1、Standard Method of Test for Solubility of Bituminous Materials AASHTO Designation: T 44-141ASTM Designation: D2042-01 American Association of State Highway and Transportation Officials 444 North Capitol Street N.W., Suite 249 Washington, D.C. 20001 TS-2b T 44-1 AASHTO Standard Method of Test for Sol
2、ubility of Bituminous Materials AASHTO Designation: T 44-141ASTM Designation: D2042-01 1. SCOPE 1.1. This method covers the determination of the degree of solubility in trichloroethylene or 1,1,1 trichloroethane of asphalt materials having little or no mineral matter. The portion that is soluble in
3、trichloroethylene or 1,1,1 trichloroethane represents the active cementing constituents. 1.2. The values stated in SI units are to be regarded as the standard. 2. REFERENCED DOCUMENTS 2.1. AASHTO Standards: M 231, Weighing Devices Used in the Testing of Materials R 16, Regulatory Information for Che
4、micals Used in AASHTO Tests 2.2. ASTM Standard: E177, Standard Practice for Use of the Terms Precision and Bias in ASTM Test Methods 3. SUMMARY OF METHOD 3.1. The sample is dissolved in trichloroethylene or 1,1,1 trichloroethane and filtered through a filter mat. The insoluble material is washed, dr
5、ied, and weighed. 4. APPARATUS AND MATERIALS 4.1. The assembly of the filtering apparatus is illustrated in Figure 1. Details of the component parts are as follows: Figure 1Filtering Apparatus Assembly 2015 by the American Association of State Highway and Transportation Officials.All rights reserved
6、. Duplication is a violation of applicable law.TS-2b T 44-2 AASHTO 4.1.1. Gooch Crucibleglazed inside and outside with the exception of outside bottom surface. The approximate dimensions shall be a diameter of 44 mm at top, tapering to 36 mm at bottom, and a depth of 24 to 28 mm. 4.1.2. Glass Fiber
7、Pad32, 35, or 37 mm in diameter.24.1.3. Filter Flaskheavy-wall, with side tube, 250-mL capacity or larger. 4.1.4. Filter Tube40- to 42-mm inside diameter. 4.1.5. Rubber Tubing or Adapterfor holding the Gooch crucible on the filter tube. Note 1Other suitable assemblies permitting vacuum filtration wi
8、th a Gooch crucible may be used. 4.2. Erlenmeyer Flask125 mL, or other suitable container. 4.3. Ovencapable of maintaining a temperature of 110 5C (230 9F). 4.4. Desiccatorof suitable size, charged with an effective desiccant. 4.5. Analytical BalanceClass A conforming to the requirements of AASHTO S
9、pecification M 231. 5. SOLVENT 5.1. Technical grade, Type I, tricholorethylene or technical grade 1,1,1 tricholorethane. 6. SAFETY PRECAUTIONS 6.1. Trichloroethylene and 1,1,1 trichloroethane are toxic materials and strict adherence to instructions in Material Safety Data Sheets are to be followed.
10、Caution: Trichloroethylene and 1,1,1 trichloroethane in the presence of heat and moisture may form acids that are extremely corrosive. 7. PREPARATION OF GOOCH CRUCIBLE 7.1. Assemble the filtering apparatus as shown in Figure 1. Place filter pad into the Gooch crucible, moisten the pad with solvent,
11、and seat firmly in the bottom of the crucible with light suction. Dry the crucible and contents at 110 5C (230 9F) for at least 20 min. Cool the crucible and contents in a desiccator for at least 20 min and determine the mass. Repeat this procedure until constant mass (0.3 mg) is obtained. Store in
12、a desiccator until ready for use. 8. SAMPLE PREPARATION 8.1. If the sample is not fluid, heat the sample with care to prevent local overheating until it has become sufficiently fluid to pour, occasionally stirring the sample to aid heat transfer and to assure uniformity. Avoid the entrapment of air.
