1、Designation: D 2318 98 (Reapproved 2003)An American National StandardStandard Test Method forQuinoline-Insoluble (QI) Content of Tar and Pitch1This standard is issued under the fixed designation D 2318; 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.1. Scope1.1 This test method covers the determination of thequinoline-insoluble matter (QI) in ta
3、r 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 address all of thesafety concerns, if any, associated with its use. It is theres
4、ponsibility 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. See Section 7.2. Referenced Documents2.1 ASTM Standards:2D71 Test Method for Relative Density of Solid Pitch andAsphalt (Displacemen
5、t Method)D95 Test Method for Water in Petroleum Products andBituminous Materials by DistillationD 329 Specification for AcetoneD 362 Specification for Industrial Grade Toluene3D 850 Test Method for Distillation of Industrial AromaticHydrocarbons and Related MaterialsD 4296 Practice for Sampling Pitc
6、hE1 Specification for ASTM ThermometersE11 Specification for Wire Cloth and Sieves for TestingPurposes3. Summary of Test Method3.1 The sample is digested in hot quinoline and filtered. Theinsoluble material is washed, dried, and weighed.4. Significance and Use4.1 This test method is useful in evalua
7、ting and character-izing tar and pitch, and as one element in establishing theuniformity of shipments and sources of supply.5. Apparatus5.1 Filtering Crucibles, porcelain, with fine-porosity bot-tom, 25 to 40-mL capacity, high-form, maximum pore diam-eter, 7 m.5.2 Filter ApparatusFilter flask and tu
8、be with crucibleadapter.5.3 SievesU. S. Standard 600-m (No. 30) and 250-m(No. 60), conforming to Specification E11.5.4 Electric Hot Plate or Water Bath, maintained at 75 65C.6. Reagents and Materials6.1 Quinoline, Refined, meeting the following requirements:6.1.1 The quinoline shall distill from 5 t
9、o 95 % within arange of 2C that shall include the temperature of 237.4C aftercorrections for barometric pressure and emergent stem havebeen applied. The distillation shall be carried out in accordancewith Test Method D 850 using a total immersion thermometerwith a range from 195 to 305C, graduated i
10、n 0.5C, andconforming to the requirements for Thermometer 69C asdescribed in Specification E1.6.1.2 The quinoline shall have a specific gravity at 15.5/15.5C of 1.092 to 1.098, as determined by Test Method D71,or other method of equivalent accuracy.6.1.3 The quinoline shall be clear and light in col
11、or and shallcontain less than 0.5 volume % of water as determined by TestMethod D95. If not, redistill the quinoline in all-glass appa-ratus, discarding the first 5 % and collecting the next 90 %. Ifthe quinoline contains suspended matter but is clear, light incolor, and contains less than 0.5 % wat
12、er, filter the quinolinethrough a crucible containing5gofCelite Filter Aid.6.1.4 Store the quinoline in a tightly closed, dark bottle.6.2 Toluene, Industrial Pure, meeting Specification D 362.6.3 Acetone, meeting Specification D 329.6.4 Concentrated Hydrochloric Acid.1This test method is under the j
13、urisdiction 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 Nov. 1, 2003. Published November 2003. Originallyapproved in 1964. Last previous edition ap
14、proved in 1998 as D 231898.2For 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 Document Summary page onthe ASTM website.3Withdrawn.1Copyright ASTM Interna
15、tional, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.6.5 Celite Analytical Filter Aid (CAFA)Dry to constantweight at 105C, and store in tightly stoppered container.6.5.1 Do not use any other grade of filter aid becausefiltration characteristics may differ. CAFA
16、 is manufacturedonly by Manville Co. and distributed through scientific supplyhouses.7. Hazards7.1 Fumes of the solvents should be removed by means ofproper hoods from all working areas. The working area shouldbe kept free of sparks and flames. Quinoline fumes should notbe inhaled, and prolonged con
17、tact with the skin should beavoided. Toluene is toxic and flammable.7.2 Observe proper laboratory procedures for handling hy-drochloric and diluting 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
18、 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 representative portion in a forced draft oven at50C.9.2 Soft PitchIf the presence of water is indicate
19、d bysurface foam on heating, maintain a representative portion ofthe bulk sample at 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.9.3 TarAwet tar sample may either be dehydrated
20、 or usedas received as long as conditions stated in 9.3.1 and 9.3.2 aremet.9.3.1 Dehydrate a representative 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 17
21、0C. Separate anyoil from the water that has distilled over (if crystals are present,warm sufficiently 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
22、ofthe tar is determined by Test Method D 95, and if the watercontent is less than 10 mass %, the QI content is corrected toa dry-tar basis (see 13.2). This alternative test method appliesonly to stable emulsions of water in tar, that is, no waterseparates when the tar sample is left undisturbed for
23、24 h atroom temperature.10. Preparation of Working Sample10.1 Hard PitchIf 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 mulli
24、te mortar and pestle. No particle in therepresentative sample shall be larger than 5 mm in anydimension. Crush this sample so that all of it will pass the250-m (No. 60) sieve but will have a minimum of fineparticles. Store the sieved working sample in a tightly closedcontainer and use within 24 h (s
25、ee 10.4).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 through the600-m (No. 30) sieve, taking care to avoid excessive loss ofvolatile matter. Do not exceed 10 min for this melt
26、ing 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.10.4 Preservation of Sample
27、sStore samples as largelumps or as solidified melts in closed containers. Discardworking samples 24 h after crushing and sieving as changes incomposition sometimes occur in pulverized pitch.11. Crucible Preparations11.1 If the crucible, after thorough cleaning (see 11.2), hasbeen used for less than
