D97 17b Spanish CC Test

Pour the specimen into the test jar to the level mark. When necessary, heat the specimen in a bath until it is just sufficiently fluid to pour into the test jar. It is known that some materials, when heated to a temperature higher than 45 degrees Celsius during the preceding 24 hours, do not yield the same pour point results as when they are kept at room temperature for 24 hours prior to testing. Examples of materials which are known to show sensitivity to thermal history are residual fuels, black oils, and cylinder stocks. Samples of residual fuels, black oils, and cylinder stocks which have been heated to a temperature higher than 45 degrees Celsius during the preceding 24 hours, or when the thermal history of these sample types is not known, shall be kept at room temperature for 24 hours before testing. Samples which are known by the operator not to be sensitive to thermal history need not be kept at room temperature for 24 hours before testing. Experimental evidence supporting elimination of the 24-hour waiting period for some sample types is contained in a research report, footnote 6 of the written standard. In the case of pour points above 36 degrees Celsius, use a higher range temperature measuring device, such as IP63C, or ASTM 61C, or a digital contact thermometer. Close the test jar with a cork carrying the test temperature measuring device. Adjust the position of the cork and temperature measuring device so the cork fits tightly, the temperature measuring device and the jar are coaxial, and the temperature measuring device is immersed to the correct depth. For liquid in glass, the thermometer bulb should be immersed so the beginning of the capillary is 3 millimeters below the surface of the specimen. For digital contact thermometers, the probe should be immersed so the end of the probe is 10 millimeters to 15 millimeters below the surface of the specimen. For the measurement of pour point, subject the specimen in the test jar to the following preliminary treatment. Heat the specimen without stirring to 9 degrees Celsius above the expected pour point but to at least 45 degrees Celsius in a bath maintained at 12 degrees Celsius above the expected pour point but at least 48 degrees Celsius. Transfer the test jar to a bath maintained at 24 degrees Celsius plus or minus 1.5 degrees Celsius and commence observations for pour point. When using a liquid bath, ensure that the liquid level is between the fill mark on the test jar and the top of the test jar. Heat the specimen without stirring to at least 45 degrees Celsius in a bath maintained at 48 degrees Celsius plus or minus 1.5 degrees Celsius. Transfer the test jar to a bath maintained at 24 degrees Celsius plus or minus 1.5 degrees Celsius. When using a liquid bath, ensure that the liquid level is between the fill mark on the test jar and the top of the test jar. When the specimen temperature reaches 27 degrees Celsius, and if using liquid and glass thermometers, remove the high cloud and pour thermometer and place the low cloud and pour thermometer in position. Transfer the test jar to the cooling bath. See 8.6.1 of the written standard. See that the disk, gasket, and the inside of the jacket are clean and dry. Place the disk in the bottom of the jacket. Place the gasket around the test jar 25 millimeters from the bottom. Insert the test jar in the jacket. Never place a jar directly into the cooling media. After the specimen has cooled to allow the formation of paraffin wax crystals, take great care not to disturb the massive specimen nor permit the thermometer to shift in the specimen. Any disturbance of the spongy network of wax crystals will lead to low and erroneous results. Pour points are expressed in integers that are positive or negative multiples of 3 degrees Celsius. Begin to examine the appearance of the specimen when the temperature of the specimen is 9 degrees Celsius above the expected pour point estimated as a multiple of 3 degrees Celsius. At each test temperature that is a multiple of 3 degrees Celsius below the starting temperature, remove the test jar from the jacket. To remove condensed moisture that limits visibility, wipe the surface with a clean cloth moistened in alcohol, ethanol, or methanol. Tilt the jar just enough to ascertain whether there was a movement of the specimen in the test jar. If movement of specimen in the test jar is noted, then replace the test jar immediately in the jacket and repeat a test for a flow at the next temperature 3 degrees Celsius lower. Typically, the complete operation of removal, wiping, and replacement shall require not more than 3 seconds. If the specimen has not ceased to flow when its temperature has reached 27 degrees Celsius, transfer the test jar to a jacket in a cooling bath maintained at 0 degrees Celsius plus or minus 1.5 degrees Celsius. As the specimen continues to get colder, transfer the test jar to a jacket in the next lower temperature cooling bath in accordance with table 2 of the written standard. If the specimen in the jar does not show movement when tilted, hold the jar in a horizontal position for 5 seconds, as noted by an accurate timing device, and observe the specimen carefully. If the specimen shows any signs of movement before 5 seconds has passed, replace the test jar immediately in the jacket and repeated a test for a flow at the next temperature 3 degrees Celsius lower. Continue in this manner until a point is reached at which the specimen shows no movement when the test jar is held in a horizontal position for 5 seconds. Record the observed reading of the test thermometer. For black specimen, cylinder stock, and residual fuel specimen, the result obtained by the procedure described in 8.1 through 8.7 of the written standard is the upper, maximum pour point. If required, determine the lower, minimum pour point by heating the sample while stirring to 105 degrees Celsius, pouring it into the jar, and determining the pour point as described in 8.4 through 8.7 of the written standard. Some specifications allow for a pass fail test or have pour point limits at temperatures not divisible by 3 degrees Celsius. In these cases, it is acceptable practice to conduct the pour point measurement according to the following schedule. Begin to examine the appearance of the specimen when the temperature of the specimen is 9 degrees Celsius above the specification pour point. Continue observations at 3 degrees Celsius intervals as described in 8.6 and 8.7 of the written standard until the specification temperature is reached. Report the sample as passing or failing the specification limit.