A1.1 Oxidation Vessel, with body, cap, closure ring, and stem, constructed as shown in Figs. A1.1-A1.4.
A1.1.1 Vessel Body and Cap, shall be constructed of 18-8 or 321S12/321S20 Part 1 (BSI) stainless steel to ensure a proper rate of heat transfer. The interior surface shall be given a smooth finish to facilitate cleaning. Alternatively, the vessel body and cap may be machined from 76.2-mm (3-in.) solid copper rod and then heavily chrome plated.
A1.1.2 Vessel Stem, shall be constructed of stainless steel, the stem having an inside diameter of 6.4 mm (1/4 in.) and shall be equipped with a 6.4-mm (1/4 in.) needle valve.
A1.1.3 Closure Ring, shall be made of chrome-plated steel or chrome-plated aluminum bronze BS 2032.
A1.1.4 The vessel shall withstand a working pressure of 3450 kPa (500 psi, 34.5 bar) at 150°C.
A1.1.5 O-ring Gaskets, Viton or silicon, 50.8 mm (2 in.) in inside diameter by 60.3 mm (2 3/8 in.) in outside diameter (BS/USA size No. 329). Caps with larger seal recess diameters will require 54 mm (2 1/8 in.) inside diameter by 60.3 mm (2 3/8 in.) in outside diameter (BS/USA size No. 227).
A1.2 Glass Sample Container, with copper catalyst coil, 175-mL capacity as shown in Fig. A1.5, constructed of borosilicate glass. Glass sample container shall have a sliding fit in the vessel with no excess side clearance. The container alone shall have a maximum wall thickness of 2.5 mm and shall weigh no more than 100 g.
A1.2.1 Top of Sample Container, shall be covered with 57.2-mm (2 1/4 in.) diameter PTFE disk. The disk will have four 3.2-mm (1/8 in.) diameter holes evenly spaced in a 9.5-mm (3/8 in.) radius from the center of the disk. The disk shall have a thickness of 1.6 mm (1/16 in.). A stainless steel hold-down spring as shown in Fig. A1.6 shall be used to ensure rotation of the sample container. The assembly is shown in Fig. A1.7.
A1.3 Recording Devices
A1.3.1 Recording Gauge, as shown in Fig. A1.8 or indicating, with a range from 0 to 1400 kPa (or 0 to 200 psi or 0 to 14 bar) and graduated in 25-kPa (or 5 psi or 0.25 bar) divisions. The accuracy shall be 2.5 % or less of the total scale interval. Recording gauges should be mounted so that the face is perpendicular to the axis of rotation.
A1.3.2 Pressure Measurement System, consisting of electronic pressure transducers, power source, mounting equipment and connecting cables. The rotary transducer couplings can be mounted directly on the vessel stem in place of the standard mechanical pressure recorders. The pressure transducer shall have a span of 0 to 1400 kPa (or 0 to 200 psi or 0 to 14 bar). The accuracy should be valid over a wide compensated temperature range. The output signal from the transducer can be channeled into a datalogger, microprocessor based recorder, or a computer for data acquisition. The data acquisition package should be capable of logging pressure data and time. The overall system accuracy of the data should be within 2.5 % of the total scale.
A1.4 Oxidation Bath, equipped with an efficient stirrer and a suitable device from holding and rotating the vessel axially at an angle of 30° at 100 more or less 5 rpm while submerged in oil to a point at least 25 mm (1 in.) below the level of the bath liquid.
A1.4.1 A bath at least 230 mm (9 in.) deep, filled with 30 L (8 gal) of heavy bath oil per vessel, has the proper heat capacity. Silicone oil shall be necessary to house the oil bath under a fume hood to contain any oil vapor generated.
A1.4.2 Provide thermal regulation to maintain the bath within 0.1°C of the test temperature. There should be sufficient, immediately available heat to bring the bath to operating temperature within 15 min after the vessels have been inserted.
A1.5 Thermometer, IP 37C sludge test thermometer having a range from 144 to 156°C graduated in 0.2°C intervals or other temperature measuring device, having an accuracy of 0.1°C.
A1.6 Gauge, for pressurizing vessel to 620 kPa (90 psi) graduated in 1.5 kPa (0.2 psi) increments.
