ASTM D2007 for characteristic groups in processing oils & petroleum-derived oils
ASTM D2007 standard test method for characteristic groups in rubber extender and processing Oils and other petroleum-derived oils by the clay-gel absorption chromatographic method
6. Apparatus
6.1 Beakers, Anticreep, 150-mL capacity, as illustrated in Fig. 1. (Warning - Beakers should be examined for sharp edges and fire polished, if necessary.)
6.2 Clay-Gel Column, constructed as illustrated in Fig. 2.
6.3 Conical Flasks, (Erlenmeyer), 250-mL capacity.
6.4 Solvent Receiver, capable of collecting solvent, without splashing or loss of material during the analysis. A wide-mouth, graduated, 500-mL capacity Erlenmeyer flask is one such example that has been found suitable to use.
6.5 Filter Funnel, long stem, 125-mm diameter; for use with 185 mm ready folded, fine-texture, rapid filter paper.
6.6 Separatory Funnel, 500 mL.
6.7 Hot Plate, explosion proof, controlled to a surface temperature of 100 to 105°C.
6.8 Round Bottom Flask, 3-necked, borosilicate, 500-mL capacity (Fig. 3).
6.9 Condenser, borosilicate (Fig. 3).
6.10 Adapter Tube with Vigreux column (Fig. 3).
6.11 Flexible Joint, TFE-fluorocarbon and borosilicate, 24/40 TS ground glass joints on each end.
7. Reagents and Materials
7.1 Purity of Reagents, Reagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended that all reagents shall conform to the specifications of the committee on Analytical Reagents of the American Chemical Society, where such specifications are available. Other grades may be used, provided it is first ascertained that the reagent is of sufficiently high purity to permit its use without lessening the accuracy of the determination.
7.2 Acetone, reagent grade, minimum purity. (Warning - Acetone is extremely flammable.)
7.3 Calcium Chloride, anhydrous granules.
7.4 Clay Adsorbent, 500 to 250 µm (30 to 60 mesh) Attapulgus.10 Clay quality may be determined using the azobenzene equivalence test shown in Annex A1. The azobenzene activity test measures the adsorptive characteristics of the clay. Azobenzene equivalence value should be 30 to 35. Clay outside of these limits should be discarded.
7.5 Cyclohexane, conforming to Specification D5309. (Optional, see 8.1.9.) (Warning - Cyclohexane is extremely flammable. Harmful if inhaled.)
7.6 Pentane, reagent grade minimum purity: (Warning - n-Pentane is extremely flammable. Harmful if inhaled.)
7.7 Silica Gel, activated, conforming to the following inspections:
Sieve analysis > 30 sieve size, 5 % (mass) maximum;
Sieve analysis > 50 sieve size, 45 % (mass) min
Sieve analysis > 100 sieve size, 80 % (mass) min
Sieve analysis > 200 sieve size, 94 % (mass) min
7.7.1 Gel should be activated for 4 h in an air oven at 190°C in a shallow pan.
7.8 Toluene, reagent grade minimum purity. (Warning - Toluene is flammable. Vapor harmful.)
7.9 Toluene-Acetone Mixture (50 to 50 by volume), mix equal volumes of toluene and acetone.
7.10 In order to obtain results that are consistent with those obtained elsewhere, it is very important that only the reagents and materials described in this section be used.
