BS 2000-47:1983 download.British Standard Methods of test for Petroleum and its products Part 47. Solubility of bituminous binders (Identical with IP 47/82).
1. SCOPE
1.1. This method is applicable to bituminous binders containing not less than
95¾ of bitumen in which volatile constituents will not normally be present. If water is present the amount is usually small, and should be removed as directed in the method.
For the determination of the bitumen content of mixtures use IP 162.
2. SUMMARY OF METHOD
2.1. The sample is dissolved in Trichloroethylene and filtered through a layer of powdered glass in a sincered crucible. The insoluble material is washed, dried and weighed.
NOTE I: The method can be used with oher solvents, but bituminous binders have varying solubilities in different solvents.
3. DEFINITION
3.1. Solubiity of bituminous binder is the percentage of material which is soluble in Trichioroethylene.
NOTE 2: The international definition of bitumen is based on the use of Carbon Disulphide as solvent.
4. APPARATUS AND MATERIALS
4.1. Filtration apparatus including:
4.1.1. Filter flask — heavy wall, with side arm, 500 ml capacity.
4.1.2. Sintered glass crucible — No. 4 porosity, effective diameter approximately 30 mm.
4.1.3. Rubber adaptor — for holding crucible in the neck of the filter flask.
4.1.4. Powdered gloss — Pyrex, particle diameter less than 74 pm.
5. SOLVENTS
5.1. Trichloroethylene, type I or 2, conforming to BS 580.
6. SAFETY PRECAUTIONS
CAUTION: Trichioroethylene is toxic and adequate ventilation should be provided. Trichioroethylene iS non-flammabk. but in the presence of a flame or red hot heating wire, the vapour is changed to highly toxic phosgene gas. For these reasons, smoking and the presence of flames etc. should be prohibited.
7. SAMPLE
7.1. If the sample contains water, heat a representative portion of between 100 to 200 grams at a temperature not exceeding 130°C with constant stirring until the binder ceases to foam.
8. PREPARATION OF APPARATUS
8.1. Weigh 3 ± 0.1 g of dried powdered glass into the sintered glass crucible.
8.2. Assemble the filtering apparatus, gently tapping the crucible in order to ensure that the glass powder is evenly distributed.
8.3. Apply gentle suction and wash the glass powder with successive portions of trichioroethylene.
8.4. Dry the crucible in an oven at 100°C under slight vacuum for I hour, Dry w constant weight.
9. PROCEDURE
9.1. Weigh 2 o 5g of the dry sample to the nearest 0.01 g into a 200 ml conical flask, and add 100 ml of solvent. CAUTION: see Section 6. Stir the contents of the flask, and allow to stand loosely corked for one hour.
9.2. Assemble the filter apparatus, moisten the powdered glass with solvent and filter the contents of the flask through the prepared sintered crucible.
Filter at the rate of not more than two drops per second initially. The filtrate shall be clear, indicating complete retention of insoluble matter by the filter.
9.3. Transfer the insoluble matter remaining in the flask to the crucible by washing out the flask with a stream of solvent from a wash bottle.
9.4. Wash the material retained in the crucible with successive small amounts of solvent until the filtrate obtained is not discoloured.
9.5. Dry the crucible in an oven at 105°C to 115°C for one hour, cool in a desiccator and weigh.
10. CALCULATION AND REPORTING
10.1. Calculate the solubility of the sample from the formula:
Solubility, ¾ mass= l00(W1—W2)/W1
Where W1 is the mass of the dry sample in g, Wis the mass of insoluble material in g retained in the Gooch crucible.
10.2. Report the result to the nearest 0.05°!. mass as the Solubility IP 47.
NOTE 3: It other solvents are used, this shall be reported.
11. PRECISION
11.1. The following criteria should be used for judging the acceptability of results (9501. confidence) on samples with solubilities greater than 99.5%.
11.1.1. Repeatability — Duplicate results by the same operator should be considered suspect if they differ by more than the following amount:
0.10’io
11.1.2. Reproducibility – The results submitted by each of two laboratories, should not be considered suspect unless the two results differ by more than the following amount:
0.15%
NOTE 4: These precision values were obtained by statistical examination of inter-laboratory test results, and were first published in 1965.