1、Designation: D4312 95a (Reapproved 2010)D4312 15Standard 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
2、revision, 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. Scope Scope*1.1 This test method covers the determination of toluene-insoluble matter (TI) in tar and pit
3、ch.1.2 Since this test method is empirical, strict adherence to all details of the procedure is necessary.1.3 The values stated in SI units are to be regarded as standard.1.3.1 ExceptionOther non-SI units are provided for information only.1.4 This standard does not purport to address all of the safe
4、ty concerns, if any, associated with its use. It is the responsibilityof the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatorylimitations prior to use. Specific hazard statements are given in Section 7.2. Referenced Documents2.1
5、ASTM Standards:2D95 Test Method for Water in Petroleum Products and Bituminous Materials by DistillationD329 Specification for AcetoneD362 Specification for Industrial Grade Toluene (Withdrawn 1989)3D370 Practice for Dehydration of Oil-Type PreservativesD850 Test Method for Distillation of Industria
6、l Aromatic Hydrocarbons and Related MaterialsD4072 Test Method for Toluene-Insoluble (TI) Content of Tar and PitchD4296 Practice for Sampling PitchE11 Specification for Woven Wire Test Sieve Cloth and Test Sieves3. Summary of Test Method3.1 The sample is digested, then extracted with hot toluene in
7、an alundum thimble. The insoluble matter is dried and weighed.4. Significance and Use4.1 This test method is useful for evaluating and characterizing tars and pitches and is one element in establishing the uniformityof shipment or sources of supply.5. Apparatus5.1 Extraction Apparatus, flask with me
8、tal cap condenser as shown in Fig. 1.5.2 Extraction Thimbles, Alundum AN 485 coarse (formerly RA 98), 30 mm in diameter by 80 mm in height with flat bottom.5.3 Sieves, U.S. Standard 600-mStandard 600 m (No. 30) and 250-m250 m (No. 60), conforming to Specification E11.5.4 Heater, having a minimum cap
9、acity of 300 W per unit. A hot plate or other heaters that maintain the proper reflux rate areacceptable.1 This test method is under the jurisdiction ofASTM Committee D02 on Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of SubcommitteeD02.05 on Properties of Fuels
10、, Petroleum Coke and Carbon Material.Current edition approved May 1, 2010Dec. 1, 2015. Published May 2010December 2015. Originally approved in 1983. Last previous edition approved in 20052010 asD4312D4312 95a (2010).95a (2005). DOI: 10.1520/D4312-95R10.10.1520/D4312-15.2 For referencedASTM standards
11、, visit theASTM website, www.astm.org, or contactASTM Customer Service at serviceastm.org. For Annual Book of ASTM Standardsvolume information, refer to the standards Document Summary page on the ASTM website.3 The last approved version of this historical standard is referenced on www.astm.org.This
12、document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Becauseit may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions
13、 as appropriate. In all cases only the current versionof the standard as published by ASTM is to be considered the official document.*A Summary of Changes section appears at the end of this standardCopyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. Un
14、ited States16. Reagents6.1 Toluene, Industrial Pure, meeting Specification D362.6.2 Acetone, meeting the requirements of Specification D329.7. Hazards7.1 Since toluene is a toxic and flammable substance, all working areas should be efficiently hooded and kept free of sparks andflames.8. Bulk Samplin
15、g8.1 Samples from shipments shall be taken in accordance with Practice D4296, and shall be free of foreign substances.Thoroughly mix the sample immediately before removing a representative portion for the determination or for dehydration.9. Dehydration of Sample9.1 Hard PitchIf the solid bulk sample
16、 contains free water, air-dry a representative portion.9.2 Soft PitchIf the presence of water is indicated by surface foam on heating, maintain a representative portion of the bulksample of a temperature between 125125 C and 150C150 C in an open container until the surface is free of foam. Take care
17、not to overheat, and remove heat source immediately when foam subsides.9.3 TarDehydrate a representative portion of the bulk sample in accordance with at atmospheric pressure using a simpleside-arm distillation apparatus similar to the one in Test Method D370D850, but and stop the distillation when
18、the temperaturereaches 170C.170 C. Separate any oil from the water that has distilled over. (Ifover (if crystals are present, warm sufficiently toensure their solution). Thoroughly solution) and thoroughly mix the oil with the residual tar in the still after the latter has cooledto a moderate temper
19、ature.9.3.1 Dehydrate a representative portion of the bulk sample at atmospheric pressure using a simple side-arm distillationapparatus similar to the one in Test Method D850 and stop the distillation when the temperature reaches 170C. Separate any oilfrom the water that has distilled over (if cryst
20、als are present, warm sufficiently to ensure their solution) and thoroughly mix theoil with the residual tar in the still after the latter has cooled to a moderate temperature.9.3.1 As an alternative to dehydration, the water content of the tar is determined by Test Method D95 and, if the water cont
21、entis less than 10 mass %,10 % by mass, the TI content is corrected to a dry-tar basis (see 13.2). This alternative method applies onlyto stable emulsions of water in tar, that is, no water separates when the tar sample is left undisturbed for 24 h 24 h at roomtemperature.10. Preparation of Working
