LABORATORY
OF THE MONTH
A n a l y t i c a l Section Plays a M a j o r Role in Conoco's Research a n d D e v e l o p m e n t D e p a r t m e n t T H E
ANALYTICAL
RESEARCH
SEC-
TION of Continental Oil's r e -
cently expanded research laboratories a t Ponca City, Okla., engages nearly 1 5 % of the professional personnel a t the laboratories. T h e section is p a r t of the Research Services Division of the company's R e search a n d Development D e p a r t ment. I t basically provides analytical support, method development, and analytical research to the Research and Development D e p a r t ment. T o some extent, however, these efforts are carried over into all segments of Conoco's operations. Much method development work is done on behalf of t h e company's petrochemical operations in L a k e Charles, La., Baltimore, Md., and Chicago, 111. At present Conoco's Ponca City research laboratories cover 200,000 square feet of space in 11 buildings. A majority of t h e personnel a n d most of the analytical section—except those people concerned with analytical radiation work—are located in the main research building which, during 1961-62, was doubled in size a t a cost of $2.2 million. I n addition t o a radiation laboratory, other auxiliary facilities in t h e Ponca City Research Center include a semiworks operations building, oil exploration laboratories, a plastics laboratory, various shop a n d service buildings, and a unique r e search pilot p l a n t built around a n 80,000-barrel storage tank. The analytical section's support work varies from simple analyses run routinely a t the rate of hundreds per day to very complex and difficult samples which m a y take weeks or months t o analyze. Method development involves both modification of analytical techniques for routine use b y non-professional personnel in the research and other departments of the comp a n y and finding methods t o analyze new materials which come from
New wing of Continental Oil's research building is shown here. Research Section occupies the entire second floor of this wing
other parts of the research department. Analytical research work attempts t o anticipate needs b y gaining basic analytical knowledge which is " p u t in the bank." The whole Analytical Research Section is aimed a t those areas where method development needs m a y occur. I t is organized into five groups by technique rather than by function; separations analysis—gas and other chromatography and distillation; spectroscopy—IR, UV, N M R , x-ray diffraction and fluorescence, emission, and atomic absorption; chemical analysis—organic, inorganic, a n d surfactants; mass spectrometry—electron diffraction, light a n d electron microscopy as well as mass spectrometry; a n d analytical instrumentation. Each of the groups divides its time in a
The Analytical
variable manner between support, method developments, and research as needs indicate. Although Conoco's analytical section as a separate section is little more t h a n a decade old, i t has been able t o apply some of the newest techniques quickly without neglecting basic method development. F o r example, the laboratory was the first to demonstrate the quantitative a p plicability of t h e Lovelock argon gas chromatographic detector and hence, by inference, the quantitative applicability of capillary columns. T h e company also pioneered application of ion pumps to analytical mass spectrometers, a technique adopted by most laboratories to reduce liquid nitrogen cost and increase operating efficiency in mass spectrometers. VOL. 3 6 , N O . 2, FEBRUARY 1 9 6 4
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135 A
Infrared spectroscopy continues to be the work horse of structural characterizations. The unit shown here is fitted with a long path gas cell for studies involving parts per million of acetylene in gaseous reaction mixtures
The mobile instrument analyzer, containing a variety of electronic generating and recording devices, permits the very rapid diagnosis of malfunctions in such instruments as nuclear magnetic resonance spectrometers, mass spectrometers, emission spectrographs, etc. It has been found mandatory to develop rapid methods of "scientific trouble shooti n g " because of the company's heavy investment in and reliance upon instrumental methods of analysis
LABORATORY OF THE MONTH
Time-of-flight mass spectrometer shown coupled with a gas chromatograph permits great speed and versatility in the characterization of complex mixtures 136 A
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ANALYTICAL CHEMISTRY
WACO POWER STIRRER
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The AutoAnalyzer is capable of prodigious speeds on large numbers of similar samples, and it has been applied to the determination of sulfonate level in biodégradation studies. Introduced at Conoco in July, 1963, it has permitted the analysis of 5000 samples at the p.p.m. level by the year's end
Micro-desulfonation apparatus has enabled elucidation of the mechanism of attack of bacteria upon sulfonate and other surfactant molecules. Samples of milligram size are used in this apparatus, with consequent analysis of the desulfonated material by gas chromatography, mass spectrometry, and infrared spectroscopy
The catalytic combustion ionization detector chromatograph was developed in Conoco's laboratories. This special purpose chromatograph shows great promise of being able to qualitatively differentiate between classes of chemical compounds. This is in contrast to the mode of operation of most chromatographs which respond in a strictly quantitative fashion
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WILKENS-ANDERSON CO. 4525 W. DIVISION ST.
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Circle No. 81 on Readers' Service Card VOL.
3 6 , N O . 2, FEBRUARY 1964
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137
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