1、Designation: D2318 141D2318 15Standard 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 rev
2、ision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.1 NOTEEditorial changes were made throughout the test method in September 2014.1. Scope*1.1 This test method covers the determination of t
3、he quinoline-insoluble matter (QI) in tar and pitch.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. No other units of measurement are included in this standard.1.4 This standard d
4、oes not purport to address all of the safety 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. For hazards information, see Sectio
5、n 7.2. Referenced Documents2.1 ASTM Standards:2D71 Test Method for Relative Density of Solid Pitch and Asphalt (Displacement Method)D95 Test Method for Water in Petroleum Products and Bituminous Materials by DistillationD329 Specification for AcetoneD362 Specification for Industrial Grade Toluene (W
6、ithdrawn 1989)3D850 Test Method for Distillation of Industrial Aromatic Hydrocarbons and Related MaterialsD4296 Practice for Sampling PitchD7280 Test Method for Quinoline-Insoluble (QI) Content of Tar and Pitch by Stainless Steel Crucible FiltrationE1 Specification for ASTM Liquid-in-Glass Thermomet
7、ersE11 Specification for Woven Wire Test Sieve Cloth and Test Sieves3. Summary of Test Method3.1 The sample is digested in hot quinoline and filtered. The insoluble material is washed, dried, and weighed.4. Significance and Use4.1 This test method is useful in evaluating and characterizing tar and p
8、itch, and as one element in establishing the uniformityof shipments and sources of supply.5. Apparatus5.1 Filtering Crucibles, porcelain, with fine-porosity bottom, 25 mL to 40 mL capacity, high-form, maximum pore diameter, 7m.5.2 Filter ApparatusFilter flask and tube with crucible adapter.5.3 Sieve
9、sU. 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 C 6 5 C.1 This test method is under the jurisdiction ofASTM Committee D02 on Petroleum Products, Liquid Fuels, and Lubricantsand is the direct responsibility of S
10、ubcommitteeD02.05 on Properties of Fuels, Petroleum Coke and Carbon Material.Current edition approved May 1, 2014Dec. 1, 2015. Published May 2014December 2015. Originally approved in 1964. Last previous edition approved in 20132014 asD2318 98 (2013).D2318 141. DOI: 10.1520/D2318-14E01.10.1520/D2318-
11、15.2 For referencedASTM standards, 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
12、 referenced on www.astm.org.This 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
13、that users consult prior editions 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, Wes
14、t Conshohocken, PA 19428-2959. United States16. Reagents and Materials6.1 Quinoline, Refined, meeting the following requirements:6.1.1 The quinoline shall distill from 5 % to 95 % within a range of 2 C that shall include the temperature of 237.4 C aftercorrections for barometric pressure and emergen
15、t stem have been applied. The distillation shall be carried out in accordance withTest Method D850 using a total immersion thermometer with a range from 195 C to 305 C, graduated in 0.5 C, and conformingto the requirements for Thermometer 69C as described in Specification E1. Temperature measuring d
16、evices such as precisionthermocouples, resistance temperature detectors (RTDs), and liquid-in-glass thermometers with equal or better accuracies in theappropriate temperature range may 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 M
17、ethod D71, or othermethod of equivalent accuracy.6.1.3 The quinoline shall be clear and light in color and shall contain less than 0.5 % volume of water as determined by TestMethod D95. If not, redistill the quinoline in all-glass apparatus, discarding the first 5 % and collecting the next 90 %. If
18、thequinoline contains suspended matter but is clear, light in color, and contains less than 0.5 % water, filter the quinoline through acrucible containing 5 g of Celite Filter Aid.6.1.4 Store the quinoline in a tightly closed, dark bottle.6.2 Toluene, Industrial Pure, meeting Specification D362.6.3
19、Acetone, meeting Specification D329.6.4 Concentrated Hydrochloric Acid.6.5 Celite Analytical Filter Aid (CAFA)Dry to constant weight at 105 C, and store in tightly stoppered container.6.5.1 Do not use any other grade of filter aid because filtration characteristics may differ. CAFA is manufactured o
20、nly byManville Co. and distributed through scientific supply houses.7. Hazards7.1 Fumes of the solvents should be removed by means of proper hoods from all working areas. The working area should bekept free of sparks and flames. Quinoline fumes should not be inhaled, and prolonged contact with the s
21、kin should be avoided.Toluene is toxic and flammable.7.2 Observe proper laboratory procedures for handling hydrochloric and diluting acid.8. Bulk Sampling8.1 Samples from shipments shall be taken in accordance with Practice D4296 and shall be free of foreign substances.Thoroughly mix the sample imme
22、diately before removing a representative portion for the determination or for dehydration.9. Dehydration of Sample9.1 Hard PitchIf the solid bulk sample contains free water, air-dry a representative portion in a forced draft oven at 50 C.9.2 Soft PitchIf the presence of water is indicated by surface
23、 foam on heating, maintain a representative portion of the bulksample at a temperature between 125 C and 150 C in an open container until the surface is free of foam. Take care not tooverheat, and remove heat source immediately when foam subsides.9.3 TarA wet tar sample may either be dehydrated or u
24、sed as received as long as conditions stated in 9.3.1 and 9.3.2 are met.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 170
25、C. Separate any oilfrom the water that has distilled over (if crystals 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.9.3.2 As an alternative to dehydration, the water content
26、 of the tar is determined by Test Method D95, and if the water contentis less than 10 mass percent, the QI content is corrected to a dry-tar basis (see 13.2). This alternative test method applies only tostable emulsions of water in tar, that is, no water separates when the tar sample is left undistu
