An experiment ’in education for automatic analysis

An experiment ’in education forautomatic analysisD. Betteridge

Chemistry Department, University College of Swansea, Swansea SA2 8PP, U.K.

In July 1979 a Summer School in Automatic Analysis wasorganised by D.G. Porter, P.B. Stockwell, both of theLaboratory of the Government Chemist, and the author,under the auspices of the Royal Institute of Chemistry]Chemical Society. Its prime objective was to provide anup-to-date account of the philosophy and practice of autom-atic analysis. The audience was drawn mainly from industryand the school lasted for one week. To the best of our know-ledge it was the first attempt to provide a course of theoryand experiment on all aspects of automatic analysis.

Preliminary discussions when planning the school showedthat there is no consensus about what constitutes an educationin automatic analysis and how it is obtained, although it isundoubtedly one of the most important issues of contem-porary analytical chemistry. This article attempts to definethe scope of the challenge, in the light of the experiencegained in July’s experiment in education.

Organisation of the summer schoolThe Summer School comprised a series of lectures, tutorials,practical exercises and demonstrations of equipment. Theoverall content and balance is indicated in Table 1.

LecturesThe lecturers were briefed to be clear and to deal with thefundamentals; to teach not to present a research paper. Theexception was Professor Denton who was asked to .let rip ashe wished, and whose lecture on the future of automationwas outstanding. The rest of the lectures, albeit many dealingwith the most recent developments, were presented so as tobe of immediate practical value to the participants.

TutorialsThe tutorials, or small group discussions, were of two kinds.One set was arranged by the indicated preferences of theparticipants, who then had the opportunity for discussingtheir specific problems with an expert. The other, with fixedgroups and tutor, was devoted to the course problem. Thiswas based on the experience of the Laboratory of theGovernment Chemist in automating the analysis of cigarettesto measure their tar, nicotine and carbon monoxide levels.There were eight groups with five students in each and theyall independently worked out a solution to the problem.Then a snowballing procedure was adopted to present thebest of the individual efforts for discussion. First the(primary) groups were combined to give three (secondary)groups of 15 (or more accurately 2x15 and lxl0). Theprimary groups had appointed a spokesman to present thegroup view and the secondary groups in turn nominated aspokesman to represent their group’s views. Finally thesethree spokesmen presented the views of the combined groupsto the whole school. The procedure ensured that discussionat the end was relevant, and organised. Furthermore therewas considerable interest in finding out what the others hadworked out. As an additional bonus, the presentations werevaried, amusing and of a very high standard. It is clear thatsnowballing is excellent for group discussions, it allowseveryone to express his views (simultaneously, but indifferent rooms) and ensures that the discussion en masse is

Table 1. Organisation of Summer School

Form of teaching

Lectures

Tutorials

Practicals

Time allocated

16x45 min12hrs

(a) Courseproblem3x45 min

(b) Specialist4x45 minTotal-51/4 hrs

(a) Fixed exer-cises 4x11/2 hr

(b) Free choice2xl hr

+ Wed.afternoonTotal=(6+3)hr

Instructors

H. Bartels, Discrete analysersD. Betteridge, MicroprocessorsG.K.E. Copeland, TobaccoSmoke Problem

D.R. Deans, GLCM.B. Denton, Spectrochemicalmethods, Future of auto-mation

J.K. Foreman, ManagementE.H. Hansen, Flow injectionanalysis

F.L. Mitchell, Introduction toAutomation, New Tech-niques in Clinical analysis

H.L. Pardue, New Electronics,Kinetics

D.G. Porter, Make or BuyJ. Ruzicka, Flow injection

analysisP.G. Sauders, ClinicalP.B. Stockwell, Computeris-ation or Automation?

Lecturers andT. Alliston, B. Karlberg,I. Scott, J.M. Skinner,I. Telford

Beckman, Bifok, Chem LabC.I. Electronics, E.D.T,Mettler, Phase Separations,Pye, Spectra Physics, Tech-nicon, Varian, Vickers,Laboratory of the GovernmentChemist, ICI Petrochemicals.

neither dominated by extroverts with an axe to grind norfalls flat because people are overawed by the occasion.

