ASTM D4746 for Determination of Quinoline Insolubles (QI) in Tar and Pitch
5. Apparatus
5.1 Pressure Filtration Vessel - The pressure filtration vessel (see Fig. 1) is a stainless steel (304) jacketed block heated by steam or cooled with water, sealed by a lid, flat gasket, and clamp. The interior of the block is designed to accept a 3A2 Berlin porcelain filtration crucible (see 5.4). The crucible is sealed within the block by the use of three O-rings, a crucible sealing collar, and an adjustable plunger.
5.1.1 The seal is accomplished when the sealing lid is placed on top of the block and clamped. The adjustable plunger applies a force to the crucible sealing collar, which in turn pushes downward on the crucible and simultaneously compresses O-ring gaskets, forming a seal between surfaces of the crucible and the wall of the block. The filtration of material is accomplished by nitrogen (10 to 30 psig) introduced through the lid of the pressure filter. The filtrate exits from the drain tube at the bottom of the block. The filtrate is disposed into a Buchner flask, attached to drain tube by a No. 7 rubber stopper. A vacuum hose is attached to the Buchner flask and placed in a 100-mL beaker containing water to indicate the exit of nitrogen when the filtration is completed.
5.2 Beaker, 50 mL.
5.3 Buchner Flask, 500.
5.4 Filtering Crucible, porcelain, with a medium-porosity bottom, top outer diameter 1 3/4 in. (45 mm), bottom outer diameter 1.2 in. (30 mm), height 2 in. (50 mm).
5.5 Analytical Balance.
5.6 Desiccator.
5.7 Thermometer, 0 to 300°F (150°C).
5.8 Drying Oven, maintained at 221°F (105°C).
5.9 Mortar and Pestle.
5.10 Two Wash Bottles, 500 mL.
5.11 Steam Bath.
6. Reagents
6.1 Quinoline - Refined, meeting the following requirements:
6.1.1 The quinoline shall be distilled from 5 to 95 % within a range of 2°F (1°C) that shall include the temperature of 459.3°F (237.4°C) after corrections for barometric pressure and emergent steam have been applied. The distillation shall be carried out in accordance with Method D850 using a total-immersion thermometer with a range from 383 to 581°F (195 to 305°C), graduated in 1°F (0.5°C) and conforming to the requirements for thermometer 69C as described in Specification E1.
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 D70, 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 an 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 1 + 1 Hydrochloric Acid Solution - Add equal volume concentrated hydrochloric acid to distilled water. (Warning - Corrosive.)
6.3 Acetone, meeting Specification D329. (Warning - Flammable (Health Hazard).)
