ASTM D4930 Test Method for Dust Control Material on Calcined Petroleum Coke
6. Apparatus
6.1 Extractor, with condenser, Soxhlet, 200 mL capacity.
6.2 Flask, round bottom with short neck, 250 mL.
6.3 Heating Mantle, for 250 mL flask.
6.4 Boiling Chips.
6.5 Thimbles, Cellulose Extraction, 43 mm in diameter by 123 mm in height (single thickness; 9 µm to 11 µm for liquid retention).
6.6 Analytical Balance, capable of weighing to 0.1 mg.
6.7 Hot Plate, with temperature control +/- 3 °C between 90 °C and 110 °C.
6.8 Hooked Glass Tube, 3 mm inside diameter, 225 mm long, bent such that about 75 mm extends into the flask when connected into the neck of the flask.
6.9 Flexible Tubing.
6.10 Drying Oven, Forced Draft or Vacuum (vacuum preferred if toluene is used).
6.11 Desiccator.
6.12 Rifflers, encased with hoppers.
6.13 Hood.
7. Reagents
7.1 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. 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.
7.1.1 Methylene Chloride, reagent grade with residue after evaporation specification of 0.002 % or less (any other solvent used shall be reagent grade with no greater residue). (Warning - The use of methylene chloride is extremely volatile (BP = 40 °C) and mildly toxic.) (Warning - All handling of methylene chloride, including volumetric measurement and transfer of the solvent to the extraction apparatus, must be done in an approved fume exhaust hood. Extractions and subsequent methylene chloride drying procedures must also be performed in this same hood.)
7.1.2 Acetone, reagent grade. (Warning - Acetone is extremely flammable.) (Warning - Keep away from heat, sparks, and flame and keep container closed when not actually pouring acetone. Use only in a well-ventilated area. Avoid inhalation and contact with the eyes or skin.)
8. Sample Preparation
8.1 Riffle divide the bulk sample to obtain a 200 g analysis sample.
8.2 Reduce the analysis sample to pass a 6.3 mm sieve by one pass through a jaw crusher set to not crush smaller than 6.3 mm (a roll crusher can be used by stage crushing to 6.3 mm).
8.3 Dry the reduced analysis sample at 110 °C to 115 °C to constant mass (about 8 h may be required; overnight drying preferred when convenient). Store in a desiccator until ready to test.
NOTE 2 - The recommended practices for collecting samples and the equipment and procedures for crushing and dividing are described in Practice D346, D4057, and Practice D2013 and Test Methods D2234/D2234M. Specifications for sieves are described in Specification E11.
