ASTM D6560 Test Method for Determination of Asphaltenes (Heptane Insolubles)
ASTM D6560 Standard Test Method for Determination of Asphaltenes (Heptane Insolubles) in Crude Petroleum and Petroleum Products
6. Apparatus
6.1 General - Ground-glass joints from different sources may have one of two diameter to length ratios. For the purposes of this test method, either is suitable, and for some applications, the diameter itself can be one of two. However, it is critical that the male and female parts of each joint are from the same series to avoid recession or protuberance.
6.2 Condenser, with a coil or double surface, fitted with a 34/45 or 34/35 ground-glass joint at the bottom to fit the top of the extractor. Minimum length is 300 mm.
6.3 Reflux Extractor, conforming to the dimensions given in Fig. 1. Tolerances are ± 1 mm on the height and outer diameter (OD) of the extractor body and ± 0.5 mm on all other dimensions. The female ground-glass joint at the top shall match the male at the bottom of the condenser, and the male ground-glass joint at the bottom shall match the female of the conical flask.
6.4 Conical Flasks, of borosilicate glass of appropriate capacity (see 11.2 and Table 1), with ground-glass joints to fit the bottom of the extractor.
NOTE 2 - Sizes 24/39, 24/29, 29/43 or 29/32 are suitable.
6.5 Stopper, of borosilicate glass of a size to fit the conical flask.
6.6 Evaporating Vessel, of borosilicate glass. Either a hemispherical dish of approximately 90 mm diameter, or another suitable vessel used in conjunction with a rotovapor.
NOTE 3 - A rotovapor in conjunction with a nitrogen atmosphere reduces the hazard of toluene evaporation (see 11.7).
6.7 Filter Funnel, of borosilicate glass, approximately 100 mm diameter.
6.8 Filter Papers, Whatman Grade 42, 110 or 125-mm diameter.
6.9 Analytical Balance, capable of weighing with an accuracy of 0.1 mg.
6.10 Forceps, of stainless steel, spade ended.
6.11 Timing Device, electronic or manual, accurate to 1.0 s.
6.12 Oven, capable of maintaining a temperature from 100 to 110°C.
6.13 Graduated Cylinders, of 50 and 100 mL capacity.
6.14 Stirring Rods, of glass or polytetrafluoroethylene (PTFE), 150 by 3-mm diameter.
6.15 Cooling Vessel, consisting of either a dessicator without desiccant, or another suitable tightly-stoppered vessel.
6.16 Mixer, high-speed, nonaerating.
7. Reagents
7.1 Toluene (methylbenzene) [C6H5CH3], analytical reagent or nitration grade.
7.2 Heptane [C7H16], analytical reagent grade.
8. Sampling
8.1 Unless otherwise specified, take samples by the procedures described in Practice D4057 or D4177.
