Retorting procedure

Oil Shale Pyrolysis-Gas Chromatography. Another important aspect of gas chromatography as applied to oil shale characterization is the ability to carry out separations directly on volatiles evolved as samples are heated under controlled conditions. The method for heating small samples of oil shale in the laboratory clearly diflFers considerably from actual larger scale retorting procedures. In the latter case, secondary reactions of organic pyrolysis product certainly occur and they are subject to contact with water and air prior to work-up and analysis. However, a... 

CH4, and H2S contents with less C3-C6 and CO2 contents. The lower C3-C6 levels in the case of the eastern oil shales are due to a more efficient condensation of those gases to the liquid product in our assay procedures (12-13). Gas cleanup would ultimately be expected to yield a higher Btu gas for the eastern oil shale-derived gas than a corresponding western gas due to elimination of H2S in the former and high CO2 levels and condensation of much of the C4-C6 range in the latter. Finally, it should be emphasized that the compositional information presented is based on Fischer assay retorting procedures and may not be entirely representative of products produced under commercial scenarios. 

Sample. Petroleum crude oil sample from Long Beach Field (TUMS Well C-331, API° 20), California, and shale oil obtained by retorting at 500°C the Green River Oil Shale (Anvil Point Mine) were studied. About 20 g of shale oil was dissolved in 200 ml of THF and then filtered. The sample was recovered by a rotary evaporator. Although the same procedure was done on the other samples, the percent ash was different for each sample. All the samples were evaporated to a constant weight in a vacuum oven at 50°C. 

People eating fish cannot detect the marine phyeotoxins associated with seafood diseases, and preparation procedures do not remove the toxins (Baden et al., 1995 Baden and Mende, 1982 Baden and Trainer, 1993 Sakamoto et al., 1987). Severe heating processes, such as retorting, may reduce the levels of some toxins (U.S. Food and Drug Administration, 2001) but this is not a practical method for protecting public health. 

In the UK, the use of animals is regulated by the Animals (Scientific Procedures) Act, 1986. For a general account of controls over the use of animals in science see Monamy (2000). For restrictions on the use of humans in medical research see World Medical Association (2000). So, for example, the European Commission rebuked a group of its scientific advisers for publicly disagreeing with its decision to ban the use of phthalate softeners in certain baby toys. The scientists on a committee that advised on phthalates did not consider that the evidence of harm was sufficient to warrant a ban, but the Commission retorted that this decision was not one for the scientists, as the conclusion that there is a serious and immediate risk is a responsibility of the commission. This concept is not scientifically defined (from ENDS Environment Daily, Friday 26 November 1999). 

This consideration as well as those concerning cost, convenience of use, and availability leads to the conclusion that petroleum fuels will be used for transportation purposes in preference to other fuels as long as crude petroleum is available. Although liquid fuels can be produced from gas, coal, or shale oil, the high energy losses involved in the conversion make such operations unattractive from an energy conservation point of view. Obviously, the direct utilization of gas and coal as produced and of the type of crude oil which can be produced from oil shale by simple retorting is the most desirable procedure and should be followed until petroleum is so scarce or expensive to find that the free play of economic forces dictates the synthesis of liquid fuels. 

In another test method (ASTM D-5515), a dilatometer is used to measure the swelling of bituminous coal. The test method is limited in applicability to coal that has a free swelling index < 1 (ASTM D-720). The principle of this test method is that the final volume of char obtained at the conclusion of a standard dilatation test is dependent on the mass of coal in the coal pencil and on the radius of the retort tube. This test method incorporates a procedure that determines the mass of air-dried coal in the coal pencil, provides a means to measure the average retort tube radii and employs a means to report coal expansion on an air-dried coal weight basis. The value of the dilatation properties of coals may be used to predict or explain the behavior of a coal or blends during carbonization or in other processes, such as gasification and combustion. 

