1、Designation: D4 86 (Reapproved 2018)Standard Test Method forBitumen Content1This standard is issued under the fixed designation D4; the number immediately following the designation indicates the year of originaladoption or, in the case of revision, the year of last revision. A number in parentheses
2、indicates the year of last reapproval. A superscriptepsilon () indicates an editorial change since the last revision or reapproval.This standard has been approved for use by agencies of the U.S. Department of Defense.Although this test method was withdrawn by the Society in June 1966 at the request
3、of Committee D04, the Committee onStandards has approved its reinstatement under the jurisdiction of Committee D08 on the basis that Procedure No. 2 still applies totheir interest. Procedure No. 1 has been replaced by Method D 2042, Test for Solubility of Asphalt Materials in Trichloroethylene.1. Sc
4、ope1.1 This test method covers the determination of bitumencontent in materials containing at least 25 % bitumen. Bitumencontent may usually be expeditiously and accurately deter-mined by Procedure No. 1, Section 7. However, some bitumi-nous materials containing finely divided mineral matter mayclog
5、 the filter or the mineral residue may not be easily retained,in which cases Procedure No. 2, Section 8, shall be followed.1.2 The values stated in SI units are to be regarded asstandard. No other units of measurement are included in thisstandard.1.3 This standard does not purport to address all of
6、thesafety concerns, if any, associated with its use. It is theresponsibility of the user of this standard to establish appro-priate safety, health, and environmental practices and deter-mine the applicability and regulatory limitations prior to use.For specific precautionary information, see Section
7、 4.1.4 This international standard was developed in accor-dance with internationally recognized principles on standard-ization established in the Decision on Principles for theDevelopment of International Standards, Guides and Recom-mendations issued by the World Trade Organization TechnicalBarriers
8、 to Trade (TBT) Committee.2. Referenced Documents2.1 ASTM Standards:2D370/D370M Practice for Dehydration of Oil-Type Preser-vativesE177 Practice for Use of the Terms Precision and Bias inASTM Test Methods3. Apparatus, Reagents, and Materials3.1 Filtering Crucible, porcelain, high-form, 25- to 40-mLc
9、apacity, with fine-porosity bottom, 7-m maximum porosity.NOTE 1Selas grade 01, size FC 30 or FC 40, or equivalent. Availablefrom various laboratory supply houses.3.2 Celite Analytical Filter Aid (CAFA), dried to constantmass at 105C and stored in a tightly stoppered container.NOTE 2Use Celite 211 or
10、 Celite 505.3.3 BeakersOne 30-mL beaker, Griffin low-form, and one150-mL beaker, Griffin low-form.3.4 Carbon Disulfide, cp.NOTE 3For filled asphaltic materials, trichloroethylene may bedirectly substituted for carbon disulfide if desired. However, carbondisulfide shall be used in referee testing.3.5
11、 Filtering Flask, with crucible adapter.3.6 Drying Oven.3.7 Bunsen Burner or Muffle Furnace.3.8 Suction Pump.3.9 Analytical Balance.3.10 Desiccator.3.11 Evaporating Dish.3.12 Watch Glasses.4. Safety Precautions4.1 Carbon disulfide is extremely flammable. The vapor willoften ignite spontaneously on c
12、ontact with a hot surface such asa hot plate, oven, or radiator. When using this solvent, be surethat the filtration is conducted under a hood and well awayfrom flame or other sources of heat. Before placing crucibles orother containers in the oven, all traces of carbon disulfideshould be removed (a
13、s indicated by the disappearance of allodor). Otherwise, the vapors will ignite. Carbon disulfide isalso very irritating to the skin and direct contact should beavoided.1This test method is under the jurisdiction ofASTM Committee D08 on Roofingand Waterproofing and is the direct responsibility of Su
14、bcommittee D08.03 onSurfacing and Bituminous Materials for Membrane Waterproofing and Built-upRoofing.Current edition approved May 1, 2018. Published June 2018. Originallyapproved in 1911. Last previous edition approved in 2010 as D4 86 (2010). DOI:10.1520/D0004-86R18.2For referenced ASTM standards,
15、 visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 1942
16、8-2959. United StatesThis international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for theDevelopment of International Standards, Guides and Recommendations issued by the World Trade Organization Techni
17、cal Barriers to Trade (TBT) Committee.15. Preparation of Sample5.1 The sample shall be representative, and if it containsmore than 2 % of water it shall be dehydrated in accordancewith Test Method D370/D370M. If the material is hard andbrittle, it may be ground and dried at a temperature below thete
