1、Designation: D 4072 98 (Reapproved 2003)e1An American National StandardStandard Test Method forToluene-Insoluble (TI) Content of Tar and Pitch1This standard is issued under the fixed designation D 4072; the number immediately following the designation indicates the year oforiginal adoption or, in th
2、e case of revision, the year of 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.e1NOTEWarning notes were editorially moved into the standard text in November 2003.1. Scope1.1 Th
3、is test method covers the determination of toluene-insoluble matter (TI) in tar and pitch.1.2 Since this test method is empirical, strict adherence toall details of the procedure is necessary.1.3 The values stated in SI units are to be regarded as thestandard.1.4 This standard does not purport to ad
4、dress 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 limitations prior to use. For specific hazardinformation, see Section 7.2. Refer
5、enced Documents2.1 ASTM Standards:2D95 Test Method for Water in Petroleum Products andBituminous Materials by DistillationD 362 Specification for Industrial Grade TolueneD 850 Test Method for Distillation of Industrial AromaticHydrocarbons and Related MaterialsD 4296 Practice for Sampling PitchE11 S
6、pecification for Wire Cloth and Sieves for TestingPurposes3. Summary of Test Method3.1 The sample is digested, then extracted with hot toluenein an alundum thimble. The insoluble matter is dried andweighed.4. Significance and Use4.1 This test method is useful for evaluating and character-izing tars
7、and pitches and as one element in establishing theuniformity of shipments or sources of supply.5. Apparatus5.1 Extraction ApparatusFlask with metal cap condenseras shown in Fig. 1.5.2 Extraction Thimble, Alundum AN 485 coarse (formerlyRA 98), 30 mm in diameter by 80 mm in height with flatbottom.5.3
8、Thimble CoverPaper cone, made by wetting withwater a 70-mm filter paper normally folded in a small glassfunnel, and drying the funnel in an oven with the paper cone inplace.5.4 Sieves, U.S. Standard 600-m (No. 30) and 250-m (No.60), conforming to Specification E11.5.5 Heater, having a minimum capaci
9、ty of 300 W per unit.6. Reagents6.1 Toluene, Industrial Pure, meeting Specification D 362.(WarningFlammable.)6.2 Concentrated Hydrochloric Acid. (WarningCorrosive.)7. Hazards7.1 Since toluene is a toxic and flammable substance, allworking areas should be efficiently hooded and kept free ofsparks and
10、 flames.7.2 Observe proper laboratory procedures for handling anddiluting hydrochloric acid.8. Bulk Sampling8.1 Samples from shipments shall be taken in accordancewith Practice D 4296, and shall be free of foreign substances.Thoroughly mix the sample immediately before removing arepresentative porti
11、on for the determination or for dehydration.9. Dehydration of Sample9.1 Hard PitchIf the solid bulk sample contains freewater, air-dry a representative portion in a forced draft oven at50C.9.2 Soft PitchIf the presence of water is indicated bysurface foam on heating, maintain a representative portio
12、n ofthe bulk sample of a temperature between 125 and 150C in anopen container until the surface is free of foam. Take care notto overheat, and remove heat source immediately when foamsubsides.1This test method is under the jurisdiction of ASTM Committee D02 onPetroleum Products and Lubricants and is
13、 the direct responsibility of SubcommitteeD02.05 on Properties of Fuels, Petroleum Coke and Carbon Material.Current edition approved Nov. 18, 2003. Published November 2003. Originallyapproved in 1981. Last previous edition approved in 1998 as D 407298.2For referenced ASTM standards, visit the ASTM w
14、ebsite, 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.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United S
