1、Designation: D 2172 05Standard Test Methods forQuantitative Extraction of Bitumen From Bituminous PavingMixtures1This standard is issued under the fixed designation D 2172; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year o
2、f last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon (e) indicates an editorial change since the last revision or reapproval.This standard has been approved for use by agencies of the Department of Defense.1. Scope1.1 These test methods cover the quant
3、itative determinationof bitumen in hot-mixed paving mixtures and pavementsamples. Aggregate obtained by these test methods may beused for sieve analysis using Test Method C117 and TestMethod C 136.1.2 The values stated in inch-pound units are to be regardedas the standard. The values given in parent
4、heses are forinformation only.1.3 This standard does not purport to address all of thesafety concerns, if any, associated with its use. It is theresponsibility of the user of this standard to establish appro-priate safety and health practices and determine the applica-bility of regulatory limitation
5、s prior to use. Specific hazards aregiven in Section 7.NOTE 1The results obtained by these test methods may be affected bythe age of the material tested, with older samples tending to yield slightlylower bitumen content. Best quantitative results are obtained when the testis made on mixtures and pav
6、ements shortly after their preparation. It isdifficult to remove all the asphalt when some aggregates are used andsome chlorides may remain within the mineral matter affecting themeasured asphalt content.2. Referenced Documents2.1 ASTM Standards:2C117 Test Method for Materials Finer than 75-m (No.20
7、0) Sieve in Mineral Aggregates by WashingC 128 Test Method for Density, Relative Density (SpecificGravity), and Absorption of Fine AggregateC 136 Test Method for Sieve Analysis of Fine and CoarseAggregatesC 670 Practice for Preparing Precision and Bias Statementsfor Test Methods for Construction Mat
8、erialsD70 Test Method for Specific Gravity and Density ofSemi-Solid Bituminous Materials (Pycnometer Method)D 604 Specification for Diatomaceous Silica Pigment3D 979 Practice for Sampling Bituminous Paving MixturesD 1461 Test Method for Moisture or Volatile Distillates inBituminous Paving MixturesD
9、1856 Test Method for Recovery of Asphalt from Solutionby Abson MethodD 2111 Test Methods for Specific Gravity and Density ofHalogenated Organic Solvents and Their AdmixturesD 6368 Specification for Vapor-Degreasing Grade and Gen-eral Grade normalPropyl Bromide2.2 Federal Specifications:O-T-634 (late
10、st) normal Propyl Bromide, Technical43. Summary of Test Methods3.1 The paving mixture is extracted with trichloroethylene,normal Propyl Bromide, or methylene chloride using theextraction equipment applicable to the particular method. Thebitumen content is calculated by difference from the mass ofthe
11、 extracted aggregate, moisture content, and mineral matterin the extract. The bitumen content is expressed as masspercent of moisture-free mixtures.4. Significance and Use4.1 All of these test methods can be used for quantitativedeterminations of bitumen in hot-mixed paving mixtures andpavement samp
12、les for specification acceptance, service evalu-ation, control, and research. Each method prescribes thesolvent or solvents and any other reagents that can be used inthe test method. Test Method D 1856 requires that MethodAbeused when asphalt is recovered from solution.5. Apparatus5.1 Oven, capable
13、of maintaining the temperature at 230 69F (110 6 5C).5.2 Pan, flat, 12 in. (305 mm) long, 8 in. (203 mm) wide,and 1 in. (25 mm) deep.1These test methods are under the jurisdiction of ASTM Committee D04 onRoad and Paving Materials and are the direct responsibilities of SubcommitteeD04.25 on Analysis
14、of Bituminous Mixtures.Current edition approved July 15, 2005. Published August 2005. Originallyapproved in 1963. Last previous edition approved in 2001 as D 2172 01e1.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual
15、 Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.3Withdrawn.4Available from Standardization Documents Order Desk, Bldg. 4 Section D, 700Robbins Ave., Philadelphia, PA 19111-5094, Attn: NPODS.1Copyright ASTM International, 100 Barr Harbor Driv
16、e, PO Box C700, West Conshohocken, PA 19428-2959, United States.5.3 Balance, or balances having an accuracy of at least0.01 % of the sample mass.5.4 Hot Plate, electric, 700-W continuous or low, medium,and high settings.5.5 Small-Mouth Graduate, 1000 or 2000-mL capacity.Optional small-mouth graduate
17、, 100-mL capacity.5.6 Ignition Dish, 125-mL capacity.5.7 Desiccator.5.8 Analytical Balance.6. Reagents6.1 Purity of ReagentsReagent grade chemicals shall beused in all tests. Unless otherwise indicated, it is intended thatall reagents shall conform to the specifications of the Commit-tee onAnalytica
18、l Reagents of theAmerican Chemical Society,5where such specifications are available. Other grades may beused, provided it is first ascertained that the reagent is ofsufficiently high purity to permit its use without lessening theaccuracy of the determination.6.2 Ammonium Carbonate SolutionSaturated
19、solution ofreagent grade ammonium carbonate (NH4)2CO3.6.3 Methylene Chloride, technical grade. CautionseeSection 7.6.4 normal-Propyl Bromide (nPB), conforming to Specifi-cation D 6368. Cautionsee Section 7.6.5 Trichloroethylene, technical grade, Type 1, FederalSpecification O-T-634, latest revision.
