearance ofthe Journal ofAutomatic Chemistryrepresents ’the beginning of the end: the end of a struggle tolegitimize automation in chemistry and the beginning of what’,Dr Peter B. Stockwell says, ’will be a valuable means ofcommunication for those of us as chemists, who becomeincreasingly involved with automatic analysis’.

Some generalized conclusions

Much talent has been applied in the service of analyticalchemistry and its application to industry, and there has beenprofuse practical applications of technology to production overmany years. Multi-disciplinary expertise required by the chemi-cal industry has encompassed the talents of chemists, engineers,physicists, biologists and managers. Chemical analysis is con-cerned with the utilization of diagnostic chemical action onsmall- and large-scale industrial processes that depend onchemical principles. Journals relating to the state-of-the-art, ofanalytical chemistry began to appear and such publicationsproliferated as greater importance began to be placed on thissubject, which was becoming transformed from rule-of-thumbtechniques to a specific discipline in its own right. As it graduallybecame more obvious that chemical manufacture was based onscientific principles and that knowledge of such principles wasimportant in terms ofindustrial competition, it was realized thatthere would be a need for increased technical or educated skilland a wider diffusion of the knowledge of scientific principles.Such a climate permitted the assayer to emerge from hismysterious alchemical workshop to develop his imaginative anddiagnostic talents in modern laboratories surrounded by a hostof ultra-modern, dehumanized and automated aids. Chemicalproduction has considerable potential for causing environ-mental damage, and there sometimes exists antagonism betweenenergy requirements and material goods on the one hand, andenvironmental pollution on the other. Angus Smith--thefamous Alkali Inspector over 100 years ago almostsingle-handedly created a style of surveillance over industrialpollution which has become a tradition. His talents andapplication allowed pollution not merely to become minimized,but to become optimized--to strike a balance between thebenefits of productive industry and clean air. Since that time,various analytical procedures have developed for differentmanufacturing industries which have extended the practice ofanalytical chemistry and illuminated malpractices. As thechemical industry grew, so did a new set of analytical require-ments for chemical control of the processes involved foreconomic and social reasons--not merely to curtail the effects ofpollution and chemical adulteration--but to determine thequality of raw materials and finished products from industrialmanufacture whose products were becoming more specialized.As such developments became apparent, chemical apparatus

12

became refined and more accurate, and new analytical tech-niques developed into more complex procedures.

After the two World Wars, it became apparent that stan-dards of living generally would improve, and there was arequirement to mass produce a whole range of consumerproducts which required an even greater degree of qualitycontrol. As a result, instrumental analytical procedures de-veloped which furnished industrialists with the means of fullyoptimizing processes in terms of decreased product losses,formulations, efficiency, process material recovery, continuousmonitoring, energy conservation, product quality, lower recyc-ling costs, and other related aspects of efficient industrialproduction. Many of these precise production techniques wereclosely guarded in an age of commercial confidentiality whichwas rife following the end of the Second War, and instrumentaltechniques in many cases were developed shrouded by secrecy ata time when the theoretical aspects of electricity were beingrigorously applied to instrumental systems. At the same time itbecame apparent that there was a shortage of analyticalchemists, technicians and laboratory assistants. This trend is stillapparent today and is similar inasmuch that the cost oflabour isexpensive and its amortization in the long term is poorcompared to sophisticated instruments costing many thousandsof pounds. Analytical chemists as independent arbiters givetechnical judgements and often give rise to public disaffection atthe academic and industrial level.

