1、Designation: D4312 95a (Reapproved 2010)Standard Test Method forToluene-Insoluble (TI) Content of Tar and Pitch (ShortMethod)1This standard is issued under the fixed designation D4312; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision
2、, the year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.1. Scope1.1 This test method covers the determination of toluene-insoluble matter (TI) in tar and pitch.1.2 Since th
3、is 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 theresponsibility of the user of t
4、his 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 Petroleum Products andBituminous Materi
5、als by DistillationD329 Specification for AcetoneD362 Specification for Industrial Grade Toluene3D370 Practice for Dehydration of Oil-Type PreservativesD850 Test Method for Distillation of Industrial AromaticHydrocarbons and Related MaterialsD4072 Test Method for Toluene-Insoluble (TI) Content ofTar
6、 and PitchD4296 Practice for Sampling PitchE11 Specification for Woven Wire Test Sieve Cloth and TestSieves3. 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 i
7、s 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,AlundumAN 485 coarse (formerlyRA 98), 30 mm in
8、 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 rateare acceptable.6. Reagents6.1 Toluene, Ind
9、ustrial Pure, meeting Specification D362.6.2 Acetone, meeting the requirements of SpecificationD329.7. Hazards7.1 Since toluene is a toxic and flammable substance, allworking areas should be efficiently hooded and kept free ofsparks and flames.8. Bulk Sampling8.1 Samples from shipments shall be take
10、n in accordancewith Practice D4296, 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 contains freewater, air-dry a representati
11、ve 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 overheat, and remove heat source immediately when
12、 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 May 1, 2010. Published May 2010. Originallyap
13、proved in 1983. Last previous edition approved in 2005 as D431295a (2005).DOI: 10.1520/D4312-95R10.2For 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 to the standards Doc
14、ument 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 D370, but stop thedistillation when the tempe
15、rature 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 representative portion of
16、 the bulk sampleat atmospheric pressure using a simple side-arm distillationapparatus similar to the one in Test Method D850 and stop thedistillation when the temperature reaches 170C. Separate anyoil from the water that has distilled over (if crystals are present,warm sufficiently to ensure their s
17、olution) 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 D95 and, if the watercontent is less than 10 mass %, the TI content is corrected
18、 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 (60-mesh) screen but so
19、 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 working sample in a tigh
20、tly 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 ofvolatile matter. Do not
21、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 removeforeign matter.
22、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 the mass.11.1.1 After
23、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 hydrochloricacid (1 + 1) to
24、 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 stirring sample with a
25、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 sample is digesting, weigh
26、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.Avoid fillingthe thimble h
27、igher 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 extraction apparatus
28、asdescribed in Test Method D4072. 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 level of liquid in the thi
29、mble. 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 thimble is placed into b
30、asket.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 ApparatusD4312 95a (2010)2filling
31、 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-insolubles, andC = mass
32、 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) content to the nearest0.1
33、 %.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 determinedpercentages differ by more
34、 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 determinethe precision o
35、f this test method, the TI was also determined byTest Method D4072 (long method). It was found that the TIdetermined by Test Method D4312 was higher than thatdetermined by Test Method D4072 by an average value ofabout 1 percentage point.16. Keywords16.1 beta resin; pitch; soft pitch; tar; toluene in
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