ISO 3016 Petroleum products - Determination of pour point
4 Reagents and materials
4.1 Sodium chloride (NaCl), crystals.
4.2 Calcium chloride (CaCl2), crystals.
4.3 Carbon dioxide (CO2), solid.
4.4 Coolant liquid: acetone, methanol or petroleum naphtha.
4.5 Wiping fluid: acetone, methanol or ethanol.
5 Apparatus (see figure 1)
5.1 Test jar, cylindrical, of clear glass, flat-bottomed, 33.2 mm to 34.8 mm outside diameter and 115 mm to 125 mm in height. The test jar shall have an inside diameter of 30.0 mm to 32.4 mm, with the constraint that the wall thickness be no greater than 1.6 mm. The jar shall be marked with a line to indicate a contents level 54 mm +/- 3 mm above the inside bottom.
5.2 Thermometers, partial immersion type conforming to the specifications given in annex A.
5.3 Cork, to fit the test jar, bored centrally to take the test thermometer.
5.4 Jacket, watertight, cylindrical, metal, flat-bottomed, 115 mm +/- 3 mm in depth with inside diameter 44.2 mm to 45.8 mm, and a wall thickness of approximately 1 mm. lt shall be supported in a vertical position in the cooling bath (5.7) so that no more than 25 mm projects out of the cooling medium, and shall be capable of being cleaned.
5.5 Disc, of cork or felt approximately 6 mm in thickness, to fit inside the jacket.
5.6 Gasket, ring form, approximately 5 mm in thickness, to fit snugly on the outside of the test jar and loosely inside the jacket. This gasket shall be made of rubber, leather or other suitable material, elastic enough to cling to the test jar and hard enough to hold its shape.
NOTE 2 The purpose of the ring gasket is to prevent the test jar from touching the jacket.
5.7 Cooling bath, of a type suitable for obtaining the required temperatures. The size and shape of the bath are optional, but a support to hold the jacket firmly in a vertical Position is essential. The bath temperature shall be monitored by means of the appropriate thermometer (specified in annex A) immersed to the correct immersion depth. For the determination of pour Points below 9 °C, two or more baths are required. The required bath temperatures shall be obtained either by refrigeration or by suitable freezing mixtures, and shall be maintained at the desired temperatures +/- 1.5 °C.
NOTE 3 The freezing mixtures commonly used are as follows:
For pour-point temperatures down to:
a) 9 °C: ice and water (tan be used to prepare the 0 °C bath in 6.8);
b) -12 °C: crushed ice and sodium chloride (4.1) (can be used to prepare the -18 °C bath in 6.8);
c) -27 °C: crushed ice and Calcium chloride (4.2) (can be used to prepare the -33 °C bath in 6.8);
d) -57 °C: carbon dioxide (4.3) and coolant liquid (4.4) (tan be used to prepare the -51 °C and -69 °C baths in 6.8).
5.8 Timing device, capable of measuring up to 30 s with an accuracy of 0.2 s.