20、 Cautionsee Section7.7. Hazards7.1 CautionThe solvents listed in Section 6 should beused only under a hood or with an effective surface exhaustsystem in a well-ventilated area, since they are toxic to variousdegrees. Consult the current Threshold Limit ConcentrationCommittee of the American Conferen
21、ce of GovernmentalIndustrial Hygienists6for the current threshold limit values.8. Sampling8.1 Obtain samples in accordance with Practice D 979.8.2 Preparation of Test Specimens:8.2.1 If the mixture is not sufficiently soft to separate with aspatula or trowel, place it in a large, flat pan and warm t
22、o 2306 9F (110 6 5C) only until it can be handled or mixed. Splitor quarter the material until the mass of material required fortest is obtained.8.2.2 The size of the test sample shall be governed by thenominal maximum aggregate size of the mixture and shallconform to the mass requirement shown in T
23、able 1 (Note 2):NOTE 2When the mass of the test specimen exceeds the capacity ofthe equipment used (for a particular method), the test specimen may bedivided into suitable increments, tested, and the results appropriatelycombined for calculation of bitumen content (Section 12).8.2.3 In addition, a t
24、est specimen is required for the deter-mination of moisture (Section 9) in the mixtures. Take this testspecimen from the remaining sample of the mixture immedi-ately after obtaining the extraction test specimen.NOTE 3If recovery of bitumen from the solution obtained from theextraction test is not re
25、quired, the entire test specimen may be dried toconstant mass in an oven at a temperature of 230 6 9F (110 6 5C) priorto extraction instead of determining the moisture content (Section 9).9. Moisture Content9.1 Determine the moisture content of the mixture (see8.2.2) in accordance using the procedur
26、e described in TestMethod D 1461.9.2 Calculate the mass of water, W2,(12.1) in the extractiontest portion by multiplying mass percent water (9.1)bythemass of the extraction test portion, W1,(12.1).TEST METHOD A10. Apparatus10.1 In addition to the apparatus listed in Section 5, thefollowing apparatus
27、 is required for Test Method A:10.1.1 Extraction Apparatus, consisting of a bowl approxi-mating that shown in Fig. 1 and an apparatus in which the bowlmay be revolved at controlled variable speeds up to 3600r/min. The speed may be controlled manually or with a presetspeed control. The apparatus shou
28、ld be provided with acontainer for catching the solvent thrown from the bowl and adrain for removing the solvent. The apparatus preferably shallbe provided with explosion-proof features and installed in ahood or an effective surface exhaust system to provide venti-lation.NOTE 4Similar apparatus of l
29、arger size may be used.10.1.2 Filter Rings, felt or paper, to fit the rim of the bowl.10.1.3 Low-ash paper filter rings may be used in place of thefelt filter ring (10.1.2). Such filter rings shall consist of low ashfilter paper stock 0.05 6 0.005 in. thick. The nominal baseweight of the paper shall
30、 be 330 6 30 lb for a ream (500sheets25 by 38 in.). The ash content of the paper should notexceed 0.2 % (approximately 0.034 g per ring).11. Procedure11.1 Determine the moisture content of the material inaccordance with Section 9.5Reagent Chemicals, American Chemical Society Specifications, American
31、Chemical Society, Washington, DC. For suggestions on the testing of reagents notlisted by the American Chemical Society, see Analar Standards for LaboratoryChemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeiaand National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC),
32、Rockville,MD.6Available from American Conference of Governmental Industrial Hygienists,1330 Kemper Meadow Drive, Cincinnati, OH 45240, (513) 7422020, (www.acgi-h.org).TABLE 1 Size of SampleNominal MaximumAggregate Size Standard,mmSieve SizeMinimum Mass of Sample,kg4.75 (No. 4) 0.59.538 in. 112.512 i
33、n. 1.519.034 in. 225.0 1 in. 337.5 112 in. 4D217205211.2 Place a 650 to 2500-g test portion into a bowl. SeeAnnex A1 for alternative procedures to those prescribed hereinand in 11.5.11.3 Cover the test portion in the bowl with trichloroethyl-ene, normal Propyl Bromide, or methylene chloride and allo
34、wsufficient time for the solvent to disintegrate the test portion(not over 1 h). Place the bowl containing the test portion andthe solvent in the extraction apparatus. Dry and determine themass of the filter ring and fit it around the edge of the bowl.Clamp the cover on the bowl tightly and place a
