1. SCOPE 1.1 This method covers the determi- nation of the degree of solubility in ti- chloroethylene or 1,1,1 trichloroethane of asphalt materials having little or no mineral matter. 12 The values stated in SI units are to be regarded as the standard, 82. SUMMARY OF METHOD Aut “The sample is dissolved in tri- chlorosthyleae or 1,1,1 trichloroethane and filtered through a filter mat. The insolublo material is washed, dried, + and weighed, ~ 3, SIGNIFICANCE AND USE 3.1_ This method is a measure of the solubility of asphalt in trichloroethylene or 1,1,1 tichloroethane. The portion that is soluble in trichloroethylene or 1,1,1 (cichloroothane represents the active ce- rong constituents, 4, APPARATUS AND MATERIALS 4.1 The assembly of the filtering ap- paratus is illustrated in Figure 1. Details of the component parts are as follows 4.1.1 Gooch Crucible, glazed inside and outside withthe exception of outside bottom surface. The approximate dimen- sions shall be a diameter of 44 mm at top, tapering to 36 mm at bottom, and a depth of 28 mm. 66 Standard Specification for Solubility of Bituminous Materials AASHTO DESIGNATION: T 44-96! (ASTM DESIGNATION: D 2042-93) 412. Glass Fiber Pad, 32, 35, or 37 mm in diameter? 413° Filter Flask, beavy-wall, with side tube, 250 mL capacity or larger 414 Filter Tube, 40 to 42 mm in- side diametec. 415 Rubber Tubing or Adapter, for holding the Gooch erucible on the fil- ter tube, NOTE 1—Other suitable assemblies per- ‘iting vacuum filration with a Gooch eruci- bie may be used. 42. Erlenmeyer Flask, 125-mL, or other suitable container. 43° Oven, capable of maintaining @ temperature of 110 + 5°C (230 = 9°F). 44 Desiccator, of suitable size, charged with an effective desiccant. 45 Analytical Balance, class A con- forming to the requirements of AASHTO Specification M 231. 5. SOLVENT SaL_Technical grade, Type 1, Tricho- lorethylene or technical grade 1.1.1 rricholorethane. 6. SAFETY PRECAUTIONS 6.1 Trichloroethylene and 1,1,1 wi- chloroethane are toxic materials and strict adherence to instructions in Mate- rial Safety Data Sheets are to be fol- Towed. Caution: Trichloroethylene and 1,1,1 trichloroethane in the presence of ‘pa aval from Reeves Angel Co Clifton, NI is ore found sabe hheat and moisture may form acids that are extremely corrosive. 7. PREPARATION OF GOOCH CRUCIBLE. 7A Assemble the filtering apparatus as shown in Figure 1. Place filter pad {nto the gooch crucible, moisten the pad ‘with solvent and seat firmly inthe bottom of the crucible with light suction. Dry the crucible and contents at 110 + $°C (230 + 9°F) for at least 20 minutes. Cool the crucible and contents in a desiccator for at least 20 minutes and determine the mass, Repeat this procedure until constant mass (+ 0.3 mg) is obtained. ‘Store in 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 suffi- ciently fuid to pour, occasionally siting the sample to aid heat transfer and 10 assure uniformity. Avoid the entrapment of ait. FIGURE 1 Filtering Apparatus ‘AssemblyStandurd Devons Wihin-Laboraory Between-Labortory Varabiliny Varabiliy™ Standara ‘Siandard Deviation’ Repeatability’ Deviation’ Reproduibiliyé ia solutly more tan 99 «0038S ca percent (chlooetyene oF 1. ehlowethane) For dctnwon of and eremmenicd we of precio Indes. ae the Resonmended Pace for Ue FE ott Tern Pccson and Accarcy 3s Applied to Mesures of oper of 3 Material (ASTM € 170), Te sumiard cevitons shown represent he imate andar devon of the ene proces fo the aued condone. They se clued by Huipyng the Sandal devin 0 the sppicable aa by We for where ithe numer oft ine se faa "Jeo ez bind by an opera on he ame spe shoul be conieed saps if thy ier by mere ‘tune sted arsunt Ascend in Recommended Pcie € 177 tha he ference torment fot “Ft rss obit by opts ieee aber soo be conse suet if hey ile by ere tan ested amour. Ae defined in Recorended Pre £177 thi te “een worema” ii or 9. PROCEDURE Wet the filter pad with a small portion of clean solvent and decant the solution 9.1 Note safety precautions in Sec- through the filter pad of the crucible with tion 6. Transfer approximately 2 g of the light suction. sample into a tared 125-mL Erlenmeyer _ When the insoluble matters apprecia- flask or other suitable container, Allow ble, retain as much of it as possible in the the container and its contents to cool {9 container until the solution has drained ambient temperatures and weigh to the through the filter pad. Wash the container nearest 1 mg. Add 100 mL ofthe trichlo- witha small amount of solvent and, using roethylene or I,1,Itrichloroethane to the 2 stream of solvent from a wash botle, container, stopper flask and agitate as transfer all insoluble matter to the cruci- necessary until the sample is dissolved ble. Use a “policeman” if necessary to and no undissolved material adheres 19 temove any insoluble matter adhering to the container. Check for undissolved ma- the container, rinse the policeman and the terial after a period of at least 15 container, thoroughly wash the insoluble minutes. matter in the crucible with solvent until Normally the temperature at which the filtrate is substantially colorless, then this testis run is not critical and it may apply strong suction to remove the re be performed at the laboratory air tem- maining solvent. Remove the crucible perature. For referee tests, however, the from the tube and wash the bottom free flask and sample in solution shall be of any dissolved mater. Dry the crucible placed in a water bath maintained at 37.8 and contents at 110 * S°C (230 + °F) = 0.25°C (100 = 05°F), for 1 hour fora least 20 minutes. Cool the crucible before filtering. and contents in a desiccator for at least 92 Place the previously prepared 20 minutes and determine the mass, Re- and tared Gooch crucible in the filter- peat this procedure until constant mass ing tube, (© 03 mg) is obtained. any METHODS OF SAMPLING AND TESTING 67 Fiber glass filter pads should be used only one time. 10, CALCULATIONS AND REPORT 10.1 Calculate either the total per- centage of insoluble matter or the per- centage of the sample soluble in the solvent used as follows: Ine, ces = 4 10 Soluble, percent where: A B total mass insoluble, and total mass of sample. 10.11 For percentages of insoluble less than 1.0, report to the nearest 0.01 percent; for percentages of insoluble 1.0 ‘or more report to the nearest 0.1 percent AL, PRECISION ALA Estimates of standard devia- tions for this procedure and the criteria, for judging the acceptability of results (95 percent confidence level) are indi- cated in the table entitled “Standard Deviations". ‘The estimates of standard deviation are based on the following: _Ssphats_ Materials + Repictons 3 Solvens 4 Laboratories 26 Degrees of feedom Withindaboraory variability 159 Berweenisborator: varbiliy SI Standard deviation (8) of dats ‘Withielabortory sanition aos Beweeniaborator: vanation 0.090,