22、Sample10.1 Hard PitchCrush samples to pass a 250-m (60-mesh)250 m (60 mesh) screen but so they are retained on a 150 m(100-mesh) 150 m (100 mesh) screen. Remove pitch from 150-m (100-mesh)150 m (100 mesh) screen by a brush. Crushingcan be done with a small jaw crusher or a mortar and pestle, or both
23、. No particle in the representative sample should be larger than5 mm 5 mm in any dimension. Store sieved working sample in a tightly closed container and use within 24 h.24 h.10.2 Soft PitchIf the pitch is too soft to grind and too sticky to mix, heat a representative portion of the dry sample to th
24、elowest temperature that will permit passage through 600-m600 m (No. 30) sieve, taking care to avoid excessive loss of volatilematter. Do not exceed 10 min for this melting period. Pass the heated sample through the 600-m600 m sieve to remove foreignmatter.FIG. 1 Extraction ApparatusD4312 15210.3 Ta
25、rHeat a representative portion of the dry tar to the lowest temperature that will permit passage through the600-m600 m (No. 30) sieve, then filter through this sieve to remove foreign matter.10.4 Discard working sample 24 h after crushing and sieving as changes in composition sometimes occur in pulv
26、erized pitch.11. Preparation of Alundum Thimble11.1 Dry the clean thimble in an oven at 105105 C 6 5C5 C for 45 min, cool in a desiccator, and weigh to the nearest 0.5mg. Record the mass.11.1.1 After each use, ignite the thimble at 700700 C to 800C800 C for a few hours. Cool the thimble slowly by pl
27、acing ina drying oven for 1 h 1 h after removal from the furnace to prevent cracking. Before reuse, condition the thimble as described in11.1.11.1.2 After repeated use, boil the thimble in hydrochloric acid (1 + 1) to remove residual ash from the pores. Then boil thethimble in distilled water and wa
28、sh with water.After drying at 105C,105 C, ignite and condition the thimble as described in 11.1and 11.1.1.12. Procedure12.1 Weigh 0.50 g 0.50 g sample to the nearest 0.5 mg 0.5 mg in a 150 mL 150 mL tared beaker.12.2 While stirring sample with a glass rod, add 75 mL 75 mL of hot toluene (95(95 C 6 5
29、C)5 C) and continue stirring fora few minutes until the sample is dispersed. Digest sample containing toluene on an appropriate heat source (preferably a hot wateror steam bath) at 9595 C 6 5C5 C for 25 min 25 min with occasional stirring.12.3 While sample is digesting, weigh the alundum thimble, AN
30、 485 (formerly RA 98, 20-m20 m porosity, 3030 mm by80-mm80 mm size) to nearest 0.5 mg. 0.5 mg. Place the thimble in a filtering tube, which is supported on a funnel rack orequivalent apparatus to drain soluble portion of sample.12.4 Pour the digested sample into the thimble. Avoid filling the thimbl
31、e higher than 20 mm 20 mm from the top. Use a glassrod, a brush, or a rubber policeman, if necessary, and cold toluene from a wash bottle to completely transfer the insoluble particlesinto the thimble.12.5 When most of the solution has drained from the thimble, transfer the thimble to the extraction
32、 apparatus as described inTest Method D4072. With a beaker, add hot toluene to extraction flask. Fill to a level approximately 25 mm 25 mm below thebottom of thimble.12.6 Adjust the hot plate, and set the drip (reflux) rate of toluene at 120120 dropsmin to 150 drops/min from the condenserto maintain
33、 the level of liquid in the thimble. Continue extraction for 3 h. The liquid level is easily observed if the paper cone isreplaced with 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
34、on before thimble is placed into basket.12.7 Cut heat off, let drain, remove with tongs, and place thimble in filtering tube. Wash the inside and outside of thimble withacetone several times from a wash bottle, starting from top of thimble (several small washes are more efficient than filling thethi
35、mble). Place thimble in an oven at 110110 C 6 5C5 C for 30 min. Cool in a desiccator and weigh.13. Calculation13.1 Calculate the toluene-insoluble (TI) content as follows:TI,mass%5100B 2A!/C (1)where:A = mass of the alundum thimble,B = mass of alundum thimble plus toluene-insolubles, andC = mass of
36、sample.13.2 If the TI was determined on a wet tar sample (see 9.3.29.3.1), correct the TI value determined in 13.1 to a dry-tar basisas follows:TI mass %dry basis!5 TI mass %wet basis!1002water content of tar,mass %!3100 (2)14. Report14.1 Report the toluene-insoluble (TI) content to the nearest 0.1
37、%.15. Precision and Bias15.1 Based upon present available data, the following criteria shall be used for judging the acceptability of results (95 %probability):D4312 15315.1.1 RepeatabilityDuplicate values by the same operator shall not be considered suspect unless the determined percentagesdiffer b
38、y more than 1.0.15.1.2 ReproducibilityThe values reported by each of two laboratories, representing the arithmetic average of duplicatedeterminations, shall not be considered suspect unless the reported percentages differ by more than 3.0.15.2 BiasDuring the interlaboratory study to determine the pr
39、ecision of this test method, the TI was also determined by TestMethod D4072 (long method). It was found that the TI determined by Test Method D4312 was higher than that determined by TestMethod D4072 by an average value of about 1 percentage point.16. Keywords16.1 beta resin; pitch; soft pitch; tar;
40、 toluene insolublesSUMMARY OF CHANGESSubcommittee D02.05 has identified the location of selected changes to this standard since the last issue(D4312 95a (2010) that may impact the use of this standard. (Approved Dec. 1, 2015.)(1) Deleted D370 from Referenced Documents.(2) Revised subsection 9.3.ASTM
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