ASTM D1025:10(R2021) pdf free download – Standard Test Method for Nonvolatile Residue of Polymerization-Grade Butadiene.
6. Preparation of Apparatus
6.1 Clean the evaporating dishes with a chromic-acid solution or other suitable cleaning agent before each test. (Warning—Causes severe burns. A recognized carcinogen. Strong oxidizer. Contact with organic material may cause fire.) Remove the dishes l’rom the cleaning solution with stainless- steel forceps and handle only with forceps thereafter. Wash the dishes thoroughly, first with tap water, then with distilled water, and dry in the oven at 105 °C for about I h. or until constant weight is obtained. Before weighing, cool the dishes for at least 30 mm in the cooling vessel.
7. Procedure
7.1 Weigh the evaporating dish to the nearest 0. 1 rng on the analytical balance.
7.2 Chill the evaporating dish to ice temperature. Cool the hutadiene and the graduated cylinder to about —20 °C. (VarningExtremely flammable gas under pressure. May form explosive peroxides upon exposure to air. Harmful if inhaled. Irritating to eyes, skin, and mucous membranes.) Determine the sample temperature to the nearest I °C and transfer 25 mL ± 1 mId of sample to the evaporating dish. Record the sample volume and temperature.
7.3 Allow the sample to evaporate at room temperature in a well-ventilated hood. When evaporation is complete, place the evaporating dish in an oven at 105 °C ± 5 °C until a weight constant to 0.1 rng is obtained. Before each weighing, cool the dish for at least 30 mm in the cooling vessel. Between each two weighings, place the dish in the oven for at least 30 mm.
8. Calculation
8.1 Calculate the amount of nonvolatile residue by means of the following equation:
where:
A = weight of the evaporating dish, g,
B = weight of the evaporating dish plus residue. g.
S = volume of the liquid butadiene sample, mL, and
d = density of the sample at the temperature of measurement. g/mL, found by using Table 1.
9. Precision and Bias
9. 1 Precision—The precision of this test method as determined by statistical examination of interlaboratory results is as follows:
9. 1. 1 Repeatability—The difference between two test results obtained by the same operator with the same apparatus under constant operating conditions on identical test material would, in the long run, in the normal and correct operation of the test method, exceed the following values in only one case in twenty: 0.02%
9.1.2 Reproducibility—The difference between two single and indepcndent results obtained by different operators working in different laboratories on identical test material would, in the long run, in the normal and correct operation of the test method, exceed the following values in only one case in twenty:
9.1.3 Bias—Since there is no accepted reference material suitable for determining the bias for the procedure in this test method for measuring non-volatile residue, no statement on bias is being made.