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D524_9 (15)

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Place a new glass coking bulb, Note 12 of the written standard, in the coking furnace at 550 degrees Celsius for about 20 minutes to decompose any foreign organic matter and to remove water. Place in a closed desiccator over a suitable desiccant, such as a desiccant containing calcium chloride or calcium sulfate, for 20 minutes to 30 minutes, and then weigh to the nearest 0.1 milligrams. Do not reuse a glass coking bulb, as unpredictable results are sometimes obtained in such cases. For routine testing, new bulbs can be used without pre-ignition, provided they are visibly free from particles or other contamination. Such bulbs, at least, should be heated in an oven to 150 degrees Celsius, placed in a desiccator, and then weighed. On making a test, it is important to adhere rigorously to the temperature conditions chosen for Section 7 of the written standard. For example, if the bath was at a temperature of 553 degrees Celsius plus or minus 1 degree Celsius when inserting the control bulb, then it is necessary to use similar temperature conditions in the coking test. When maintained in normal operation, the temperature of an electrically heated furnace with automatic controls will generally fluctuate within a specific temperature range. Therefore, when making a coking test, it is generally important that the test bulbs be inserted when the furnace is at the same temperature or at the same position in the temperature cycle as it was when the inspection test was started, unless it has been proven that the temperature variations are inappreciable. Shake thoroughly the sample to be tested, first heating to 50 degrees Celsius plus or minus 10 degrees Celsius for 0.5 hours, when necessary, to reduce its viscosity. Immediately following the heating and shaking, strain the sample through a 100-mesh wire screen by means of a hypodermic syringe, or the device shown in Figure 3 of the 1 Standard. Introduce into the coking bulb an amount of sample, as indicated in Table of the written standard. Make sure that no oil remains on the exterior surface or on the inside of the neck of the bulb. Reweigh the bulb and contents to the nearest milligram. If the sample foams or spatters, repeat the test, using the next smaller sample size listed in Table 1 of the written standard. In reporting the results, include the size when such small samples are used. If difficulty is encountered in loading very viscous or asphaltic samples of any size into the glass coking bulb, the apparatus shown in Figure X1.2 of the written standard can be used. Place the coking bulb in a standard performance well with the furnace at the checking temperature, Note 12 of the written standard, and allow to remain for 20 minutes plus or minus 2 minutes. Remove the bulb with metal tongs, the tips of which have just been heated. Duplicate the furnace and bulb conditions used when standardizing that bulb well-- Section 7 and Note 9 of the written standard. If there is appreciable loss of oil from frothing, discard the test and repeat the determination, using a smaller sample-- Note 13 of the written standard. Frothing can be due to water, which can be removed by heating gently in a vacuum and sweeping out the vapor with nitrogen prior to filling the bulb. After removal, cool the bulb in a desiccator under the same conditions, including time for weighing, used before filling the bulb, 9.2 of the written standard. When removing the bulb from the desiccator, examine it to make sure there are no foreign particles adhering to the bulb. If any are found, as black particles sometimes are on the capillary neck, brush them off with a piece of sized paper or camel's hair brush. Weight to the nearest 0.1 milligrams. Discard the used glass coking bulb. In studies of oil characteristics, useful information can often be gleaned from a simple visual examination of the coking bulb after the test. Thus, significance can be attached to noting, with the results, such findings as coke more or less fills the bulb. Liquid material is present, either as limpid residue or drops. The residue is not black and flaky, but is colored and pulverulent, presumably from presence of inorganic materials.

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Duration: 5 minutes and 16 seconds
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Posted by: abuckmaster on Aug 22, 2018

D524_9 (15)

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