PracticalsThe practical sessions were organised with the objectives ofgiving participants experience of a wide variety of automatedinstrumentation, and providing opportunities for discussingpractical matters in depth, both with the. representativesof the manufacturers and with independent experts, i.e. thecourse lecturers and tutors. With so many companies beingrepresented it was impossible to give everybody ’hands on’experience of every instrument, but the combination of aformal allocation of experiments for some of the time and afree choice for the rest of the time satisfied most people. Themanufacturers also, in the main, entered into the spirit of theschool and this was much appreciated by the participants.The manufacturers also benefitted from having a captiveaudience and being able to discuss their instruments on aone to one basis in more calmer surroundings than a,n

exhibition hall. They learnt a lot about their customers and

Volume No. 5 October 1979 249

Betteridge Experiment in education

)- IDEFINE PROBLEN

PREPARE SANPLE

CREATE OR ISOLATE DETECTABLE SPECIES

tDATA COLLECTION

tDATA PROCESSING --),--I

RECORD OF RESULTS

Figure 1. A general scheme ofautomated analysis.

their needs, and thus the school may be of long term benefitto all in automation.

Student responseAnalysis of the course evaluation questionnaires completedby the students showed an extremely high level of approval.Thus it may be assumed that the objectives of the SummerSchool were met, but, like all good experiments, it raisedmany questions and provoked a number of reflections on thetheme of ’education in automation’.

Reflections on the educational significanceof the Summer SchoolIt has been argued elsewhere that successful developments inanalytical chemistry take place as a consequence of dynamicinteraction between theory, technique and analyticalproblems [1]. This led to the concept of the ’AnalyticalTrinity’ and logo:

Technique Theory

Problem

It provides a convenient framework in which to discuss the

achievements of the Summer School and the lessons to belearnt from it.

TheoryA uniform approach to the theory of automatic analysis wasmost notable by its absence. The elements of a completetheory were often discussed, and indeed a very usefuldiagram (Figure 1) summarising the various aspects ofautomation was presented, in several forms by a numberof lecturers. However, most lectures were concerned withone particular aspect to the exclusion of others. A moregenerally accepted theory would help define and developautomatic analysis as a separate branch of analytical chemistry.This represents a challenge for the future.

One criterion for automatic analysis as defined by theIUPAC definition, is the presence of a feedback loop in thesystem. This seems a rather facile basis for characterisation.For most people the chief interest and distinguishing featureof automation is the capability of producing a large numberof results with a high rate of sample throughput, usuallyfor long periods. The motivation for setting up such ananalytical service may be political, managerial or scientific,but, in all cases, the cost and organisation of the analysis areon a much greater scale than conventional manual analyses.In automated systems the amount of data generated alsoposes a number of implications. On the one hand, it must beprocessed and presented in a useable form, on the other, itcan be used to help improve the analytical step (optimis-ation), to refine the initial statement of the problem and tomaintain a continuous statistical check on the quality of theanalysis. The reliability of results and the stability ofapparatus is of greater significance with automatic analysisthan with conventional. Hence, there is an additionalanalytical factor. Thus, those specialising in the design anddevelopment of automatic analysis instruments need to havea grounding in systems analysis, operational research, marketresearch, network analysis, statistics, data processing,optimisation techniques and electronics in addition to thestandard analytical techniques.

This may seem to over emphasise the problem but is isobvious that for chemists entering automation the noveltieslie in management aspects and data processing.

It was often said during the school, that the definition ofthe problem was the most difficult part of the analysis,because of the economic and management problems associatedwith its solution. This was aptly illustrated by the courseproblem. Every tutorial group had great difficulty in decidinghow, and on what basis, representative samples were to betaken and how the analytical results for each sample were tobe recorded, collated and reported. It was a far cry fromconventional analytical chemistry. Similarly, the excitingglimpses of what can now be achieved in the realms of datacollection and evaluation showed what could be gained byapplying advanced computational techniques to analysis.For example the introduction of Vidicon detectors enablesets of spectra to be taken at 10 m sec intervals over a periodof sec, this produces 100 spectra from which plots ofabsorbance as a function of time at various wavelengths canbe reconstructed. Also Simplex optimisation methods canbe used to set up the operating parameters of a complexapparatus to provide the maximum signal output.

All of the basic theory is currently available, from this thebasic theory for automatic analysis must be synthesised. Theresult must be rigorous enough to underpin and effectivelydefine automatic analysis, but it must be simple enough to beunderstood and readily accepted. Given the tendency forspecialists in management and the mathematical skills toconfuse straightforward ideas with jargon and equations,presentation of automation theory will not be easy. Thelectures given during this summer school however provedthat it can and should be done.