15、tates.9.3 TarDehydrate a representative portion of the bulksample at atmospheric pressure using a simple side-armdistillation apparatus similar to the one in Test Method D 850and stop the distillation when the temperature reaches 170C.Separate any oil from the water that has distilled over (ifcrysta
16、ls are present, warm sufficiently to ensure their solution)and thoroughly mix the oil with the residual tar in the still afterthe latter has cooled to a moderate temperature.9.3.1 As an alternative to dehydration, the water content ofthe tar is determined by Test Method D95and, if the watercontent i
17、s less than 10 mass percent, the TI content is correctedto a dry-tar basis (see 13.2). This alternative method appliesonly to stable emulsions of water in tar, that is, no waterseparates when the tar sample is left undisturbed for 24 h atroom temperature.10. Preparation of Working Sample10.1 Hard Pi
18、tchIf the pitch can be crushed at roomtemperature, prepare a 20-g working sample by suitablecrushing, mixing, and quartering of a representative portion ofthe dry sample. The crushing can be done with a small jawcrusher and a mullite mortar and pestle. No particle in therepresentative sample shall b
19、e larger than 5 mm in anydimension. Crush this sample so that all of it will pass the250-m (No. 60) sieve. Store the sieved working sample in atightly closed container and use within 24 h (see 10.4).10.2 Soft PitchIf the pitch is too soft to grind and toosticky to mix, heat a representative portion
20、of the dry sample tothe lowest temperature that will permit passage through the600-m (No. 30) sieve. Do not exceed 10 min for this meltingperiod. Pass the heated sample through the 600-m sieve toremove foreign matter.10.3 TarHeat a representative portion of the tar to thelowest temperature that will
21、 permit passage through the600-m (No. 30) sieve: then filter through this sieve to removeforeign matter.10.4 Discard working samples 24 h after crushing andsieving as changes in composition sometimes occur in pulver-ized pitch.11. Preparation of Extraction Thimble11.1 Dry the clean thimble in an ove
22、n at 105 6 5C for 45min, cool in a desiccator, and weigh to the nearest 0.5 mg.Record the mass.11.1.1 After each use, ignite the thimble at 700 to 800C fora few hours. Cool the thimble slowly by placing in a dryingoven for 1 h after removal from the furnace to preventcracking. Before reuse, conditio
23、n the thimble as described in11.1.11.1.2 After repeated use, boil the thimble in 1 + 1 hydro-chloric acid. (Add equal volume of concentrated hydrochloricacid to distilled water.) to remove residual ash from the pores.Then boil the thimble in distilled water and wash with water.After drying at 105C,
24、ignite and condition the thimble asdescribed in 11.1 and 11.1.1.12. Procedure12.1 The mass of sample taken for analysis shall yieldbetween 150 and 250 mg of matter insoluble in toluene (TI),unless this would require less than the minimum acceptablesample mass of 1 g, in which case 1 g shall be used.
25、12.2 Place the required amount of sample in a tared 150-mLbeaker and weigh to the nearest 0.5 mg. Pour 60 mL of tolueneinto the beaker, stirring continuously while introducing thetoluene, to ensure complete mixture of the sample and tolueneand thorough dispersion of the insoluble matter (see 7.1). P
26、lacethe beaker on an electric hot plate or on a steam or water bathand heat the contents to a temperature of 95 6 5C. Maintainthis temperature for 25 min. Stir occasionally with a stirringrod during this period to ensure that the sample is completelydispersed in the toluene. Check for completeness o
27、f dispersionby inspecting the bottom of the beaker for undigested material.12.3 Place the tared extraction thimble in a filter tubesupported over a beaker or flask. Wet the thimble completelywith toluene. After digestion, carefully decant portions of thehot mixture into the wetted thimble (see 7.1).
