Analytical chemistry in India

trendsin aaalytical chemtitry,

vol. 7, no. 6,1988

Analytical chemistry in India Mohsin Qureshi and K. G. Varshney Aligarh, India and

Mukhtar A. Khan New Delhi, India

Introduction Analytical chemistry is often considered to be an entirely service activity that is intended to provide qualitative evaluation and quantitative assays of submitted samples. However, while there undoubtedly is a strong service component in chemical analysis, there is also the rigorous and challenging aspect of interdisciplinary communication. In industrial settings analysis is increasingly being required by engineers and decreasingly by chemists. Analytical chemists thus have to explain the chemical transformation taking place in the given reaction to engineers through technical discussions. It is the responsibility of the universities to evolve curricula in analytical chemistry with this end in view. At present Indian universities, in general, can educate chemists only in the fundamentals of theoretical and experimental analytical chemistry and cannot give them professional training for want of suitable equipment, qualified teaching personnel and other facilities. It is here that the universities and industries can collaborate to make analytical chemistry a real tool for the progress of countries such as India. Historical development Prior to 1947, when India was under British rule, most products were imported. As only very few industries existed then there was little demand for quality control of raw materials and products. Since independence, it has been government policy to establish an industrial base in the country. The fertilizer industry, the canning industry and steel produc-

tion for the manufacture of machinery have all flourished. Analytical chemistry in India may be considered to have started with the significant contribution of Prof. P. Ray’ to the field in 1926. He emphasized the importance of organic reagents in inorganic analysis and demonstrated that rubeanic acid (dithiooxamide) could be used for the detection of Cu, Co and Ni. He also introduced another new organic reagent, quinaldic acid. For the next 30 years, however, Indian publications in this field were only 1% of the world total. As a result of the industrial expansion, in 1956 the percentage had increased to 4. Since then only two general review articles2’3 have been published on analytical chemistry in India, one in 1964 and another in 1974. The University Grants Commission periodically publishes status reports on the teaching and research activities of Indian universities in different areas of chemistry. It is unfortunate that these reports have never included the work in analytical chemistry separately. In 1979 for the first time a brief report4 was compiled on inorganic analytical chemistry. The Asian Chemical Society has also commissioned a report on the topic’. The review of Brooks and Smythe6 is of interest in this connection. These workers compared entries in Analytical Abstracts and Chemical Abstracts and were able to calculate the percentage of total activity in chemical research in different countries devoted to analytical chemistry. We have analyzed the entries published in Analytical Abstracts for the year 1986 and these are included in

Table I. Entries for 1965 and 1970 are taken from Brooks and Smythe’s review. It is apparent from Table I that India is far behind in analytical publications compared to advanced countries such as Russia, the U.S.A. and Japan. However, it is trying to close this gap. Present status Graduate and postgraduate courses in analytical chemistry are offered by many Indian universities. Three universities offer graduate courses, whereas 17 offer postgraduate courses and at 16 it is possible to do a PhD course. The Commonwealth directory’ of universities, though published in 1986, is very incomplete and lists only eight universities which teach courses in analytical chemistry. We will discuss some typical cases in detail such as Aligarh, Andhra and Guru Nanak Dev universities. Aligarh Muslim University is one of the oldest Indian universities and is directly controlled by the Government of India. It offers a course on analytical chemistry in the final year

TABLE I. Percentage of analytical work carried out in various countries in the years 1965,197O and 1986. Country

Year 1965

U.S.S:R. U.S.A. Japan Germany U.K. Czechoslovakia France India Scandinavia Romania Poland Spain Netherlands Italy Rest of the world