250 Journal of Automatic Chemistry

Betteridge Experiment in education

TechniqueThere is no doubt that the Autoanalyser, Gemsaec, theAutolab and similar devices are of the utmost importance inanalytical laboratories requiring a high sample throughput.There is equally, no doubt that they are far too expensivefor undergraduate teaching laboratories.

To an academic, therefore, one of the most cheeringfeatures of the course was the demonstration of what couldbe done with DIY apparatus. For example a solvent extractionapparatus based on solenoid operated valves and developedin house by an automation development team was described.The construction of such an apparatus would be a worth-while academic project, whilst its routine use would makebasic, but tedious, experiments on solvent extraction possible.

The principles of continuous flow analysis are very welldemonstrated by flow injection analysis, and this techniquecan also be introduced on a DIY basis.

The easily programmed microcomputer will also have asignificant impact on the teaching of automated analysis. It isnot difficult to envisage projects to develop automaticdiscrete analysers or to control continuous flow systemsbeing based on interfacing minicomputers to readily availablesimple instruments.

Thus, there is considerable scope for the introduction ofautomated analysis into undergraduate teaching, and thereare many advantages to be gained. Experience with flowinjection analysis at the author’s laboratory shows that thestudents find it interesting, that important chemical principlesare illustrated simply and that it helps to have a high samplethroughput. The speed of analysis results in a saving oninstrumentation one piece of FIA apparatus set up for aphotometric determination can be used in one lab period bymany more students than a spectrophotometer. It also meansthat the analytical results can be analysed statistically andthat this important subject can be introduced to the studentswith the minimum of pain.

ProblemsOn the course, one of the most valuable educational exerciseswas derived from the course problem. It brought home tothe students the true complexity of modern analysis. Theintroductory statement of the objective is simple enough:’As a member of the ’Transautomatia’ Government Analyst’slaboratory you have been asked to undertake work todetermine the tar, nicotine and carbon monoxide levelsproduced by cigarettes available on the home market. Thisrequires a carefully standardised and reproducible approachif the results are to be of value for comparative purposes.The Government wishes to publish twice yearly leaguetables similar in format to those produced by the UK govern-ment. These list the brands available in ascending order oftar level, grouping them in mg increments, and should alsoshow both nicotine and CO values. There are around 120-150different cigarette brands currently available on theTransautomatia market’. The individuals were asked todevelop a strategy for automating the analyses required.

However, it soon becomes apparent that the analyst has tobe content with an arbitrary definition of tar, variability ofthe same brand of cigarette, the humidity, the variation oflength of tobacco and filter and the need to establish a repro-ducible and reasonable puff profile.A full account of one solution is given by Copeland and

Stockwell [2]. Since the introduction of league tables oftar content, the pattern of smoking in the UK has changedsignificantly, cigarettes With low tar content being morefavoured than before. This demonstrates rather well, thesocial and economic significance of analysis.

It was a challenging exercise and opinion was divided as .toits worth, some thought it was a waste of time, others ratedit the best part of the course. It has the merit of focussingthe students’ attention to a real world problem and to use the

Volume No. 5 October 1979

ConclusionsThe lectures covered a wide range of topics and dealt withthe more routine issues as well as novel techniques andinstrumentation recently introduced. The tutorials andpractical sessions enabled participants to discuss their ownspecific problems in depth and the course problem broughtout many useful points and stimulated considerablediscussion. Overall, the blend of theory, techniques andproblems was such that most of the participants felt they hadclearly benefitted. As an experiment in education by meansof the short course it must be counted a success.

The stimulus provided by the interdisciplinary combinationof management skills, science and technology was summarisedfor all, not just laboratory managers, by the concludingremarks of the opening lecture by J.K. Foreman:’Perhaps the most significant problem the laboratory managerhas concerns himself. To launch a laboratory into anautomatic regime satisfactorily is a considerable achievement,involving, as has been summarised above, much learning andchange of attitude. But he must stay abreast of developmentin his new arena. We have only just begun to extract, in anysort of cost-effective way, the maximum valuable informationcontained in a sample. Further developments in automationtechnology, if correctly oriented, are a powerful way ofcontinuing this process and the laboratory manager’s role init can be a challenging and rewarding one’.

It may be that in the future this Summer School will bedesignated as the place where the concepts in education forautomation began to gel.

REFERENCES[1 Betteridge, D, Analytical Chemistry, 1976, 48, 1034A.[2] Copeland, G.K.E. and P.B. Stockwell in "Topics of Automated

Chemical Analysis". Volume 1. Eds. P.B. Stockwell and J.K.Foreman, 1979 Horwood, Chichester.

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