28、 Do not permit thelevel of the toluene to rise higher than 20 mm from the top ofthe thimble. It is advisable while filtering to retain the majorpart of the insoluble matter in the beaker. Finally transfer theinsoluble matter from the beaker to the thimble with smallportions of toluene. Wash the beak
29、er with toluene until it isclean, using a suitable brush or policeman to detach anyparticles adhering to the beaker. Transfer all washings to thethimble.12.4 When almost all toluene has drained from the thimble,wash the thimble and its contents once with a small quantity oftoluene. Allow the toluene
30、 to drain from the thimble.12.5 While the extraction thimble is still moist with toluene,remove it from the filter tube and place it in the wire supportof the extraction apparatus. Cover the thimble with the papercone, point down. Assemble the extraction apparatus on a hotplate, with a felt gasket b
31、etween the top of the extraction flaskand condenser cover, and with fresh toluene in the bottom ofthe extraction flask. Add three to six small lumps of pumicestone to the flask to promote smooth boiling, thereby prevent-ing bumping and spattering during extraction. The surface ofthe toluene in the f
32、lask shall be about 25 mm below the bottomof the thimble (see 7.1).FIG. 1 Extraction ApparatusD 4072 98 (2003)e1212.6 Conduct the extraction at such a rate of heating thatcondensed toluene falls continuously from the condenser at arate of not less than 1 nor more than 2 drops/s. Continue theextracti
33、on at this rate for a period of 18 h (Note 1).NOTE 1The reflux rate can be affected by the ambient temperature,especially when the apparatus is operating overnight unattended (forexample, the temperature of the laboratory is reduced at night and thereflux rate slows or ceases). One way to alleviate
34、this condition is to placea metal shield around the heater and extraction apparatus which wouldprevent the colder air entering the hood from excessively cooling theextraction apparatus. The shield can be as simple as a can with the endscut out.12.7 At the end of this period, remove the heat source a
35、ndallow the toluene to drain from the thimble, then remove thethimble from the extraction apparatus. Remove the paper coneand gently lay the thimble on its side, with the open end tiltedup, on a watch glass in the fume hood so that the toluene canevaporate. Leave it for 30 min. Place the air-dried t
36、himble in adrying oven at 105 6 5C for 60 min. Remove the dry thimblefrom the oven and place it immediately in a desiccator. Whencool, weigh the thimble and contents to the nearest 0.5 mg, andrecord the mass (see 12.8).12.8 If the mass of matter insoluble in toluene is less than150 mg or more than 2
37、50 mg, repeat the determination with anadjusted sample weight of not less than 1 g (see 11.1).13. Calculation13.1 Calculate the toluene-insoluble (TI) content as follows:TI,%5 B 2 A!/C 3 100 (1)where:A = mass of alundum thimble without cone,B = mass of alundum thimble plus toluene-insoluble mate-ria
38、l, andC = mass of sample.13.2 If the TI was determined on a wet tar sample (see9.3.1), correct the TI value determined in 13.1 to a dry-tar basisas follows:TI mass % dry basis!5TI mass % wet basis!100 2 water content of tar, mass %!3 100(2)14. Report14.1 Report the toluene-insoluble (TI) content to
39、the nearest0.1 %.15. Precision and Bias15.1 The following criteria shall be used for judging theacceptability of results (95 % probability):15.1.1 RepeatabilityDuplicate values by the same opera-tor shall not be considered suspect unless the determinedpercentages differ by more than 0.9.15.1.2 Repro
40、ducibilityThe values reported by each of twolaboratories, representing the arithmetic average of duplicatedeterminations, shall not be considered suspect unless thereported percentages differ by more than 2.0.15.2 BiasThis procedure has no bias because the value oftoluene insoluble is defined in ter
41、ms of this test method.16. Keywords16.1 extraction; pitch; tar; toluene-insolublesASTM International takes no position 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 v
42、alidity of any such patent rights, and the riskof infringement of such rights, are entirely their own responsibility.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 c
43、omments are invited either for revision of this standard or for additional standardsand should be addressed to ASTM 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 ha
44、ve not received a fair hearing you shouldmake your views known to the ASTM Committee on Standards, at the address shown 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), 610-832-9555 (fax), or serviceastm.org (e-mail); or through the ASTM website(www.astm.org).D 4072 98 (2003)e13