18、mperature of volatilization of the material.6. Crucible Preparation6.1 If the crucible, after thorough cleaning (see 6.2), hasbeen used for less than six determinations, clean it as follows:Remove the CAFA mat completely, wash the crucible withdistilled water, dry, and ignite in a muffle furnace for
19、1hatabout 800C. Cool the crucible slowly by placing it in a dryingoven for 1 h after removal from the furnace to prevent crackingand place it in a desiccator while still warm.6.2 After the crucible has been used for six determinations,remove any residual ash from pores in the filtering area byboilin
20、g in 1 + 1 hydrochloric acid. Then boil the crucible indistilled water, thoroughly back wash with distilled water, dry,and ignite as in 6.1.7. Procedure No. 17.1 Weigh approximately2gofthesample (size sample toobtain 0.1 to 0.3 g of insoluble matter) into a tared 150-mLbeaker and add 100 mL of carbo
21、n disulfide to the beaker insmall portions, with continuous agitation, until all lumpsdisappear and nothing adheres to the beaker. Cover the beakerwith a watch glass and set it aside for 15 min.7.2 Transfer 0.45 to 0.55 g of dry CAFA to a clean, dry,filtering crucible. Distribute the Celite evenly o
22、ver the bottom.Immediately weigh and record the weight of crucible plusCelite.7.3 Decant the carbon disulfide solution carefully throughthe CAFA mat (previously wetted with carbon disulfide) in theprepared crucible, with or without light suction as may benecessary, retaining as much sediment as poss
23、ible in the beakeruntil the solution has drained through the mat. Wash the beakerwith a small amount of carbon disulfide and transfer allsediment from the beaker to the mat. Do not allow the mat todry out at any time until filtration is complete. Wash withcarbon disulfide until the filtrate is subst
24、antially colorless, thenapply strong suction to remove the remaining carbon disulfide.Remove the crucible from the adapter, wash the bottom free ofany bitumen, and place the crucible on top of the oven untilpractically all of the carbon disulfide has been driven off.(Warningsee 4.1). Place in the ov
25、en at 110 6 10C for atleast 20 min. Cool in a desiccator and weigh.7.4 If insoluble matter adheres to the beaker, dry the beakerin the oven at 110C and weigh. Add the mass of this adherentmaterial as a correction to the mass of the insoluble matter inthe crucible.7.5 If a determination of mineral ma
26、tter is required, ignitethe crucible from 7.3 until it glows with a dull red color. Holdat this temperature until all carbon has been consumed; thenraise the temperature to produce a bright red.After cooling, addto the residue about five times its mass of saturated ammoniumcarbonate solution and let
27、 it digest for1hatroom temperaturein a covered beaker; then dry in an oven at 105 to 110C toconstant mass (Note 4). Add the corrections described in 7.4and, if needed, 7.6 to the mass of mineral matter in the crucible.NOTE 4In the event that water-soluble salts insoluble in carbondisulfide are prese
28、nt, the amount of these salts may be determined inaccordance with the procedure described in the 1937 Report of CommitteeD04 on Road and Paving Materials.37.6 If there is any question involving the amount of mineralmatter that may have passed through the filter, a correction maybe determined as desc
29、ribed in 8.5.8. Procedure No. 28.1 Weigh approximately2gofthesample into a tared50-mL beaker. Add to the beaker about 0.5 g, weighed to thenearest 0.001 g, of freshly dried CAFA. Cover with about 25mL of carbon disulfide and stir the filter aid into the liquid. Letstand, covered with a watch glass,
30、at least 1 h, stirringoccasionally in order to dissolve the sample completely.8.2 Transfer 0.45 to 0.55 g of dry CAFA to a clean, dry,filtering crucible. Distribute the Celite evenly over the bottom.Immediately weigh and record the mass of crucible plus Celite.8.3 Immediately before starting the fil
31、tering process, stir thefilter aid into the liquid. Wet the CAFAmat in the crucible withcarbon disulfide. Pour the solution from the beaker onto thepad, filling the crucible to the top. Apply light suction and, asthe liquid filters through, pour the remaining contents of the50-mL beaker into the cru
32、cible. Wash the beaker with a smallamount of carbon disulfide and transfer all sediment from thebeaker to the mat. Do not allow the CAFA mat to dry out untilfiltration is complete. Wash with carbon disulfide until thefiltrate is substantially colorless, then apply strong suction toremove the remaini
33、ng carbon disulfide. Remove the cruciblefrom the adapter, wash the bottom free of any bitumen, andplace on top of the oven until practically all of the carbondisulfide has been driven off. Place in the oven at 110 6 10Cfor at least 20 min. Cool in a desiccator and weigh.8.4 If insoluble matter adher
