ASTM D5805-00(R2019) pdf free download

ASTM D5805-00(R2019) pdf free download.Standard Test Methods for Rubber—Determination of Carbon Black in Masterbatches
6. Reagents
6.1 Purity of Reagents—Reagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended that all reagents conform to the specifications of the Committee on Analytical Reagents of the American Chemical Society, where such specifications are available. 5 Other grades may be used, provided it is first ascertained that the reagent is of sufficiently high purity to permit its use without lessening the accuracy of the determination.
7. Preparation of Sample
7.1 Blend 200 g of dried sample obtained in accordance with 4.1 or 9.1 by passing it five times between the rolls of a laboratory mill. Maintain the roll temperature at 50 6 5°C (122 6 9°F) and a distance between the rolls of 0.5 6 0.13 mm (0.020 6 0.005 in.). After blending, sheet the sample from the mill with the distance between the rolls set at 0.25 6 0.05 mm (0.010 6 0.002 in.). Dry approximately 2 g of the blended, thinly sheeted material for 1 h in the oven at 100 6 5°C (212 6 9°F). Keep the dried sheet in a desiccator until ready to weigh the samples.
8. Procedure
8.1 Into the tared porcelain crucibles accurately weigh three 0.3 to 0.5-g samples from the sheet ofmaterial being tested and three 0.3 to 0.5-g samples from a similarly prepared sheet of standard SBR black determinate (see Note 2). Due to the hygroscopic nature of the samples and the carbon black, weigh the crucibles and contents in the tared weighing bottles.8.2 Place the six crucibles in a fused alumina combustion boat, or boats, alternating the samples of determinate and the test samples. Insert the combustion boat, or boats, into the combustion tube. Pass a stream of oxygen-free CO 2 through the tube at a flow rate of 150 to 240 cm 3 (atmospheric pressure)/min. After the tube has been swept free of oxygen (approximately 5 min is sufficient time), place it in the combustion furnace maintained at a temperature of 550 6 25°C, and distill off the rubber hydrocarbon. Continue to pass CO 2 through the tube, while allowing the tube to remain in the furnace for 30 min. At the end of this period, remove the combustion tube from the furnace and allow it to cool, meanwhile continuing the flow of CO 2 through it. When it is cool, remove the boat, or boats, and place the crucibles in a desiccator until they cool to room temperature and are ready to be weighed. Accurately weigh the crucibles and contents. 8.3 After weighing the crucibles containing the carbon black residues, ignite the samples by either of the following methods: 8.3.1 Place the crucibles and contents in a combustion boat, or boats, and insert them into a second combustion tube. Place the tube in a combustion furnace maintained at 550 6 25°C and pass a stream of oxygen or air through the tube. 8.3.2 Alternately, place the crucibles and contents in a muffle furnace maintained at 550 6 25°C. After the carbon has been completely burned, remove the boat, or boats, from the muffle furnace and place the crucibles in a desiccator. When the crucibles have cooled to room temperature, weigh them.
15. Procedure
15.1 Place into a tared crucible 0.3 to 0.5 g (to the nearest 0.1 mg) from the sheet of material being tested. Using the insertion rod, insert the boat containing the crucibles into the tube to maximum depth. Insert the ground-glass stopper coated properly with vacuum seal lubricant, turn on the vacuum pump, and evacuate the tube to less than 1.3 kPa. 15.2 Introduce the combustion tube into the combustion furnace maintained at 600 6 25°C, using care not to rotate the tube or otherwise cause sample disturbance. Allow the tube to remain in the furnace for 10 min, maintaining maximum pressure of 1.3 kPa (10 mm Hg) during combustion. Remove the tube from the furnace, allow the tube and contents to cool for 7 min, and slowly allow pressure to increase to prevent blowing residue out of crucible. 15.3 Remove the boat and place it in a desiccator to cool to room temperature. Weigh each crucible and residue to the nearest 0.1 mg. Determine the ash content on a portion of sample.