28、six determinations, clean it as follows:Remove the mat, wash the crucible with distilled water, dry,and ignite in a muffle furnace for1hatabout 800C. Cool thecrucible slowly by placing it in a drying oven for 1 h afterremoval from the furnace to prevent cracking and place it in adesiccator while sti
29、ll warm.11.2 After the crucible has been used for six determinations,remove any residual ash from pores in the filtering area byboiling in 1 + 1 hydrochloric acid. Add equal volume ofconcentrated hydrochloric acid to distilled water. Then boil thecrucible in distilled water, thoroughly back wash wit
30、h distilledwater, dry, and ignite as in 11.1.12. Procedure12.1 Make and record all weighings to the nearest 1 mg.12.2 Select a sample mass that will yield between 75 and150 mg of matter insoluble in quinoline (QI), unless this wouldrequire less than the minimum acceptable sample mass of 0.5g, in whi
31、ch case 0.5 g shall be used.12.3 Transfer 1 6 0.1 g of dry CAFA to a clean, dry,filtering crucible. Weigh immediately, and record the mass ofcrucible plus CAFA.12.4 Place the required amount of sample in a tared beakerand weigh. Calculate and record the mass of the sample.Transfer about half of the
32、CAFAfrom the crucible to the beakerwith sample. Distribute the remaining CAFA evenly over thebottom of the crucible.12.5 Add 25 mL of quinoline to the beaker while stirring themixture with a stirring rod or thermometer to break up lumps,then cover the beaker with a small watch glass. Place thebeaker
33、 and a wash bottle containing quinoline on an electrichot plate or in a water bath maintained at 75 6 5C. (Asuitableweight can be used to keep the beaker from being upset in thewater bath.) Digest for at least 20 min. Occasionally stir thecontents of the beaker to promote digestion. Check for com-pl
34、eteness of digestion by inspecting the bottom of the beakerfor undigested pitch.D 2318 98 (2003)212.6 Insert the filter tube with adapter in the filter flask, andplace the previously prepared and tared crucible in the adapter.Carefully add sufficient quinoline to the crucible to wet theCelite thorou
35、ghly. Apply suction and form a mat of evenlydistributed Celite. Maintain suction until filtration and subse-quent washing with quinoline are completed.12.7 Pour the hot quinoline-pitch mixture into the crucible,while the Celite in the crucible is still wet, without disturbingthe mat. Stir the mixtur
36、e in the beaker immediately beforepouring successive portions into the crucible. Allow the con-tents to drain completely, but not to the extent that the insolublematerial on the filter appears substantially dry.12.8 Wash the beaker, thermometer, or stirring rod, andcrucible with small portions (2 to
37、 3 mL each) of quinoline at 756 5C from the wash bottle. Pass all the washes through thefilter. Allow each wash to pass almost completely through thefilter before the next is added. Use a suitable policeman tosweep the insoluble particles into the crucible. Repeat thequinoline washes until the filtr
38、ate is the same color as thequinoline used for washing. Twelve washings are usuallyenough.12.9 After the final quinoline wash has passed through thefilter, fill the crucible with toluene and wash with a total of 75to 100 mL of toluene using suction. After all the toluene haspassed through the filter
39、, wash the contents of the crucible inthe same manner with acetone. Maintain full suction for aminimum of 5 min after the acetone wash. Remove thecrucible, and wipe the outside with a clean, soft cloth or tissuemoistened with acetone.12.9.1 During the quinoline and toluene washing do notallow the CA
40、FA mat to get completely dry as the filtration ratemay decrease considerably.12.10 Place the filtering crucible in the drying oven at 105to 110C and dry to constant weight (61 mg). When the hotcrucible is removed from the drying oven it shall have no odorof quinoline. Transfer the crucible to the de
41、siccator and coolfor 25 min, then weigh and record the weight of the filteringcrucible and its contents (see 12.1).12.10.1 Insoluble matter on the filter, after washing withacetone, should have no odor of quinoline, which is evidenceof insufficient washing. If odor of quinoline is detectable,repeat
42、the entire determination.12.11 If the mass of matter insoluble in quinoline is lessthan 75 mg or more than 150 mg, repeat the determination withan adjusted sample mass of not less than 0.5 g (see 12.2).13. Calculation13.1 Calculate the QI content as follows:QI, mass % 5 A 2 B!/C 3 100(1)where:A = to
43、tal mass of the filtering crucible and CAFA added tothe crucible, and matter insoluble in quinoline,B = initial mass of the filtering crucible containing driedCAFA, andC = mass of sample taken for the determination.13.2 If the QI was determined on a wet tar sample (see9.3.2), correct the QI value de
44、termined in 13.1 to a dry-tar basisas follows:QI, mass % dry basis!5QI, mass % wet basis!100 2 water content of tar, mass %!3 100(2)14. Report14.1 Report the QI content to the nearest 0.1 %.15. Precision and Bias15.1 The following criteria shall be used for judging theacceptability of results (95 %
45、probability):15.1.1 RepeatabilityDuplicate values by the same opera-tor shall not be considered suspect unless the determinedpercentages differ by more than 0.2 when the QI content is 4 %or less, or by more than 0.3 when the QI content is more than4%.15.1.2 ReproducibilityThe values reported by each
46、 of twolaboratories, representing the arithmetic average of duplicatedeterminations, shall not be considered suspect unless thereported percentages differ by more than 0.3 when the QIcontent is 4 % or less, or by more than 0.6 when the QI contentis more than 4 %.15.2 BiasThis test method has no bias
47、 because the valueof quinoline-insouble is defined in terms of this test method.16. Keywords16.1 coal-tar insolubles; pitch; QI; quinoline insolubles; tarASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentionedin this standard.
48、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.This standard is subject to revision at any time by the responsible technical committee and must be reviewed ev
49、ery 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 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 shown below.This standard is copyrighted by ASTM International, 1
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