LABORATORY OF THE
MONTH
Kellogg's Chemical Process Research Makes Broad Demands on Analytical Section
Research and Development Laboratory of M. W. Kellogg Co., Division of Pullman, Inc., was moved less than t w o years ago to t h e new Research and Development Center in Piscataway Township, N. J . The Center has nearly two acres of floor space housing a staff of 180 chemists, engineers, and service people working in chemical process research. The building is an assembly of five interconnected units: the administration and office wing in the front, the connecting unit which houses the auditorium, conference rooms and library, the laboratory wing in the rear, the service unit containing machine shop and storeroom, and the unique A-frame pilot plant building capable of holding as many as 3 5 pilot plants from 2 0 to 8 0 feet high
R
ESOURCEFUL
and
imaginative
re-
search is basic t o t h e world-wide operations of T h e M . W . Kellogg C o . This research is responsible -for m a n y of Kellogg's contributions t o process engineering a n d plant construction. A s a vital p a r t n e r of t h e oil industry in the thirties, Kellogg research played a key role in creating a n d developing m a n y of t h e basic processes: fluid catalytic cracking, catalytic reforming, nlkylation, polymerization. These processes, adopted b y t h e industry on a world-wide basis, are presently responsible for t h e majority of t h e world's refined petroleum capacity. M o r e r e cently, t h e development of processes for t h e production of ammonia a n d ethylene a n d t h e extraction of helium from hydrocarbon feedstocks has established n e w standards of efficiency and yield. T h e majority of Kellogg research is chemical process research, involving great d e p t h and b r e a d t h . Unlike p r o d uct research, where investigation is intense b u t t h e corridor is narrow, Kellogg research, to b e productive, must range t h e technologies. T o s u p -
port this t y p e of research, t h e r e is a constant need for developing a great variety of analytical m e t h o d s t o meet the particular accuracy a n d m a n - h o u r requirements faced b y t h e three phases of exploratory, process, a n d pilot plant research. T h e analytical requirements of Kellogg research effort are m e t b y a centralized Analytical Section with a regular staff of 15, occupying 3S00 square feet of laboratory space. Because of the strong dependence on i n s t r u m e n t a tion, t h e l a b o r a t o r y space p e r analytical person is nearly twice t h a t for other technical personnel. T h e Section includes four g r o u p s : Chemical Analysis, Gas C h r o m a t o g r a p h y , I n s t r u m e n t a l Analysis, a n d Chemical a n d Physical Testing. T h e Analytical Section works very closely with the. chemist or engineer right from t h e beginning of a research project. Sampling points and sampling technique a r e discussed: a p p r o p r i a t e analytical m e t h o d s are tailored t o t h e special needs, keeping b o t h accuracy and m a n - h o u r requirements in mind. An example of this cooperation oc-
curred during a recent s t u d y of v a c u u m tower stripping of carbon dioxide from sea water, financed b y t h e Office of Saline W a t e r of t h e U . S. D e p a r t ment of Interior. A special arrangement was worked o u t for sampling liquid under v a c u u m without loss of carbon dioxide through flashing. An A S T M method was adopted to determine carbon dioxide in low p.p.m. range. T o monitor the absolute amount of air leak into t h e tower, a measured q u a n t i t y of helium was a d m i t t e d a n d the ratio of helium to air was determined b y mass spectrometry. T h e Chemical Analysis G r o u p handles nonroutine organic a n d inorganic chemical analysis with t h e use of small instruments such as flame photometer, electroanalyzer, and p H meter. An a p preciable amoTint of time is directed toward analytical research a n d development. F o r instance, a rapid method has been developed for t h e determination of silica in phosphate rock. Aside from handling analytical problems arising out of research endeavor, this group works o u t reliable, simple tests, and trains operators to analyze pilot VOL. 38, NO. 7, JUNE 1966 •
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plant streams on 24-hour operation. T h e Gas Chromatography Laboratory is equipped, with b o t h isothermal and temperature-programmed gas chromatographs with thermal conductivity and flame ionization detectors. There are about 20 gas chromatographs located in various research laboratories. F r e q u e n t assistance is given to chemists a n d engineers to solve t h e problems encountered in the performance of onthe-spot analysis in gas chromatography. To serve pilot plant operations, this group is responsible for setting u p and calibrating stream analyzers such as process chromatograph, modified laboratory chromatograph, density instrument, etc. T h e I n s t r u m e n t a l Analysis Group has installed a new analytical mass spectrometer to replace one purchased more t h a n 20 years ago. T h e new ins t r u m e n t is provided with gas and liquid sample entries a t ambient temperature and a 350° C. inlet system for the introduction of high-boiling liquids and solids. I t has a mass range of 2 to 700, encompassing the range of petroleum and petrochemical samples encountered in our research efforts. Coupled with the use of a computer located in Kellogg's office in New York, the mass spectrometer is a powerful tool, not only in yielding accurate analysis of complicated mixtures b u t also in structure elucidation. T h e laboratory is equipped with a recording spectrophotometer covering the ultraviolet, visible, and near infrared ranges, and both double- and single-beam infrared spectrophotometers. These