1、Designation: D 4312 95a (Reapproved 2005)An American National StandardStandard Test Method forToluene-Insoluble (TI) Content of Tar and Pitch (ShortMethod)1This standard is issued under the fixed designation D 4312; the number immediately following the designation indicates the year oforiginal adopt
2、ion or, in the 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.1. Scope1.1 This test method covers the determination of toluene-insoluble matter (T
3、I) 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 asstandard.1.4 This standard does not purport to address all of thesafety concerns, if any, associated with its use. It is th
4、eresponsibility 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. Specific hazardstatements are given in Section 7.2. Referenced Documents2.1 ASTM Standards:2D95 Test Method for Water in Petrole
5、um Products andBituminous Materials by DistillationD 329 Specification for AcetoneD 362 Specification for Industrial Grade Toluene3D 370 Test Method for Dehydration of Oil-Type Preserva-tivesD 850 Test Method for Distillation of Industrial AromaticHydrocarbons and Related MaterialsD 4072 Test Method
6、 for TolueneInsoluble (TI) Content ofTar and PitchD 4296 Practice for Sampling PitchE11 Specification 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. Si
7、gnificance and Use4.1 This test method is useful for evaluating and character-izing tars and pitches and is one element in establishing theuniformity of shipment or sources of supply.5. Apparatus5.1 Extraction Apparatus, flask with metal cap condenser asshown in Fig. 1.5.2 Extraction Thimbles,Alundu
8、mAN 485 coarse (formerlyRA 98), 30 mm in diameter by 80 mm in height with flatbottom.5.3 Sieves, U.S. Standard 600-m (No. 30) and 250-m (No.60), conforming to Specification E11.5.4 Heater, having a minimum capacity of 300 W per unit.A hot plate or other heaters that maintain the proper reflux ratear
9、e acceptable.6. Reagents6.1 Toluene, Industrial Pure, meeting Specification D 362.6.2 Acetone, meeting the requirements of SpecificationD 329.7. Hazards7.1 Since toluene is a toxic and flammable substance, allworking areas should be efficiently hooded and kept free ofsparks and flames.8. Bulk Sampli
10、ng8.1 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 portion for the determination or for dehydration.9. Dehydration of Sample9.1 Hard PitchIf the solid bulk sample
11、 contains freewater, air-dry a representative portion.9.2 Soft PitchIf the presence of water is indicated bysurface foam on heating, maintain a representative portion ofthe bulk sample of a temperature between 125 and 150C in anopen container until the surface is free of foam. Take care notto overhe
12、at, and remove heat source immediately when foamsubsides.1This test method is under the jurisdiction of ASTM Committee D02 onPetroleum Products and Lubricants and is the direct responsibility of SubcommitteeD02.05 on Properties of Fuels, Petroleum Coke and Carbon Material.Current edition approved Ma
13、y 1, 2005. Published May 2005. Originallyapproved in 1983. Last previous edition approved in 2000 as D 431295a (2000)e1.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer
14、 to the standards Document Summary page onthe ASTM website.3Withdrawn.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.9.3 TarDehydrate a representative portion of the bulksample in accordance with Test Method D 370, but stop thedisti
15、llation when the temperature reaches 170C. Separate anyoil from the water that has distilled over. (If crystals arepresent, warm sufficiently to ensure their solution). Thoroughlymix the oil with the residual tar in the still after the latter hascooled to a moderate temperature.9.3.1 Dehydrate a rep
16、resentative portion of the bulk sampleat atmospheric pressure using a simple side-arm distillationapparatus similar to the one in Test Method D 850 and stop thedistillation when the temperature reaches 170C. Separate anyoil from the water that has distilled over (if crystals are present,warm suffici
17、ently to ensure their solution) and thoroughly mixthe oil with the residual tar in the still after the latter has cooledto a moderate temperature.9.3.2 As an alternative to dehydration, the water content ofthe tar is determined by Test Method D95and, if the watercontent is less than 10 mass %, the T
18、I content is corrected to adry-tar basis (see 13.2). This alternative method applies only tostable emulsions of water in tar, that is, no water separateswhen the tar sample is left undisturbed for 24 h at roomtemperature.10. Preparation of Working Sample10.1 Hard PitchCrush samples to pass a 250-m (
19、60-mesh) screen but so they are retained on a 150 m (100-mesh)screen. Remove pitch from 150-m (100-mesh) screen by abrush. Crushing can be done with a small jaw crusher or amortar and pestle, or both. No particle in the representativesample should be larger than 5 mm in any dimension. Storesieved wo
