FEATURED LABORATORY
I
Oil Shale Corporation Research Center
Research Center of the Oil Shale Corp. (TOSCO) is attractively designed to suit its site on the eastern edge of the Rocky Mountains 94A
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ANALYTICAL CHEMISTRY
H E ROCKY FLATS RESEARCH
CENTER
of The Oil Shale Corporation (TOSCO) is located northwest of Denver, Colo., on the eastern edge of the Rocky Mountains. Executive offices are located in New York City and operational forces are stationed near Grand Valley, Colo., at the site of a 1000 ton-per-day SemiWorks Plant on the western slope of the Rocky Mountains. Recoverable reserves in the Tri-State area of Colorado, Utah, and Wyoming are measured in the hundreds of billions of barrels. One of the primary functions of the Research Center is control and evaluation in support of the TOSCO II Process for extracting oil from the kerogenrich shale, as encompassed in both the 25 tons-per-day Pilot Plant at Rocky Flats and the Semi-Works Plant. The staff of four scientists and five laboratory technicians is supported by 10 part-time technicians, mainly students a t the Colorado School of Mines located in nearby Golden. Research and development is also carried out in other areas of potential synthetic fuel sources, such as tar sands, coal, and foreign oil shale. In addition, work is being conducted on the evaluation and recovery of other minerals found in Colorado oil shale, principally compounds of aluminum and sodium. Working toward the first commercial production of shale oil in the United States, the laboratory staff has the continuing task of refining conventional shale oil analytical procedures to improve their accuracy and of developing new ]irocedures as required to maintain technological leadership. In this context, the Research Center has developed a most modern analytical laboratory, employing the latest in automatic electronic instrumentation.
For control of the TOSCO I I Process, samples of raw materials used and products produced are thoroughly analyzed. On a continuous basis, the following materials are subjected to analysis or examination: raw shale, spent shale, the oil, gas, and water produced, and the ceramic balls used to heat the shale. Raw shale (crushed) is analyzed and, after retorting, the spent shale is analyzed for particle size, carbon, hydrogen, nitrogen, and other elements. Recovered oil from the plant is measured for density, viscosity, water content, base sediments, and elements. An analytical distillation of the oil is carried out. Hydrogen sulfide contained in the gas from the retort process can be removed and converted to sulfur, a valuable by-product. The ceramic balls used to heat the shale are probably the most important single element of the TOSCO I I Process. Representative samples of the balls are removed from the plant at intervals and are then sliced, mounted, polished, and the microstructure is examined by microscopy. Although all instrumentation is available for applied research work, two thermal analysis instruments are especially important: a differential scanning calorimeter and a thermobalance. T h e differential scanning calorimeter is used to determine heat capacities and heat requirements, such as the heat of retorting. The thermobalance is applied to the kinetics of retorting ; it measures and records the continuous weight loss of a sample specimen as the temperature is programmed in a predetermined fashion. Thermal analysis work is being conducted on oil shale as well as other materials such as coal and tar sands.
Gas chromatograph analyzes gas produced f r o m the retort for m o l e % of major c o m p o u n d s . Studies by gas chromatography are made on raw oil stock as well as distilled fractions and simulated distillations are often made by GC
Constant search for by-products of the retorting process is underway at the center. Spent shale is analyzed for extractable minerals. Shown is an atomic absorption spectrophotometer which is highly useful for the determination of AI, Na, Si, and V
Kinetics of retorting is studied by use of a thermobalance. Versatility of this ins t r u m e n t permits study of fast, high t e m p e r a t u r e kinetics involving weight changes
Modified Fischer assay is used to calculate oil yield f r o m raw shale which has been crushed and blended into representative samples. Carbon, hydrogen, and nitrogen determinations are made with an automatic elemental analyzer. Mineral carbonate is measured by conventional wet chemistry VOL. 4 1 , NO. 3, MARCH 1969 ·
95 A