25.4 15.8 11.0 6.4 4.3 5.3 3.5 3.5 0.7 3.5 4.1 1.8 0.8 3.1 10.8

1970 28.2 17.7 7.7 6.1 5.9 5.6 2.6 2.6 2.1 2.0 1.8 1.5 1.3 14.9

1986 8.1 22.4 10.6 5.9 8.0 1.4 3.2 3.6 1.9 1.4 1.5 2.0 2.7 27.3

trends in analyticalchemistry, vol. 730. 6,198s

194 of graduation which includes evaluation of analytical data, solvent extraction, chromatography, absorption spectroscopy and titrimetry. The MSc programme is of two year duration. In the first year all branches of chemistry such as analytical, inorganic, organic and physical chemistry are studied. In analytical chemistry the topics covered are as follows: errors in quantitative analysis, metal complex equilibria, acid-base equilibria, adsorption and partition chromatography, ion exchange, gas chromatography, electrophoresis, gel permeation chromatography, principles of polarographic and spectrometric analyses, and a laboratory course comprising modern techniques. At the MSc 2nd year level there are six courses in each branch and none is common to all. For those who wish to specialize in analytical chemistry, there are courses on acidbase equilibria, nuclear radiation methods, thermoanalytical methods, X-ray methods, theoretical aspects of ion exchange, electroanalytical methods of analysis, and a laboratory course based on the instrumental methods of analysis only. Andhra University is a state university situated at Waltair in the state of Andhra Pradesh. Here also, the MSc programme is of two years duration and in the first year there are four branches for specialization such as analytical and nuclear, inorganic, organic and physical chemistry. In the second year of analytical and nuclear chemistry there are four courses: sampling and separation methods, traditional analytical methods, applied analysis, and instrumental methods. Guru Nanak Dev University is another young and upcoming state University situated at Amritsar in the state of Punjab. It offers a diploma course in instrumental and chemical analysis and an MSc (chemistry) course in instrumental analysis. University research programmes

The research programme in Indian universities is a two step process. Students registering for their PhD degree must first complete a M.Phil. course. For this course they have to sit for two written papers (one exter-

Fig. 1. Dr. K. G. Varshney (right) with his research colleague Dr. A. Lal.

nal and one internal) on topics assigned by the supervisor and approved by the Board of Studies of the department, the Committee for Advanced Studies and Research (CASR) and finally by the Academic Council. They have to complete the experimental work and submit a dissertation on the topic assigned by the supervisor. Finally, they defend their dissertation before an external examiner. When all these requirements are completed the candidate is awarded the M.Phil. degree. The minimum period in which this degree can be obtained is one year. The students who do not wish to pursue their research any further, or who do not have sufficient aptitude for research, drop out at this stage. For the PhD degree the candidate has to do research for a minimum period of two years before submitting a thesis. The thesis is evaluated by two examiners as well as the candidate’s supervisor. One of the two examiners is generally a foreigner from an advanced country. Examiners are appointed by the Vice Chancellor of the university from a panel of six examiners approved by the Board of Studies. The research grants are generally funded by a number of agencies such as the University Grants Commission (UGC), the Council of Scientific and Industrial Research (CSIR), the Indian Council of Agricultural Re-

search (ICAR), the Indian Council of Medicinal Research (ICMR), the Department of Science and Technology (DST), the Department of Atomic Energy (DAE), the State Councils of Science & Technology (SCST) and the Ministry of Environmental Sciences, etc. Centres of research

Research in analytical chemistry is carried out in a number of centres/institutes/universities. Depending upon the nature of the samples analyzed the analysis is sometimes classified as organic and inorganic. Research work in organic analysis has been confined to only a few centres. At Aligarh methods have been developed for the detection and determination of organic functional groups such as esters, amides, imides, anilides, aldehydes and ketones. Other developing centres for organic research are the Jabalpur and Himachal Pradesh universities. Andhra university has pioneered in food and drug analysis. The work being carried out in India on inorganic analytical chemistry is summarized in Table II. As it is clear from Table II there are a few well established centres of research in analytical chemistry in addition to the universities. Two centres deserve special mention the Bhabha Atomic Research Centre

trends in analytical chemistry,

195

vol. 7, no. 61988

(BARC), Bombay and the Regional Research Laboratory (RRL), Hyderabad. The BARC has had a separate analytical division since 1958 to help geologists in assaying the available resources of nuclear raw materials. It has developed methods for the determination of trace impurities at ppm and ppb levels. Some of the techniques used are molecular absorption and fluorescence, atomic absorption and fluorescence, thermal emission spectrophotometry, thermal neutron activation analysis, mass spectrometry, and electrochemical techniques. The BARC runs a training school in which a course on analytical chemistry is an essential constituent. The students must have at least an MSc degree before being admitted to this training course. The central library of this centre has a very large number of books and journals (1701 periodicals, of which 1388 are on a subscription basis, 142 on an exchange basis and 171 are received free). Most of the journals related to analytical chemistry are subscribed to. The centre has developed a know how for the manufacture of some instruments such as gas chromatographs, pH-meters, polarographs etc. In RRL Hyderabad the Analytical Chemistry Division was established

TABLE

II. Research centres in analytical chemistry

Centre

Major research activities

Bhabha Atomic Research Centre, Bombay Regional Research Laboratory, Hyderabad

Radiochemical analysis Analysis of oils, fats, drugs, pesticides, coal etc Solvent extraction, synthetic inorganic ion exchangers Determination of platinum metals Adsorption indicators

Visva Bharati University,

Santiniketan

Kurukshetra University, Kurukshetra Rajasthan University, Jaipur Industrial Toxicological Research Centre, Lucknow Central Drug Research Institute, Lucknow Aligarh Muslim University