Metallurgy. As is true for any metal, the procedure employed in the metallurgy of silver must be adapted to the particular form in which the metal exists in its ores. Native silver may be separated by the process of amalgamation. The crude ore containing metallic silver is treated with mercury to form an amalgam, which is then separated from the undesired earthy components of the ore. The amalgam is heated in a retort, and the silver remains behind as a residue, while the mercury is distilled from the retort, condensed, and used again. This... 

The concentration of Cl in the samples was measured by standard chemical procedure (Schoniger s method ) based on decomposition of analyzing compound by burning it in the glass retort [8], The mixture of caustic potash and hydrogen peroxide was used as an absorbent. The content of Cl in absorbent was detected by mercurous titration. 

Procedure Melt the tin. Commence the generation of chlorine, and regulate it so that the tin in the retort can be seen to bum... 

Determine the condensate load. The first step in selecting a steam trap for any type of equipment is determination of the condensate load. Use the following general procedure. a. Solid materials in autoclaves, retorts, and sterilizers. How much condensate is formed when 2000 lb of solid material with a specific heat of 1.0 is processed in 15 min at 240°F by 25-psig steam from an initial temperature of 60°F in an insulated steel retort ... 

Shale oil and a fuel gas have been produced by microwaveheating oil shale in a standard microwave oven in conjunction with experimentation to develop an in situ microwave retorting process. Various grades of oil shale have been subjected to high microwave fields. The derived oil has been submitted to various physical and chemical testing methods, and the chemical composition of the evolved gas has been evaluated. The specific gravity pour point yields of oil, water, gas, and losses and spent shale are compared with parallel data obtained with the Fischer assay procedure. Important differences in oil flow properties and gas composition are discussed in view of microwave interactive theory. 

Oil shale represents an enormous reserve of fossil fuel for domestic and foreign needs (1,2). Shale oil production can be divided into direct and indirect heating processes (2). In direct heating, some of the products or some other fuel is combusted to raise the oil shale to the necessary temperature for conversion to gas and oil while an indirect process transfers heat from an outside source. Although high yields have been demonstrated in some indirect procedures (3), the application to in situ retorting has been limited. Direct processes developed for in situ recovery of shale oil have not demonstrated sufficient control of the underground combustion for reliable operation. 

Crude oil analysis techniques, developed by the Bureau of Mines (9), was used initially to describe the overall quality of the product. Spent shale samples were ashed using a two-day, low temperature procedure. The covered samples were placed in a room temperature furnace, and the temperature was increased to 700°C (370°C) in a near-reductive atmosphere. The sample was uncovered and the temperature was increased to 750°F (300°C) for one more day with air forced over the sample. This method has been suggested to cause the least changes to heat-sensitive mineral components of the shale (17). Actual experience has shown that the time for this procedure can be halved because of the porous nature of the spent shale and the small sample size. Results are presented as weight percent of the pre-retorted sample. 

The oil yield results of the Fischer assay obtained by the modified TOSCO procedure have been discussed previously (16) and are summarized in Table I. The relative standard deviation in this set of assays was 2.5% on nine oil-yield assays. TOSCO has obtained precision limits of 0.6%. Further examination of the weight fractions in 46 retort runs showed that the major source of this scatter was in the weight of liquid product obtained. This probably can be attributed to the inadequate control of the retort temperature program. The above summary indicates... 

Tlie mdlting nd boiling points of the aJipbatio /3-Iactonee ere listed in Table 2, and those of the aromatio /3 laotones in Table 3. We have mentioned thoee -laetones whioh have been definitely isolated even if thedr purification has not been aooon lIsbed On the other hand, we have not included the -lactone which have been retorted in patents but for which preoise preparative procedures are not given. 

Procedure. The above reactants are mixed thoroughly and heated in a retort or in an apparatus as described by Steinkopf Die Chemie des Thiophens, page 9). The distillate from this reaction is washed with caustic to remove 5-methyl-2-hydroxythiophene, and the organic layer is steam distilled. The crude 2-methylthiophene is dried over sodium sulfate or calcium sulfate, and then dLstilled from sodium, b.p. 113°. 

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