ASTM D2318 Test Method for Quinoline-Insoluble (QI) Content of Tar and Pitch
5. Apparatus
5.1 Filtering Crucibles, porcelain, with fine-porosity bottom, 25 mL to 40 mL capacity, high-form, maximum pore diameter, 7 µm.
5.2 Filter Apparatus - Filter flask and tube with crucible adapter.
5.3 Sieves - U. S. Standard 600 µm (No. 30) and 250 µm (No. 60), conforming to Specification E11.
5.4 Electric Hot Plate or Water Bath, maintained at 75 °C +/- 5 °C.
6. Reagents and Materials
6.1 Quinoline, Refined, meeting the following requirements:
6.1.1 The quinoline shall distill from 5 % to 95 % within a range of 2 °C that shall include the temperature of 237.4 °C after corrections for barometric pressure and emergent stem have been applied. The distillation shall be carried out in accordance with Test Method D850 using a total immersion thermometer with a range from 195 °C to 305 °C, graduated in 0.5 °C, and conforming to the requirements for Thermometer 69C as described in Specification E1. Temperature measuring devices such as precision thermocouples, resistance temperature detectors (RTDs), and liquid-in-glass thermometers with equal or better accuracies in the appropriate temperature range may be used.
6.1.2 The quinoline shall have a specific gravity at 15.5/15.5 °C of 1.092 to 1.098, as determined by Test Method D71, or other method of equivalent accuracy.
6.1.3 The quinoline shall be clear and light in color and shall contain less than 0.5 % volume of water as determined by Test Method D95. If not, redistill the quinoline in all-glass apparatus, discarding the first 5 % and collecting the next 90 %. If the quinoline contains suspended matter but is clear, light in color, and contains less than 0.5 % water, filter the quinoline through a crucible containing 5 g of Celite Filter Aid.
6.1.4 Store the quinoline in a tightly closed, dark bottle.
6.2 Toluene, Industrial Pure, meeting Specification D362.
6.3 Acetone, meeting Specification D329.
6.4 Concentrated Hydrochloric Acid.
6.5 Celite Analytical Filter Aid (CAFA) - Dry to constant weight at 105 °C, and store in tightly stoppered container.
6.5.1 Do not use any other grade of filter aid because filtration characteristics may differ. CAFA is manufactured only by Manville Co. and distributed through scientific supply houses.
7. Hazards
7.1 Fumes of the solvents should be removed by means of proper hoods from all working areas. The working area should be kept free of sparks and flames. Quinoline fumes should not be inhaled, and prolonged contact with the skin should be avoided. Toluene is toxic and flammable.
7.2 Observe proper laboratory procedures for handling hydrochloric and diluting acid.