I.T.T. Bombay Roorkee University, Roorkee Allahahad University, Allahahad

in 1954. This division deals with the

analysis of oils, fats, drugs, pesticides, coal etc. The RRL interacts with educational institutions as well as with industries. It has developed know how for the synthesis of industrial product such as glyoxal. It is helping various industries in setting up quality control centres and in training their personnel. In addition to the BARC and RRL, which interact with industries, there are at least three major universities -Guru Nanak Dev, Raipur

Atomic absorption spectrometry HPLC Synthetic inorganic ion exchangers, charge transfer processes, environmental Solvent extraction Solvent extraction Spectrophotometry, ring oven technique

and South Gujaratwhere analytical chemistry students interact with people from industries. The Guru Nanak Dev University awards an MSc degree in instrumental analysis. The students who pass from this university are absorbed by the industries. Short trips are arranged for the students from time to time to apprise them of the nature of the work being done in industries. In Raipur the students interact with the Bhilai Steel Plant and try to solve the problems faced there. The students of the South Gujarat University are sent right from the start of their MSc course for training at the various R&D laboratories of big complexes for instance KRIBHCO Fertilizers. The industrial complexes offer cooperation in this venture.

Current trends In order to get an idea of the current trends in analytical research in India, the papers abstracted in the Analytical Abstracts for the year 1986 were examined. These papers were then divided into various categories based on the topics on which reviews appeared in the April 1986 issue of Analytical Chemistry. AS

Fig. 2. Dr. Pushkin M. Qureshi (extreme right), Lecturer, with his research students in the Analytical Research Laboratory of the Chemistry Department, Aligarh Muslim University.

many as 177 papers out of a total of 468 were covered in this classification. If we assume that the topics in the April 1986 review of Analytical Chemistry represent the mainstream of analytical research, then only

trendsin analyticalchemistry, vol. 7, RO.6,1988

196

tron spectroscopy and organic elemental analysis. These areas need to be strengthened.

Problems

Fig. 3. Analytical research laboratory of Dr. K. G. Varshney, Faculty of Engineering and Technology, Aligarh Muslim University.

about 38% of the total 1986 Indian research output is in it. To include the rest of the papers seven topics marked with an asterisk were added. The final percent distribution of papers on different topics is given in Table III. It is apparent that most of the analytical research in India is done in spectrophotometry. Spectrophotometers are now commercially available in India at a modest price and the work is not based on any complicated theoretical basis. Most TABLE III. Percent topic-wise

distribution

of this work was on food and drug analysis. The second most popular field of activity is radiochemistry where the main contribution is from the BARC, Bombay. Thin-layer and paper chromatography occupy the third position. Almost no work has been reported on Mossbauer spectroscopy, functional group analysis, electron spin resonance, emission spectrometry and surface analysis. A negligible number of papers were published on thermal analysis, elec-

of papers from India abstracted

in Analyti-

cal Abstracts in 1986 Topic

Percentage

Spectrophotometry Nuclear and radiochemical analysis Thin layer and paper chromatography Column liquid chromatography Electrical methods of analysis Titrimetry Solvent extraction Gas chromatography Atomic absorption, atomic fluorescence and flame emission spectrometry Ion exchange Complexometry Trace analysis Ion selective electrodes X-ray spectrometry Kinetic determination and some aspects of analytical chemistry Mass spectrometry Molecular fluorescence, phosphorescence and chemisorption spectroscopy

40.4 11.1 9.4 7.1 6.2 5.4 4.1 2.8 1.9 1.9 1.7 1.3 1.1 1.1 0.9 0.6 0.6

Analytical chemistry is a relatively new discipline and has no chairs of its own in Indian universities. Due to the lack of properly trained personnel the topics in analytical chemistry are generally taught by teachers who have specialized in physical, organic and inorganic chemistry. Full justice is therefore not done to the subject and it is growing haphazardly. As more and more industries are opting for instrumental methods it is necessary to strengthen the teaching of this subject in the universities. However, most universities cannot afford to buy costly instruments. In some universities, these instruments are available but they do not work properly because of the lack of repair and maintenance facilities. The second major problem is the shortage of good and cheaper books on analytical chemistry. The books available are generally by foreign authors and are very expensive. Another major problem in India is the lack of proper research and development (R&D) laboratories in many industries. Though many industries utilize analytical chemistry for their quality control programme much R&D work has not been taken up by many of them. As a result they adopt very tedious procedures for routine analyses or compromise on quality. Some industries are either unable or unwilling to equip their quality control laboratories with modern instruments. This, together with a lack of committed and qualified analysts, reflects in quality control. In conclusion it may be pointed out that the cloud does have a silver lining. Good books written by some Indian authors are becoming available. The formation of the Indian Society of Analytical Scientists (ISAS) in 1980 has promoted the interests of analytical chemistry through a number of successful symposia which have increased awareness in the scientific community about the analytical sciences.

