1、Designation: D2318 141Standard 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 last revision. A
2、 number in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.1NOTEEditorial changes were made throughout the test method in September 2014.1. Scope*1.1 This test method covers the determination of thequinoli
3、ne-insoluble matter (QI) 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. No other units of measurement are included in thisstandard.1.4 This standard does not purpo
4、rt to address all of thesafety concerns, if any, associated with 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. Refer
5、enced Documents2.1 ASTM Standards:2D71 Test Method for Relative 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)3
6、D850 Test Method for Distillation of Industrial AromaticHydrocarbons 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
7、quinoline and filtered. Theinsoluble material is washed, dried, 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,
8、porcelain, with fine-porositybottom, 25 mL to 40 mL capacity, high-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, maintaine
9、d at 75 C 65 C.6. Reagents and Materials6.1 Quinoline, Refined, meeting the following requirements:6.1.1 The quinoline shall distill from 5 % to 95 % within arange of 2 C that shall include the temperature of 237.4 Cafter corrections for barometric pressure and emergent stemhave been applied. The di
10、stillation shall be carried out inaccordance with Test Method D850 using a total immersionthermometer with a range from 195 C to 305 C, graduated in0.5 C, and conforming to the requirements for Thermometer69C as described in Specification E1. Temperature measuringdevices such as precision thermocoup
11、les, resistance tempera-ture detectors (RTDs), and liquid-in-glass thermometers withequal or better accuracies in the appropriate temperature rangemay be used.6.1.2 The quinoline shall have a specific gravity at 15.5/15.5 C of 1.092 to 1.098, as determined by Test Method D71,or other method of equiv
12、alent 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 next1This test method is under the jurisdiction of
13、 ASTM Committee D02 onPetroleum Products, Liquid Fuels, and Lubricantsand is the direct responsibility ofSubcommittee D02.05 on Properties of Fuels, Petroleum Coke and Carbon Material.Current edition approved May 1, 2014. Published May 2014. Originallyapproved in 1964. Last previous edition approved
14、 in 2013 as D2318 98 (2013).DOI: 10.1520/D2318-14E01.2For 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 las
15、t approved version of this historical standard is referenced onwww.astm.org.*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. United States190 %. If the quinoline contains suspended mat
16、ter 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 D362.6.3 Acetone, meeting Specification D329.6.4 C
17、oncentrated Hydrochloric Acid.6.5 Celite Analytical Filter Aid (CAFA)Dry to constantweight at 105 C, 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
18、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 contact with the skin should beavoided. Toluene is toxic and fla
19、mmable.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 D4296 and shall be free of foreign substances.Thoroughly mix the sample immediately before removing arepresentative portio
20、n 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 at50 C.9.2 Soft PitchIf the presence of water is indicated bysurface foam on heating, maintain a representative portio
21、n ofthe bulk sample at a temperature between 125 C and 150 C inan open container until the surface is free of foam. Take carenot to overheat, and remove heat source immediately whenfoam subsides.9.3 TarAwet tar sample may either be dehydrated or usedas received as long as conditions stated in 9.3.1
22、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 D850 and stop thedistillation when the temperature reaches 170 C. Separate anyoil from the water that has distilled over
23、 (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 ofthe tar is determined by Test Method D95, and if the wat
24、ercontent is less than 10 mass percent, the QI content is correctedto a dry-tar basis (see 13.2). This alternative test methodapplies only 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 Sa
25、mple10.1 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 mullite mortar and pestle. No particle in therepresentativ
26、e 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 (see 10.4).10.2 Soft PitchIf the pitch is too soft to g
27、rind 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 melting period.Pass the heated sample through the 600 m s
28、ieve 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 SamplesStore samples as largelumps or as solidified melts i
29、n 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 six determinations, clean it as follows:Remove the ma
30、t, wash the crucible with distilled water, dry,and ignite in a muffle furnace for1hatabout 800 C. 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 si
31、x 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 with distilledwater, dry, and ignite as in 11.1.12. Pro
32、cedure12.1 Make and record all weighings to the nearest 1 mg.12.2 Select a sample mass that will yield between 75 mgand 150 mg of matter insoluble in quinoline (QI), unless thiswould require less than the minimum acceptable sample massof 0.5 g, in which case 0.5 g shall be used.12.3 Transfer 1 g 6 0
33、.1 g of dry CAFA to a clean, dry,filtering crucible. Weigh immediately, and record the mass ofcrucible plus CAFA.D2318 141212.4 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 beakerwi
34、th 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 and a wash bottle containing quinoli
35、ne on an electrichot plate or in a water bath maintained at 75 C 6 5 C. (Asuitable weight can be used to keep the beaker from beingupset in the water bath.) Digest for at least 20 min. Occasion-ally stir the contents of the beaker to promote digestion. Checkfor completeness of digestion by inspectin
36、g the bottom of thebeaker for undigested pitch.12.6 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 thoroughly. Apply suction and form a mat of evenlydistri
37、buted 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 mixture in the beaker immediately beforepouring successi
38、ve 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 mL to 3 mL each) of quinolineat 75 C 6 5 C from the
39、wash bottle. Pass all the washesthrough the filter. Allow each wash to pass almost completelythrough the filter before the next is added. Use a suitablepoliceman to sweep the insoluble particles into the crucible.Repeat the quinoline washes until the filtrate is the same coloras the quinoline used f
40、or 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 of75 mL to 100 mL of toluene using suction.After all the toluenehas passed through the filter, wash the contents of the cruciblein the
41、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 CAFA mat to get completely dry as the filtra
42、tion ratemay decrease considerably.12.10 Place the filtering crucible in the drying oven at105 C to 110 C and dry to constant weight (61 mg). Whenthe hot crucible is removed from the drying oven it shall haveno odor of quinoline. Transfer the crucible to the desiccator andcool for 25 min, then weigh
43、 and record the weight of thefiltering crucible 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 the entire determination.12.11 If the m
44、ass 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# 3100 (1)where:A = total mass of the filtering crucible and
45、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 determined in 13.1 to a dry-tar basisas f
46、ollows:QI, mass % dry basis!5 (2)QI, mass % wet basis!100 2 water content of tar, mass%!310014. 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 RepeatabilityDuplica
47、te 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 of twolaboratories, representing the ar
48、ithmetic 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 because the valueof quinoline-insouble
49、is defined in terms of this test method.16. Keywords16.1 coal-tar insolubles; pitch; QI; quinoline insolubles; tarD2318 1413SUMMARY OF CHANGESSubcommittee D02.05 has identified the location of selected changes to this standard since the last issue(D2318 98 (2013) that may impact the use of this standard. (Approved May 1, 2014.)(1) Revised subsection 6.1.1.ASTM 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 exp
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