13、 2015 by the American Association of State Highway and Transportation Officials.All rights reserved. Duplication is a violation of applicable law.TS-2b T 44-3 AASHTO 9. PROCEDURE 9.1. Note safety precautions in Section 6. Transfer approximately 2 g of the sample into a tared 125-mL Erlenmeyer flask
14、or other suitable container. Allow the container and its contents to cool to ambient temperatures and determine the mass to the nearest 1 mg. Add 100 mL of the trichloroethylene or 1,1,1 trichloroethane to the container, stopper flask and agitate as necessary until the sample is dissolved and no und
15、issolved material adheres to the container. Normally the temperature at which this test is run is not critical, and it may be performed at the laboratory air temperature. For referee tests, however, the flask and sample in solution shall be placed in a water bath maintained at 37.8 0.25C (100 0.5F)
16、for 1 h before filtering. 9.2. Place the previously prepared and tared Gooch crucible in the filtering tube. Wet the filter pad with a small portion of clean solvent and decant the solution through the filter pad of the crucible with light suction. When the insoluble matter is appreciable, retain as
17、 much of it as possible in the container until the solution has drained through the filter pad. If the filter paper becomes clogged with insoluble material and the solution cannot drain through, the use of additional crucibles is permitted, provided they are conditioned as described in Section 7.1.
18、Wash the container with a small amount of solvent and, using a stream of solvent from a wash bottle, transfer all insoluble matter to the crucible. Use a “policeman” if necessary to remove any insoluble matter adhering to the container, rinse the policeman and the container, thoroughly wash the inso
19、luble matter in the crucible with solvent until the filtrate is substantially colorless, then apply strong suction to remove the remaining solvent. Remove the crucible from the tube and wash the bottom free of any dissolved matter. Dry the crucible and contents at 110 5C (230 9F) for at least 20 min
20、. Cool the crucible and contents in a desiccator for at least 20 min and determine the mass. Repeat this procedure until constant mass (0.3 mg) is obtained. Fiberglass filter pads should be used only one time. 10. CALCULATIONS AND REPORT 10.1. Calculate either the total percentage of insoluble matte
21、r or the percentage of the sample soluble in the solvent used as follows: Insoluble, percent 100CAB= (1) ( )Soluble, percent 100B CAB= (2) where: A = mass of crucible and filter; B = total mass of sample; and C = mass of crucible, filter, and insoluble material. 10.1.1. Report the percentage of inso
22、luble material to the nearest 0.1 percent. 11. PRECISION 11.1. Estimates of standard deviations for this procedure and the criteria for judging the acceptability of results (95 percent confidence level) are indicated in Table 1. 2015 by the American Association of State Highway and Transportation Of
23、ficials.All rights reserved. Duplication is a violation of applicable law.TS-2b T 44-4 AASHTO Table 1Standard Deviations Standard Deviations Within-Laboratory VariabilityaBetween-Laboratory VariabilityaStandard DeviationbRepeatabilitycStandard DeviationbReproducibilitydAsphalts solubility more than
24、99 percent (trichloroethylene or 1,1,1 trichloroethane) 0.035 0.10 0.090 0.26 aFor definition of terms and recommended use of precision indexes, see the Recommended Practice for Use of the Terms Precision and Accuracy as Applied to Measurement of a Property of a Material (ASTM E177). bThe standard d
25、eviations shown represent the estimated standard deviation of the measurement process for the stated conditions. They are calculated by multiplying the standard deviations of the applicable data by the factor: where N is the number of tests in the set of data. cTwo results obtained by an operator on
26、 the same sample should be considered suspect if they differ by more than the stated amount. As defined in ASTM E177, this is the “difference two-sigma” limit for single-laboratory-operator-machine-multiday precision. dTwo results obtained by operators in different laboratories should be considered
27、suspect if they differ by more than the stated amount. As defined in ASTM E177, this is the “difference two-sigma” limit for multilaboratory-operator-machine-day precision. The estimates of standard deviation are based on the following: Asphalts Materials 4 Replications 3 Solvents 4 Laboratories 26
28、Degrees of freedom: Within-laboratory variability 159 Between-laboratory variability 81 Standard deviation(s) of data: Within-laboratory variation 0.035 Between-laboratory variation 0.090 11.2. AASHTO Materials Reference Laboratory (AMRL) data for T 44 and ASTM D2042 were analyzed in 2001. These dat
29、a represent approximately 13,200 repetitions of the test conducted on 132 samples having solubility values between 99.5 percent and 100 percent. For samples within this range, the analysis suggests the following precision values are appropriate: Multilaboratory standard deviation (1s) = 0.01 + (0.75
30、 % insoluble) Single-operator standard deviation (1s) = 0.01 + (0.25 % insoluble) 1Similar, but not technically identical to ASTM D2042-01. 2Whatman Grade 934 AH glass microfiber filter pad, available from Reeve Angel & Co., Clifton, NJ, has been found suitable. ( )1411+N 2015 by the American Association of State Highway and Transportation Officials.All rights reserved. Duplication is a violation of applicable law.