197

trends in analytical chemistry, vol. 7, no. 6, I988

References P. Ray and R. M. Ray, J. Ind. Chem. Sot., 3 (1926) 118. P. Ray, Fifty Years of Science in IndiaProgress in Chemistry, Indian Science Congress Association, Calcutta, 1984. R. D. Tiwari and A. K. Dey, A Decade (1963-72) of Science in India - Progress of Chemistry, Indian ‘Science

Congress Association,

Calcutta, 1974.

Report on the Status of Chemistry in Indian Universities, University Grants

Commission, New Delhi, 1979. M. N. Sastri, Relevence of Analytical

Chemistry, 3rd ISAS National Symposium, Waltair, 1986. 6 R. R. Brooks and L. P. Smythe, Talanta, 22 (1975) 495. Year Universities 7 Commonwealth Book 1986, Association of Common-

wealth Universities,

London, 1986.

Professor Mohsin Qureshi is an Emeritus Scientist of the Council of Scientific and Industrial Research, India. He received his PhD degree in Analytical Chemistry from the Louisiana State University with Professor P. W. West in 1958 and initiated

a course in Analytical Chemistry at the MSc level in 1963 in the Aligarh Muslim University. Dr. K. G. Varshney and Dr. Mukhtar A. Khan received their PhD degrees in Analytical Chemistry from the Aligarh Muslim University working with Professor Qureshi. Mohsin Qureshi and K. G. Varshney are at the Department of Applied Chemistry, Faculty of Engineering and Technology, Aligarh Muslim University, Aligarh202001, India. Mukhtar A. Khan is at the Department of Chemistry, Jamia Millia Islamia, New Dehli, India.

in the

news Data treatment in atomic spectroscopy Chemometric techniques for data evaluation and processing are increasingly been used in the analytical laboratory. Often the necessary software is already provided in the computerized commercial instrument, thereby allowing the analyst to use mathematical procedures without having to understand their fundamentals. In general, despite the rapid growth of chemometrics, there is a significant lack of knowledge about these techniques among members of the analytical community even those in analytical research, as can be seen from the literature. One obvious reason is the gap between scientific progress and university curricula. Thus even today the probability is high that an analytical graduate does not know much about the mathematical techniques for evaluating and processing analytical results. One way to help solve this problem is to offer postgraduate courses, which primarily address the analyst in the laboratory, but also those who are interested in obtaining a basic knowledge of the methods now available. The Working Group for Atomic Spectroscopy of the Austrian Society for Microchemistry and Analytical Chemistry, recently organized a one-

week course (22-26 February 1988) on data evaluation in atomic spectroscopy at The Technical University Graz. The course was prepared by Wolfhard Wegscheider (Graz) and Matthias Otto (Freiberg), two internationally respected experts on chemometrics. Wegscheider and Otto also gave most of the lectures themselves, which was fortunate as in the frequent question-and-answer sessions their profound and wide knowledge proved invaluable. Attendance was limited to 17 participants, who came mainly from industry. The course provided an excellent combination of discussion on the basics of a mathematical approach and hands-on computer work doing actual data evaluation. For this purpose the STATGRAPHICS@ program (STSC Inc. Rockville, MD, U.S.A.) was mainly used. For the demonstration of some chemometric techniques, the program CLEOPATRA@ (Kateman et al., Elsevier, Amsterdam, the Netherlands) proved very useful. As part of the general philosophy of this course, the basic mathematical operations for data evaluation and processing were presented in a problem-oriented approach. This naturally guided the selection of the

topics, which included most of chemometric techniques used today in the laboratory: linear and non-linear regression, regression diagnostics, robust regression, confidence intervals for calibration of analytical measurements; statistical methods for determination of sampling errors, control charts and evaluation of round robin tests; principles and techniques for experimental design; information theory and description of target values, e.g. by fuzzy methods; optimization by models or search methods like SIMPLEX, response surfaces or non-linear regression; processing of spectra by smoothing, filtering, differentiation and cross correlation; multivariate data evaluation by pattern recognition, clustering, linear discrimination analysis, projection methods, eigenvalue and principal component analysis, factor analysis, target factor analysis; and expert systems. Due to the wide scope of the program, most of these topics were covered in a fundamental manner. Relevant literature was recommended for each section so that graduates of the course can pursue their special interests further. Overall the course was found to be very useful by all participants. How important such teaching