35、beaker underthe drain to collect the extract.11.4 Start the centrifuge revolving slowly and graduallyincrease the speed to a maximum of 3600 r/min or until solventceases to flow from the drain. Allow the machine to stop, add200 mL of trichloroethylene, normal Propyl Bromide, ormethylene chloride and
36、 repeat the procedure. Use sufficient200-mL solvent additions (not less than three) so that theextract is not darker than a light straw color. Collect the extractand the washings in a suitable graduate.11.5 Remove the filter ring from the bowl and dry in air. Iffelt filter rings are used, brush off
37、mineral matter adhering tothe surface of the ring and add to the extracted aggregate. Drythe ring to constant mass in an oven at 230 6 9F (110 6 5C).Carefully remove all the contents of the bowl into a metal panand dry on a steam bath and then, dry to constant mass in anoven or on a hot plate at 230
38、6 9F (110 6 5C). Iftrichloroethylene or normal Propyl Bromide is used as theextraction solvent, the preliminary drying on a steam bath maybe omitted. The mass of the extracted aggregate, W3, is equalto the mass of the aggregate in the pan plus the increase in massof the filter rings.11.5.1 Use the f
39、ollowing alternative procedure when low-ash filter rings are used: Place the aggregate and filter rings ina clean metal pan. Dry as specified above. Carefully fold thedried filter ring and stand it on the aggregate. Burn the filterring by igniting with a bunsen burner or match. Determine themass of
40、the extracted aggregate in the pan, W3.NOTE 5Since dry aggregate absorbs moisture when exposed to aircontaining moisture, determine the mass of the extracted aggregateimmediately after cooling to a suitable temperature.11.6 Determine the amount of mineral matter in the extractby any of the following
41、 test methods:11.6.1 Ashing Method:11.6.1.1 Record the volume of the total extract in thegraduate (11.4). Determine the mass of an ignition dish.Agitatethe extract thoroughly and immediately measure approximately100 mL into the ignition dish. Evaporate to dryness on a steambath or hot plate, except
42、use a steam bath when the solvent isbenzene. Ash residue at a dull red heat (500 to 600C), cool,and add 5 mL of saturated ammonium carbonate solution pergram of ash. Digest at room temperature for 1 h. Dry in an ovenat 100C to constant mass, cool in a desiccator, and determinethe mass.11.6.1.2 Calcu
43、late the mass of mineral matter in the totalvolume of extract, W4, as follows:W45 GV1/V12 V2!# (1)NOTE 1See Table 2 for metric equivalents.FIG. 1 Extraction Unit Bowl (Test Method A)D2172053where:G = ash in aliquot, g,V1= total volume, mL, andV2= volume after removing aliquot, mL.11.6.2 Centrifuge M
44、ethod:11.6.2.1 For this test method use any suitable high-speed(3000 g or higher) centrifuge of the continuous-flow type.11.6.2.2 Determine the mass of a clean empty centrifugecup (or bowl) to 0.01 6 0.005 g and place in the centrifuge.Position a container at the appropriate spout to catch theefflue
45、nt from the centrifuging operation. Transfer all of theextract (from Test Methods A, B, C, D, or E as appropriate) toan appropriate (feed) container suitably equipped with a feedcontrol (valve or clamp, etc.). To ensure quantitative transfer ofthe extract to the feed container, the receptacle contai
46、ning theextract should be washed several times with small amounts ofclean solvent and the washings added to the feed container.Start the centrifuge and allow to reach a constant operationalspeed (for example, 9000 r/min for the SMM type and20 000 + r/min for the Sharples type). Open the feed line an
47、dfeed the extract into the centrifuge at a rate of 100 to 150mL/min.After all the extract has passed through the centrifuge,wash the feed mechanism (with centrifuge still running) withseveral increments of clean solvent, allowing each increment torun through the centrifuge until the effluent is esse
48、ntiallycolorless.11.6.2.3 Allow the centrifuge to stop and remove the cup (orbowl). Clean the outside with fresh solvent. Allow the residualsolvent to evaporate in a funnel or steam hood and then dry thecontainer in an oven controlled at 230 6 9F (110 6 5C).Cool the container and redetermine the mas
49、s immediately. Theincrease in mass is the mass of mineral matter, W4,(12.1)intheextract.11.6.3 Volumetric Method:11.6.3.1 Place the extract in a previously tared and cali-brated flask. Place the flask in a controlled-temperature bathcontrolled to 0.2F (60.1C), and allow to come to thetemperature at which the flask was calibrated. When thedesired temperature has been reached, fill the flask with solventwhich has been kept at the same temperature. Bring the level ofthe liquid in the flask up to the neck, insert the stopper, makingsure the liquid
