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This standard (D2764-20) defines an empirical test method for measuring the dimethylformamide-insoluble (DMF-I) content in tar and pitch. The test is crucial for evaluating and characterizing these materials, providing a rapid and reasonably accurate way to establish the uniformity of shipments or sources of supply. It serves as a strong correlative measure to the toluene-insoluble (TI) content determined via Test Method D4072. Strict adherence to every detail of the procedure is necessary, as the method is empirical and outcomes are procedure-dependent.
The following specific equipment and reagents are mandated by D2764-20 to ensure consistent test results:
| 🟦 Apparatus | 📏 Specification Per Standard |
|---|---|
| Filtering Crucible | Porcelain, high form, fine-porosity bottom; 30–40 mL capacity; max pore diameter 7 µm |
| Water Bath | Maintained at 203 °F to 212 °F (95 °C to 100 °C) |
| Test Sieves | U.S. Standard 600 µm (No. 30) and 250 µm (No. 60), conforming to Specification E11 |
| Filter Apparatus | Filter flask and tube with a crucible adapter |
| 🧪 Reagent / Material | 🎯 Specification & Handling |
|---|---|
| Dimethylformamide (DMF) | Reagent grade. Boiling range 4 °F (2 °C) including 307 °F (153 °C). Stored over desiccant, filtered to optical clarity before use. |
| Celite Analytical Filter Aid (CAFA) | Dried to constant mass at 221 °F (105 °C). Stored in a tightly stoppered container. No other filtering medium is permitted. |
| Acetone | Meeting Specification D329. (Warning—Flammable. Health hazard.) |
A sample of tar or pitch is digested in hot dimethylformamide (DMF). The insoluble matter is then filtered using a prepared porcelain crucible containing a bed of Celite Analytical Filter Aid. The residue is washed, dried to a constant mass, and weighed. The procedure precisely controls particle size through the required 600 µm and 250 µm sieves, digestion temperature via a water bath held at 203–212 °F (95–100 °C), and filtration through a crucible with a maximum pore diameter of 7 µm.