20、rking sample in a tightly closed container and usewithin 24 h.10.2 Soft PitchIf the pitch is too soft to grind and toosticky to mix, heat a representative portion of the dry sample tothe lowest temperature that will permit passage through600-m (No. 30) sieve, taking care to avoid excessive loss ofvo
21、latile matter. Do not exceed 10 min for this melting period.Pass the heated sample through the 600-m sieve to removeforeign matter.10.3 TarHeat a representative portion of the dry tar to thelowest temperature that will permit passage through the600-m (No. 30) sieve, then filter through this sieve to
22、 removeforeign matter.10.4 Discard working sample 24 h after crushing andsieving as changes in composition sometimes occur in pulver-ized pitch.11. Preparation of Alundum Thimble11.1 Dry the clean thimble in an oven at 105 6 5C for 45min, cool in a desiccator, and weigh to the nearest 0.5 mg.Record
23、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, condition the thimble as described in11.1.11.1.2 After repeated use, boil the thimble in hydro
24、chloricacid (1 + 1) to remove residual ash from the pores. Then boilthe thimble in distilled water and wash with water.After dryingat 105C, ignite and condition the thimble as described in 11.1and 11.1.1.12. Procedure12.1 Weigh 0.50 g sample to the nearest 0.5 mg in a 150 mLtared beaker.12.2 While s
25、tirring sample with a glass rod, add 75 mL ofhot toluene (95 6 5C) and continue stirring for a few minutesuntil the sample is dispersed. Digest sample containing tolueneon an appropriate heat source (preferably a hot water or steambath) at 95 6 5C for 25 min with occasional stirring.12.3 While sampl
26、e is digesting, weigh the alundum thimble,AN 485 (formerly RA 98, 20-m porosity, 30 by 80-mm size)to nearest 0.5 mg. Place the thimble in a filtering tube, whichis supported on a funnel rack or equivalent apparatus to drainsoluble portion of sample.12.4 Pour the digested sample into the thimble.Avoi
27、d fillingthe thimble higher than 20 mm from the top. Use a glass rod,a brush, or a rubber policeman, if necessary, and cold toluenefrom a wash bottle to completely transfer the insolubleparticles into the thimble.12.5 When most of the solution has drained from thethimble, transfer the thimble to the
28、 extraction apparatus asdescribed in Test Method D 4072. With a beaker, add hottoluene to extraction flask. Fill to a level approximately 25 mmbelow the bottom of thimble.12.6 Adjust the hot plate, and set the drip (reflux) rate oftoluene at 120 to 150 drops/min from the condenser to maintainthe lev
29、el of liquid in the thimble. Continue extraction for 3 h.The liquid level is easily observed if the paper cone is replacedwith one made from coarse stainless steel or brass screen.However, it is not necessary to use a cone.NOTE 1One could fill extraction flask to required level, turn heat onbefore t
30、himble is placed into basket.12.7 Cut heat off, let drain, remove with tongs, and placethimble in filtering tube. Wash the inside and outside of thimblewith acetone several times from a wash bottle, starting fromtop of thimble (several small washes are more efficient thanFIG. 1 Extraction ApparatusD
31、 4312 95a (2005)2filling the thimble). Place thimble in an oven at 110 6 5C for30 min. Cool in a desiccator and weigh.13. Calculation13.1 Calculate the toluene-insoluble (TI) content as follows:TI, mass % 5 100B 2 A!/C (1)where:A = mass of the alundum thimble,B = mass of alundum thimble plus toluene
32、-insolubles, andC = mass of sample.13.2 If the TI was determined on a wet tar sample (see9.3.2), 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) c
33、ontent to the nearest0.1 %.15. Precision and Bias15.1 Based upon present available data, the following cri-teria shall be used for judging the acceptability of results (95 %probability):15.1.1 RepeatabilityDuplicate values by the same opera-tor shall not be considered suspect unless the determinedpe
34、rcentages differ by more than 1.0.15.1.2 ReproducibilityThe values reported by each of twolaboratories, representing the arithmetic average of duplicatedeterminations, shall not be considered suspect unless thereported percentages differ by more than 3.0.15.2 BiasDuring the interlaboratory study to
35、determinethe precision of this test method, the TI was also determined byTest Method D 4072 (long method). It was found that the TIdetermined by Test Method D 4312 was higher than thatdetermined by Test Method D 4072 by an average value ofabout 1 percentage point.16. Keywords16.1 beta resin; pitch;
36、soft 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 validity of any such patent rights, and the risk
37、of 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 comments are invited either for revision of this
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39、our 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 4312 95a (2005)3