Often, parallels are drawn between scientificand technical research and economic well-being. Ambiguity hereoccurs by economic recession in the West and political oppres-sion around the world, and only too often there are widespreadfears that new applications of such technology, whilst raisingstandards of living, may threaten collective security. In such aclimate educated issues are raised as specialized syllabi andheavy emphasis placed upon academically biassed examinationrequirements has made wider the social and professional tiersbetween those with academic and those with practical skills, andmay have also made worse the socio-economic divisions. Manyteachers in Britain are not involved in the conditions of themarket place in which their students must find employment.Such a condition can be said to have contributed to awidespread ignorance of the ways in which much classroomknowledge may be relevant to the industrial world. A morecoherent interfacing ofcurricula should be apparent through thelevels of science and social education from the primary throughto the tertiary levels. Moveover, the educator should beprepared to become re-educated to keep abreast of newtechnologies as they affect the interfacing of his discipline withindustry and the social and economic world in which we live, andthe penetrating implications that the world of microprocessortechnology has to offer. Related to this is the desperate shortageof graduate science teachers at the secondary level and the poorcareer structure. A trend in the early 1970s was that manyscientists moved into posts such as accountancy where basicnumeracy and basic logic are important. They li.ked what theyobserved and they stayed. Growth was also apparent on thenumerate and social sciences such as business studies, manage-ment sciences, accounting and financial management. In ourrapidly changing technological society, changes are taking placemore than at any time in our history. Now adaptability andwide-ranging personal skills are required and just being a goodscientist is not enough (perhaps it never was). Scientists need tobe ’interfaced’ at all levels to embrace the full consequences oftheprocesses they set out to control and develop.

In recent times, it may be said that in Britain, the ambitiousstudent often became a victim of the ’dirty-hands disease’--asituation whereby he quite easily became infatuated with thoseacademic courses promising better financial rewards and greater

personal recognition. There has been a reaction against thepopularity of subjects such as analytical science in recent times,even though such subjects can be said to be the backbone of theeconomic prosperity of this country. The application of auto-matic control to analytical chemistry is a typical example ofhowBritain has the available technology but failed to capitalize uponthe principles involved. This situation was typified by theintuitive exploits of John Sargrove, a Londoner, who died in1974 and whose work is now almost entirely forgotten. He andhis team of 20 young engineers laid down the foundations formodern automation which was seen as the answer to post-Warlabour shortages. From 1947 to 1949 the team designed ’masterbrains’ to automate industrial processes; he was a victim ofpolitical pressure and tried to convince people that automationwould not create unemployment--rather, that it meant re-deployment. His arguments did not prevail; money dried up andso did government interest. Now, 30 years later, the UK has toimport electronic circuit-making equipment similar to thatmade by Sargrove [50]. Like automation in analytical chem-istry, this is a doleful reminder ofhow the UK fails to capitalizeon technical ideas. In the 19th century, the British chemicalindustry failed to exploit Perkins’s discoveries. Foreign instru-ment competitors very often seem to have much better sellingorganizations, highly trained staffs of technical scientists readyto help any customer with instrumental problems, and a muchmore outward-looking attitude to business generally. Over thelast few decades in Britain, there appears to have been lacking awillingness to bring together more the instrument maker and theinstrument user. Applications engineering likewise has not beenexploited to the full. In Britain, male models appear to rankhigher than engineers. It has been said that Britain’s currentpoor economic performance may be blamed on the predomin-antly non-technical backgrounds from which the seniordecision-makers in British industry, finance and government aredrawn. The attitude of the instrument user to the instrumentmaker has waxed and waned throughout time, and the lack ofrapport between the two appears to have been more pronouncedin the UK. Perhaps it has always been reflected in the classposition held by the humble craftsmen and the snobbishintellectuals, and this again is perhaps reflected in their academicchoice of subjects is already noted. The USA does not seem tohave such deep-rooted intellectual rivalries, and, typical of itsinstrument companies, Technicon Instrument Corporationwere able to capitalize on interfacing a whole variety ofdisciplines to fully exploit the instrumentation business. Forinstance, they surmounted the problems of professional secrecyby inviting professionals to contribute to their manuals, publi-cations and international symposia.

Liebig drew parallels between the prosperity ofa nation andthe quantity of sulphuric acid it produced. Perhaps a moreintrinsic study of analytical and control instruments wouldreveal similar conclusions. Dr Lyon Playfair in the 19th centurywas only too well aware of the systematic industrial training ofqualified students in industrial studies in Germany in his reporton industrial construction on the Continent in 1852. Thissituation is somehow reminiscent of the situation prevailing inthe UK engineering industry, and has parallels in the instrumentbusiness in the UK, as Sir Monty Finniston said in his reportEngineering Our Future, 1980:

Inventive talents have not been harnessed effectively bymanufacturing industry because, compared withContinental Europe and the large part ofthe world whichhas followed its lead, there have been neither the pe-cuniary rewards in this country to attract sufficient of thebrightest national talents into engineering in industry...

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