34、es to the beaker, dry the beakerin the oven at 110C and weigh. Add the mass of this adherentmaterial as a correction to the mass of the insoluble matter inthe crucible.8.5 Ignite the evaporating dish to a dull red heat, cool in adesiccator, and weigh. Pour the filtrate from the filtering flaskinto t
35、he dish and wash the flask thoroughly with carbondisulfide, putting these washings into the dish also. Burn off thecarbon disulfide in a hood and ignite the residue until no blackor glowing spots remain. Extreme care must be exercisedduring the ignition to prevent the light mineral matter frombeing
36、blown out of the dish. Cool in a desiccator and weighimmediately. This mass shall be added as a correction to theweight of the insoluble matter in the crucible.8.6 If a determination of mineral matter is required, heat thecrucible and its contents from 8.3 until they glow with a dullred color. Hold
37、at this temperature until all carbon has been3Proceedings, ASTM, Vol 37, Part I, 1937, p. 395.D4 86 (2018)2consumed; then raise the temperature to produce a bright red.After cooling, add to the residue about five times its mass ofsaturated ammonium carbonate solution and let it digest for 1h at room
38、 temperature in a covered beaker; then dry in an ovenat 105 to 110C to constant mass (Note 4). Add the correctionsdescribed in 8.4 and 8.5 to the mass of mineral matter in thecrucible.8.7 The mass of additional filter aid used must be subtractedfrom the total mass of insoluble residue and also from
39、the totalmass of mineral matter in the crucible in order to obtain netmass.9. Calculation9.1 Calculate the bitumen content, as follows:% Bitumen % Soluble in Carbon Disulfide! 5 100 2SAB3100D(1)where:A = total mass of insoluble material present, g, andB = total mass of water free sample used, g.9.1.
40、1 Report to the nearest 0.1 %.10. Precision10.1 Estimates of standard deviations () for this proce-dure and the criteria for judging the acceptability of results(95 % confidence level) are listed in Table 1.11. Keywords11.1 bitumen; coal tar; solubilityD4 86 (2018)3ASTM International takes no positi
41、on respecting the validity of any patent rights asserted in connection with any item mentionedin this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the riskof infringement of such rights, are entirely their own responsibility
42、.This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years andif not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standardsand should be addressed to ASTM
43、International Headquarters. Your comments will receive careful consideration at a meeting of theresponsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you shouldmake your views known to the ASTM Committee on Standards, at the address sh
44、own below.This standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,United States. Individual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the aboveaddress or at 610-832-9585 (phone), 610-83
45、2-9555 (fax), or serviceastm.org (e-mail); or through the ASTM website(www.astm.org). Permission rights to photocopy the standard may also be secured from the Copyright Clearance Center, 222Rosewood Drive, Danvers, MA 01923, Tel: (978) 646-2600; http:/ 1 Estimates of Standard DeviationsWithin-labora
46、toryvariabilityABetween-laboratoryvariabilityAStandarddeviation,BRepeat-abilityCStandarddeviationBReproduci-bilityDTars, liquid grades(applicable whencarbon disulfide isused)0.11 0.31 0.22 0.61Tars, semisolid(applicable whencarbon disulfide isused)0.17 0.48 0.83 2.34LiquidTarsSemisolidTarsMaterials
47、1 1Replications 3 3Solvents 1 1Laboratories 8 8Degrees of freedom:Within-laboratory variability 14 15Between-laboratory variability 6 7Standard deviation (S)ofdataWithin-laboratory variation 0.103 0.167Between-laboratory variation 0.208 0.798AFor definitions of terms and recommended use of precision
48、 indexes, see PracticeE177. The estimates of standard deviation are based on the following:BThe standard deviations shown () represent the estimated standard deviationof the measurement process for the stated conditions. They are calculated bymultiplying the standard deviations of the applicable dat
49、a by the factor 1 +14(N1)where N is the number of tests in the set of data.CTwo results obtained by an operator on the same sample should be consideredsuspect if they differ by more than the stated amount.As defined in Practice E177,this is the “difference two-sigma” limits for single-laboratory-operator-machine-multiday precision.DTwo results obtained by operators in different laboratories should be consideredsuspect if they differ by more than the stated amount. As defined in Practice E177this is the “difference two-sigma” l
