ASTM-D4530:15(R2020) pdf free download – Standard Test Method for Determination of Carbon Residue (Micro Method).
8.3 Final Weighing—Transfer sample vials (maintained in place in the vial holder) to desiccator and allow vials to cool to room temperature. Weigh the cooled vials to the nearest 0.1 mg and record. Handle the vials with forceps. Discard the used glass sample vials.
8.4 Occasionally examine the condensate trap at the bottom of the oven chamber; empty if necessary and replace. (Warning—The condensate trap residue may have some carcinogenic materials present. Avoid contact with the trap residue; dispose of it in accordance with local laboratory practice.)
9. Procedure for Carbon Residue on 10 % (V/V) Distillation Residue
9.1 This procedure is applicable to light distillate materials, such as ASTM No. I and No. 2 fuel oil or materials expected to have less than 0.1 % (rn/rn) carbon residue.
9.2 A distillation analysis using either a 100 mL or 200 rnL starting volume is required in order to collect a sufficient amount of the 10 % (V/V) residue needed in this analysis. For a 100 mL distillation, assemble the distillation apparatus described in Specification E133, using flask B (125 mL bulb volume), flask support board with 50 mm diameter opening, and graduated cylinder B (100 mL capacity). For a 200 mL distillation, assemble the distillation apparatus described in Specification E133, using flask D (250 mL bulb volume), flask support hoard with 50 mm diameter opening, and graduated cylinder C (2(X) mL capacity). A thermometer is not required. hut the use of the ASTM High Distillation Thermometer 8F or C, as prescribed in Specification El, or the IP High Distillation Thermometer 6C, as prescribed in the Specification for IP Thermometers, is recommended.
9.3 Depending upon which distillation flask is used, place either 1(X) mL or 2(X) mL of sample (as measured at ambient temperature) into a distillation flask that is held at a temperature between 13 °C and ambient. Maintain the condenser bath temperature between 0 °C and 60 °C so as to provide a suflicient temperature differential for sample condensation, while avoiding any solidification of waxy material in the condenser tube. Use, without cleaning, the cylinder from which the sample was measured as the receiver, and place it so that the tip of the condenser does not touch the wall of the cylinder. The receiver temperature is required to be maintained at the same temperature (within ±3 °C) as the sample taken at the start of the test in order to obtain an accurate volume measurement in the receiving flask.
9.4 Apply the heat to the flask at a uniform rate so regulated that the first drop of condensate exits from the condenser between 10 mm and 15 mm (for 200 mL samples) or between 5 mm and 15 mm (for 100 mL samples) after initial application of heat. If performing a manual distillation, after the first drop falls, move the receiving cylinder so that the tip of the condenser tube touches the wall of the cylinder. Then regulate the heat so that the distillation proceeds at a uniform rate of 8 mLAnin to 10 mLArün (for 200 mL samples) or 4 mL/min to 5 mL/min (for 100 mL samples).