LABORATORY
OF THE MONTH
University in the Netherlands Has M o d e r n Instrumental Analysis Division
Contemporary architectural design is a distinctive feature of the Technical University at Eindhoven. Glass walls, used throughout, ensure maximum light. The University was founded in 1956. In 1966 the erection of 13 buildings will complete the first stage of the building program. The three major areas of engineering, chemi cal, mechanical, and electrical, are taught. The Chem ical Engineering Department's 500 students occupy five buildings: an 80,000 sq. f t . freshmen chemistry build ing; a 130,000 sq. f t . main chemistry building housing organic, inorganic, and physical chemistry and instru mental analysis divisions; two 60,000 sq. f t . buildings,
one for unit operations and process engineering, and one for chemical engineering and reactor design; and a build ing for high pressure reaction studies. There is a central auditorium/lecture hall capable of seating 1200 people as well as 12 smaller lecture theatres throughout the campus. The University expects over 3 0 0 0 students to attend by 1968. A novel feature of the design is the series of connecting "air bridges" between the buildings. These not only serve as convenient walkways during in clement weather, but, more important, equipment can be moved from one area to another without the necessity of negotiating steps
and imaginative attitude toward higher technical education in the Netherlands is no better ex emplified than by the Instrumental Analysis Division of the Technical University's Chemical Engineering Department in Eindhoven. A wide range of up-to-date equipment coupled with a dynamic program of undergraduate and graduate study in modern surroundings make the work there of the highest quality. The "Technische Hogeschool" at Eindhoven is one of ten institutes for higher education in Holland and comes under the university system of the Netherlands. Founded as re cently as 1956, the first phase of the building program that
began in 1957 will be complete by 1966. Originally designed for 1000 students in chemical, mechanical, and electrical en gineering, the university is expected to exceed 3000 students by 1968. The chemical engineering department now has 500 students but will probably have 800 by 1970. The Instrumental Analysis division under the direction of Prof. A. I. M. Keulemans is one of eight occupying the five buildings of the Chemical Engineering Department. These buildings cost over one third of the $30 million spent on the campus to date. Equipping the Instrumental Analysis di vision alone has cost over $500 thousand. The total capital laid aside for instruments and equipment in the Chemical
Τ Ή Ε PROGRESSIVE
VOL 35, NO. 11, OCTOBER 1963
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115 A
Gas chromatographic investigations are carried out in this laboratory, one of many for graduate students in instrumental analysis. Here specially designed instru ments permit more accurate measurements than are often possible using commercially available apparatus. Gradu
ate courses place considerable emphasis on sponsoring inventiveness and adaptability in the students. There are 20 students working toward their doctorate in chemical engineering, seven of whom will take their doctorate in instrumental analysis by next year
Engineering D e p a r t m e n t during 1Θ57 to 1965 is about $3.3 million. Prof. Keulemans, who was appointed to his present posi tion after nearly 25 years with Royal D u t c h Shell, has been given every opportunity of equipping his division with the most up-to-date analytical tools available. These include an extensive range of instruments for gas chromatographic analysis, a mass spectrometer, two Zeiss spectrophotometers, two automatic ultraviolet spectrophotometers and five au tomatic infrared spectrophotometers, a nuclear magnetic resonance instrument with permanent magnet, a n d an in strument for atomic absorption studies. There is also an extensive variety of a p p a r a t u s for analytical distillation, counter-current extraction, and electroanalysis. I n addition, the Instrumental Analysis Division uses the services of the Chemical Engineering D e p a r t m e n t ' s up-todate instrument and glass-blowing shops. T h e staff and students have designed and built special equipment for analytical studies. These include ultra high efficient stills for improved analytical rectification, gas chromatography detectors, devices for preparing gas streams of extremely low concentrations of organic vapors used in the calibration of such detectors and in studying performance characteristics of organic compounds. A new detector for mass spectrometry is currently under construction. The improvements in analytical tools should provide an
important stimulus to the development of physico-chemical theories. I t is now possible to detail the products of chemi cal reactions which previously could n o t be studied with such a high degree of accuracy. Studies currently under way are the detailed investigation of elimination reactions such as pyrolysis of acetates and the catalytic dehydration of alcohols. Prof. Keulemans points out t h a t students a t all levels, from undergraduates to P h . D . candidates, have-the oppor tunity to use the best analytical tools available. And they are encouraged and expected to design their own equip ment to fill specific needs. Research is carried out mainly in the field of natural prod ucts such as petroleum fractions and flavors. T h e work generally falls into two categories. One is the study and improvement of physical methods of separation involving all phases of chromatography and analytical distillation. The other is concerned with structure determination and identification. A long term research program t h a t Prof. Keulemans ini tiated is the accumulation of precise gas chromatography profiles for a wide range of organic compounds. T h e work is still in its initial stage of checking gas chromatography characteristics of these classes of compounds which differ in their functional group. F o r instance alkanes, olefins, ketones, esters, ethers, etc. are being investigated. H e esti-
116 A
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ANALYTICAL CHEMISTRY
LABORATORY
OF
ΤHE
MONTH
Both an analog and a digital computer are in use at the University at Eindhoven. These permit rapid and accur ate analyses of statistical measurements and by simu lating reaction equations, aid in the interpretation of chemical processes
mates it will take about two or three years to complete a good starting catalog before being able to launch into a compound-by-compound study of the various classes of compounds. His aim is to have published a series of gas chromatographic charts, issued periodically, to aid in the rapid and accurate identification of all known substances t h a t lend themselves to this t y p e of analysis. There are two full-time staff members working on this project. Stu dents during their regular course work also carry out gas chromatographic analysis on the compounds so t h a t each is subjected to no less t h a n ten analyses. Prof. Keulemans also sees a great need to build u p a good catalog of infrared spectra data for organic compounds based on modern improved techniques and standards. This involves the design of equipment to get complete separation of compounds and their recovery in a pure state. Eventually he hopes to prepare comprehensh r e charts for each com pound showing characteristic gas chromatographic profiles as well as I R , UV, N M R , and mass spectral characteristics. Prof. Keulemans' ambitions m a y seem extraordinarily high. B u t in a country such as the Netherlands where there is such a remarkable drive toward high educational and technical standards, and where the current education budget is higher t h a n any other, including t h a t of defense, the chances of his achieving his goals are not remote. (Continued
on page 118 A)
Distillation columns in the Pilot Operations section of Technical University's Chemical Engineering Depart ment are over 18 feet high and are serviced at the top by means of platforms. Here distillation studies are con ducted with major emphasis on improvement in separation techniques. One simple but effective development is the wrapping of the columns with aluminum foil to ensure maximum retention of heat throughout their length. The foil wrappings have slits to allow viewing during distilla tion. Instrumental control is an important aspect of the distillation units and serves to give students a thorough groundwork in modern industrial distillation procedures VOL. 3 5 , N O . 1 1 , OCTOBER 1 9 6 3
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117 A
LABORATORY OF THE M O N T H
Continued
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1 18 A
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ANALYTICAL CHEMISTRY
The accumulation of reliable gas chromatographic data for a wide range of chemicals is one of the special projects of the Instrumental Analysis division. Two specialists are engaged full time on the project and graduate students also make gas chromatograph measurements which serve to double-check the ac curacy of the results as well as giving them practice in use of the equipment. During the first year of this program over 4 0 simple basic compounds have been analyzed to establish the optimum conditions of temperature, pressure, flow, etc. This work will continue during the next two years during which compounds repre senting alkenes, olefins, ketones, alcohols, esters, ethers, and aromatics will be studied. The ultimate goal is to issue an accurate gas chromatographic diction ary of compounds
