ASTM D367 Standard Test Method for Xylene-Insoluble Matter in Creosote
7. Procedure
7.1 Take the original, undehydrated sample and, if necessary, heat and stir until any crystalline material is in solution and the sample is homogeneous. Determine the percentage of water in accordance with Test Method D370.
7.2 Weigh the following size sample, into a 100-mL beaker:
New creosote: 10 more or less 1 g
Used creosote: 5.0 more or less 0.5 g
Creosote solutions: 2.0 more or less 0.1 g
7.3 Calculate and record the weight of the sample.
7.4 Warm 50 mL of xylene to a temperature of 50 to 60°C, and immediately add it to the sample while stirring thoroughly. Continue stirring until the sample is dispersed and the bottom of the beaker is clean. Bring the beaker or flask containing the solution to boiling on a hot plate.
7.5 Insert the filter tube with the adapter in the filter flask and place the previously prepared and tared crucible in the adapter. Fill the crucible before the xylene has been drawn entirely through the diatomaceous silica. Take care that the diatomaceous silica is never free from liquid, either during the addition of the solution containing the sample, or during the subsequent washing with xylene.
7.6 Wash the beaker, thermometer, or stirring rod, and crucible with hot xylene. Pass all washes through the filter. Use a suitable policeman to sweep the insoluble particles into the crucible. Wash the crucible and contents with the hot xylene, allowing each wash to pass almost through the filter before the next is added, until the washings are colorless.
7.7 Reduce the suction and wash the contents with acetone until the washings are colorless. Four additions of 5 mL each are usually sufficient. Remove the crucible, and wipe the outside clean with a tissue moistened with xylene.
8. Calculation
8.1 Calculate the xylene-insoluble matter as a percentage of the water-free preservative, as follows:
Xylene-insoluble matter, % = [100(A - B)/C] x [100/(100 - D)]
where:
A = weight of crucible after filtration,
B = weight of prepared crucible before filtration,
C = weight of sample used, and
D = percentage of water in the sample.
