1、Designation: D2318 98 (Reapproved 2013)Standard Test Method forQuinoline-Insoluble (QI) Content of Tar and Pitch1This standard is issued under the fixed designation D2318; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of
2、 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 thequinoline-insoluble matter (QI) in tar and pitch.1.2 Since this test
3、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. No other units of measurement are included in thisstandard.1.4 This standard does not purport to address all of thesafety concerns, if any, associated wi
4、th 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 hazardsinformation, see Section 7.2. Referenced Documents2.1 ASTM Standards:2D71 Test Method for Relativ
5、e Density of Solid Pitch andAsphalt (Displacement Method)D95 Test Method for Water in Petroleum Products andBituminous Materials by DistillationD329 Specification for AcetoneD362 Specification for Industrial Grade Toluene (Withdrawn1989)3D850 Test Method for Distillation of Industrial AromaticHydroc
6、arbons and Related MaterialsD4296 Practice for Sampling PitchE1 Specification for ASTM Liquid-in-Glass ThermometersE11 Specification for Woven Wire Test Sieve Cloth and TestSieves3. Summary of Test Method3.1 The sample is digested in hot quinoline and filtered. Theinsoluble material is washed, dried
7、, and weighed.4. Significance and Use4.1 This test method is useful in evaluating 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-porositybottom, 25 to 40-mL capacity, hig
8、h-form, maximum porediameter, 7 m.5.2 Filter ApparatusFilter flask and tube 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, meet
9、ing the following requirements:6.1.1 The quinoline shall distill from 5 to 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 D850 using
10、 a total immersion thermometerwith a range from 195 to 305C, graduated in 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
11、 equivalent accuracy.6.1.3 The quinoline shall be clear and light in color and shallcontain less than 0.5 volume % of water as determined by TestMethod D95. If not, redistill the quinoline in all-glassapparatus, discarding the first 5 % and collecting the next90 %. If the quinoline contains suspende
12、d matter but is clear,light in color, and contains less than 0.5 % water, filter thequinoline through a crucible containing5gofCelite FilterAid.6.1.4 Store the quinoline in a tightly closed, dark bottle.6.2 Toluene, Industrial Pure, meeting Specification D362.1This test method is under the jurisdict
13、ion of ASTM Committee D02 onPetroleum Products and Lubricantsand is the direct responsibility of SubcommitteeD02.05 on Properties of Fuels, Petroleum Coke and Carbon Material.Current edition approved July 15, 2013. Published August 2013. Originallyapproved in 1964. Last previous edition approved in
14、2008 as D2318 98 (2008).DOI: 10.1520/D2318-98R13.2For 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.3The last ap
15、proved version of this historical standard is referenced onwww.astm.org.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States16.3 Acetone, meeting Specification D329.6.4 Concentrated Hydrochloric Acid.6.5 Celite Analytical Filter Aid (CAFA)
16、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 is manufacturedonly by Manville Co. and distributed through scientific supplyhouses.7. Hazards7.1 Fumes of the solvents should be
17、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 contact with the skin should beavoided. Toluene is toxic and flammable.7.2 Observe proper laboratory procedures for handling hy-drochl
18、oric and diluting acid.8. Bulk Sampling8.1 Samples from shipments shall be taken 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
19、 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 portion ofthe bulk sample at a temperature between 125 and 150C in anopen con
20、tainer until the surface is free of foam. Take care notto overheat, and remove heat source immediately when foamsubsides.9.3 TarA wet tar sample may either be dehydrated 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 sam
21、pleat 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 solution) and
22、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 QI content is corrected toa dry-tar
23、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 24 h atroom temperature.10. Preparation of Working Sample10.1 Hard PitchIf the pitch can be crushed at roomtemperature, prepare a 20-
24、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 be larger than 5 mm in anydimension. Crush this sample so that al
25、l 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 (see 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
26、 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 melting period.Pass the heated sample through the 600-m sieve to removeforeign matter.10.3 TarHeat a representative portion of the dry ta
27、r 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 SamplesStore samples as largelumps or as solidified melts in closed containers. Discardworking samples 24 h after crushing and sieving as c
28、hanges incomposition sometimes occur in pulverized pitch.11. Crucible Preparations11.1 If the crucible, after thorough cleaning (see 11.2), hasbeen used for less than six determinations, clean it as follows:Remove the mat, wash the crucible with distilled water, dry,and ignite in a muffle furnace fo
29、r1hatabout 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 still warm.11.2 After the crucible has been used for six determinations,remove any residual ash from pores in the filtering area byboili
30、ng in 1 + 1 hydrochloric acid. Add equal volume ofconcentrated hydrochloric acid to distilled water. Then boil thecrucible in distilled water, thoroughly back wash with 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
31、 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 which 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
32、 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 CAFAfrom the crucible to the beakerwith sample. Distribute the remaining CAFA evenly over thebottom of the crucible.12.5 Add 25 mL of
33、 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 theD2318 98 (2013)2beaker and a wash bottle containing quinoline on an electrichot plate or in a water bath maintained at 75 6 5C. (Asuitablew
34、eight 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-pleteness of digestion by inspecting the bottom of the beakerfor undigested pitch.12.6 Insert the filter tube with adap
35、ter in the filter flask, andplace the previously prepared and tared crucible in the adapter.Carefully add sufficient quinoline to the crucible to wet theCelite thoroughly. Apply suction and form a mat of evenlydistributed Celite. Maintain suction until filtration and subse-quent washing with quinoli
36、ne 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 mixture in the beaker immediately beforepouring successive portions into the crucible. Allow the con-tents to drain completely, but not to t
37、he 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 3 mL each) of quinoline at 756 5C from the wash bottle. Pass all the washes through thefilter. Allow each wash to pass almost complet
38、ely through thefilter before the next is added. Use a suitable policeman tosweep the insoluble particles into the crucible. Repeat thequinoline washes until the filtrate is the same color as thequinoline used for washing. Twelve washings are usuallyenough.12.9 After the final quinoline wash has pass
39、ed 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, wash the contents of the crucible inthe same manner with acetone. Maintain full suction for aminimum of 5 min after the acetone wash
40、. 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 CAFA mat to get completely dry as the filtration ratemay decrease considerably.12.10 Place the filtering crucible in the drying oven at
41、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 desiccator and coolfor 25 min, then weigh and record the weight of the filteringcrucible and its contents (see 12.1).12.10.1 Insoluble m
42、atter on the filter, after washing withacetone, should have no odor of quinoline, which is evidenceof insufficient washing. If odor of quinoline is detectable,repeat the entire determination.12.11 If the mass of matter insoluble in quinoline is lessthan 75 mg or more than 150 mg, repeat the determin
43、ation 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# 3100 (1)where:A = total mass of the filtering crucible and CAFA added tothe crucible, and matter insoluble in quinoline,B = initial mass of the filtering
44、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 determined in 13.1 to a dry-tar basisas follows:QI, mass % dry basis!5 (2)QI, mass % wet basis!100 2 water content of tar, mass%!310014.
45、 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 % probability):15.1.1 RepeatabilityDuplicate values by the same opera-tor shall not be considered suspect unless the determinedpercentage
46、s 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 of twolaboratories, representing the arithmetic average of duplicatedeterminations, shall not be considered suspect unless thereported
47、 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 because the valueof quinoline-insouble is defined in terms of this test method.16. Keywords16.1 coal-tar insolubles; pitch; QI; quinol
48、ine insolubles; tarD2318 98 (2013)3ASTM 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
49、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 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 commen
