ASTM D4421 Standard Test Method for Volatile Matter in Petroleum Coke
7. Apparatus
7.1 Furnace, Fieldner, electric, ASTM, calibrated (Test Method E 220) and regulated to maintain a temperature of 950°C (1742°F) +/- 15°C as measured by a thermocouple mounted inside the furnace.
7.2 Nickel Chromium Crucible Support for the platinum crucible.
7.3 Platinum 90 % - Rhodium 10 % Crucible, volatile matter form, reinforced top and bottom, capacity 15 mL; height 33 mm; top diameter 29 mm; fitted with a capsule-type cover 10 mm high. The cover is to have a 0.5-mm diameter hole drilled through the center. The total weight, crucible and cover, approximately 20 g.
7.4 Reshapers for the platinum crucible and cover.
7.5 Rifflers, with hoppers and closures.
7.6 Jaw Crusher and Roll Crusher - Other style crushers which allow control over particle size without contamination are acceptable. (See Annex A1.)
7.7 Sieves, as required (Specification E 11).
7.8 Timers, stopwatch or second-timer accurate to +/- 1 s.
8. Precautions
8.1 Effusion of gaseous products, including soot and various hydrocarbons and the increase of heat associated with the test can make use of a hood desirable.
9. Preparation of Furnace
9.1 If desired, the radiant heat loss to the room from the outside metal cylinder can be reduced by insulating the furnace with a thick layer of insulation and glass wool.
9.2 Fit a thermocouple into the bottom of the furnace. Use borosilicate glass wool to close the opening around the thermocouple. Adjust the thermocoupled position so it rests 2 to 3 mm below the bottom of the platinum crucible with the platinum crucible positioned in the crucible support and the support resting on the top of the furnace.
9.3 Hang a 100 to 150-mm (4 to 6-in.) mirror above the furnace, positioned to allow the operator to observe the platinum crucible during the time it is positioned in the furnace.