are used b y research chemists for^ the study of mechanisms of heterogeneous catalysis, and for structure work and functional group analysis by analytical personnel. X - r a y diffraction together with differential thermal analysis is employed to study the change in phases and crystallite sizes of catalysts. These bring to light the factors which affect the catalyst performance under various conditions. The x-ray emission spectrometer is equipped with a pulse height analyzer which discriminates the background noise from the radiation of interest. A method has been developed for the direct determination of metals in petroleum products down to the low p.p.m. range b y this instrument. The Chemical and Physical Testing Group carries out all the necessary testing of petroleum products and their related materials, iron ores, fertilizers, etc. I t handles the control work generated from a large variety of pilot plant operations and routine analysis from research laboratories. Because of widely fluctuating analytical requirements, the equipment in this laboratory far exceeds the manpower available. All analysts permanently assigned are experienced in manipulating 96 A
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ANALYTICAL CHEMISTRY
For a laboratory engaging essentially in petroleum and petrochemical research, a mass spectrometer is essential for multicomponent quantitative analysis and frequently for qualitative analysis. This instrument has a usable mass range up to 700 and is equipped with specially designed gas sampling system, 150° C. liquid entry, and 3 5 0 ° C. inlet for high-boiling liquids and solids
LABORATORY OF THE MONTH
Special analytical methods are developed to handle unusual samples. The components of a calibration gas mixture are accurately determined by wet chemical procedures after reaction in this absorption apparatus
all the equipment and running a wide variety of tests. H e a v y work load and shift work demands are met by temporary transfer of technicians from other divisions. Cracking catalyst is evaluated for activity and selectivity in bench scale fluidized catalytic cracking unit. Iron ore reduction is monitored by reducible oxygen measurement and Dings-Davis magnetic separation. P a r ticle size distribution of fluidizable
powders is determined by Roller analyzer, micro-mesh sieve, Micromerograph, or sedimentation. Atmospheric and vacuum distillation units equipped with u p to 100 theoretical plate fractionation columns handle the fractionation of feeds and products. Two knock test engines are used for octane number measurement. A p p a r a t u s is available for measuring such physical p r o p erties as viscosity, flash point, pour
W AP 1U II - TI E F iM RM A TI P i¥ H h Uft L t ! rP D ft Evaluation of t h e results of a pilot plant program required numerous trace nitrogen determinations. A m o d i f i e d D e v a r d a ' s m e t h o d is c a r r i e d out using this laboratory-built apparatus with which 12 samples may be handled simultaneously
COOLS HEATS ONLY... $440.
Various types a n d sizes o f d i s t i l l a tion apparatus occupy the entire r i g h t w a l l , 9 6 feet, of t h e C h e m i c a l a n d Physical T e s t i n g Laboratory. These u n i t s a r e used in p r e p a r i n g feedstocks for pilot plant studies, topping and fractionating products for t e s t i n g , a n d c a r r y i n g o u t A S T M distillation tests
SEVEN WAYS B E T ! Heats and Cools—almost double the range of the average visibility bath. Accuracy — constant temperature at any level from — 10°C t o + 6 5 ° C ± . 0 1 ° C — ideal where precise temperature control is required. 3 Large Capacity—coils fit snug against the bottom, the entire volume of the jar is usable. Glass jar permits fast observa, tion. ! Compact — only 20V->" wide 27 y 2 " high. Saves space. Fits on any lab table or desk. Self-contained — heating controls, cooling compressor, all ' parts are housed in this compact unit. Low Maintenance —Waco LoTemp has been proved troublefree by laboratories from coast to coast. Low Price — $440.00. Specify: No. 882 Waco Lo-Temp Refrigerated Bath, complete with Pyrex jar 1 2 " in diameter, for 115 volt 50/60 cycle AC
1 2 Pilot plant operator s h o w n is b e i n g t r a i n e d t o use a l a b o r a t o r y g a s c h r o m a t o g r a p h . T h e i n s t r u m e n t is set u p to measure accurately the main product p r e s e n t i n c o n c e n t r a t i o n s o f less t h a n 1 % o f t h e p r o d u c t s t r e a m . Because o f t h e large n u m b e r o f inexperienced operators involved a n d t h e unstable instrument conditions, internal standard techniques are usually employed for such purposes
4 5 6
7 point, surface tension, and color. Chemical analyses include bromine n u m b e r b y electromctric t i t r a t i o n , carbon and sulfur by combustion, Orsat analysis, etc. Kellogg's engineering departments frequently call on the Analytical Section to carry out special assignments in connection with problems arising in t h e design or operation of Kellogg-built plants. Analytical m e t h o d s are s u p -
plied in connection with setting of p r o d u c t specification guarantees. Corrosion samples a n d fouling deposits are analyzed and the analyses are interpreted. Special sampling devices have been constructed for sampling multiphase p l a n t streams. T h e Analytical Section m a y send an experienced technician, for example, t o a refinery to sample t h e product s t r e a m s from a catalytic cracker.
Other sizes and accessories available to fit your needs. Write for Waco Bath Bulletin for complete information. LABORATORY SUPPLIES A N D EQUIPMENT
WILKENS-ANDERSON CO. 4525 W
D I V I S I O N 5T
C H I C A G O 5 1 , ILL.
Circle No. 99 on Readers' Service Card VOL.
38, NO. 7, JUNE 1966 •
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