27、rbed for 24 h at room temperature.10. Preparation of Working Sample10.1 Hard PitchIf the pitch can be crushed at room temperature, prepare a 20 g working sample by suitable crushing, mixing,and quartering of a representative portion of the dry sample. The crushing can be done with a small jaw crushe
28、r and a mullitemortar and pestle. No particle in the representative sample shall be larger than 5 mm in any dimension. Crush this sample so thatall of it will pass the 250 m (No. 60) sieve but will have a minimum of fine particles. Store the sieved working sample in a tightlyclosed container and use
29、 within 24 h (see 10.4).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 thelowest temperature that will permit passage through the 600 m (No. 30) sieve, taking care to avoid excessive loss of volatilematter. Do not exceed 10
30、min for this melting period. Pass the heated sample through the 600 m sieve to remove foreign matter.D2318 15210.3 TarHeat a representative portion of the dry tar to the lowest temperature that will permit passage through the 600 m(No. 30) sieve, then filter through this sieve to remove foreign matt
31、er.10.4 Preservation of SamplesStore samples as large lumps or as solidified melts in closed containers. Discard workingsamples 24 h after crushing and sieving as changes in composition sometimes occur in pulverized pitch.11. Crucible Preparations11.1 If the crucible, after thorough cleaning (see 11
32、.2), has been 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 for 1 h at about 800 C. Cool the crucibleslowly by placing it in a drying oven for 1 h after removal from the furnace to prevent cracki
33、ng and place it in a desiccator whilestill warm.11.2 After the crucible has been used for six determinations, remove any residual ash from pores in the filtering area by boilingin 1 + 1 hydrochloric acid.Add equal volume of concentrated hydrochloric acid to distilled water. Then boil the crucible in
34、 distilledwater, thoroughly back wash with distilled water, 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 mg and 150 mg of matter insoluble in quinoline (QI), unless this wouldrequire less than the
35、minimum acceptable sample mass of 0.5 g, in which case 0.5 g shall be used.12.3 Transfer 1 g 6 0.1 g of dry CAFA to a clean, dry, filtering crucible. Weigh immediately, and record the mass of crucibleplus CAFA.12.4 Place the required amount of sample in a tared beaker and weigh. Calculate and record
36、 the mass of the sample. Transferabout half of the CAFA from the crucible to the beaker with sample. Distribute the remaining CAFA evenly over the bottom ofthe crucible.12.5 Add 25 mLof quinoline to the beaker while stirring the mixture with a stirring rod or thermometer to break up lumps, thencover
37、 the beaker with a small watch glass. Place the beaker and a wash bottle containing quinoline on an electric hot plate or ina water bath maintained at 75 C 6 5 C. (A suitable weight can be used to keep the beaker from being upset in the water bath.)Digest for at least 20 min. Occasionally stir the c
38、ontents of the beaker to promote digestion. Check for completeness of digestionby inspecting the bottom of the beaker for undigested pitch.12.6 Insert the filter tube with adapter in the filter flask, and place the previously prepared and tared crucible in the adapter.Carefully add sufficient quinol
39、ine to the crucible to wet the Celite thoroughly. Apply suction and form a mat of evenly distributedCelite. Maintain suction until filtration and subsequent 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
40、, without disturbing themat. Stir the mixture in the beaker immediately before pouring successive portions into the crucible. Allow the contents to draincompletely, but not to the extent that the insoluble material on the filter appears substantially dry.12.8 Wash the beaker, thermometer, or stirrin
41、g rod, and crucible with small portions (2 mL to 3 mL each) of quinoline at 75 C6 5 C from the wash bottle. Pass all the washes through the filter. Allow each wash to pass almost completely through the filterbefore the next is added. Use a suitable policeman to sweep the insoluble particles into the
42、 crucible. Repeat the quinoline washesuntil the filtrate is the same color as the quinoline used for washing. Twelve washings are usually enough.12.9 After the final quinoline wash has passed through the filter, fill the crucible with toluene and wash with a total of 75 mLto 100 mLof toluene using s
43、uction.After all the toluene has passed through the filter, wash the contents of the crucible in the samemanner with acetone. Maintain full suction for a minimum of 5 min after the acetone wash. Remove the crucible, and wipe theoutside with a clean, soft cloth or tissue moistened with acetone.12.9.1
44、 During the quinoline and toluene washing do not allow the CAFA mat to get completely dry as the filtration rate maydecrease considerably.12.10 Place the filtering crucible in the drying oven at 105 C to 110 C and dry to constant weight (61 mg). When the hotcrucible is removed from the drying oven i
45、t shall have no odor of quinoline. Transfer the crucible to the desiccator and cool for25 min, then weigh and record the weight of the filtering crucible and its contents (see 12.1).12.10.1 Insoluble matter on the filter, after washing with acetone, should have no odor of quinoline, which is evidenc
46、e ofinsufficient washing. If odor of quinoline is detectable, repeat the entire determination.12.11 If the mass of matter insoluble in quinoline is less than 75 mg or more than 150 mg, repeat the determination with anadjusted sample mass of not less than 0.5 g (see 12.2).13. Calculation13.1 Calculat
47、e the QI content as follows:QI,mass%5A 2B!/C# 3100 (1)D2318 153where:A = total mass of the filtering crucible and CAFA added to the crucible, and matter insoluble in quinoline,B = initial mass of the filtering crucible containing dried CAFA, andC = mass of sample taken for the determination.13.2 If
48、the QI was determined on a wet tar sample (see 9.3.2), correct the QI value determined in 13.1 to a dry-tar basis asfollows:QI,mass %dry basis!5 (2)QI,mass %wet basis!1002water content of tar,mass%!310014. Report14.1 Report the QI content to the nearest 0.1 %.15. Precision and Bias15.1 The following
49、 criteria shall be used for judging the acceptability of results (95 % probability):15.1.1 RepeatabilityDuplicate values by the same operator shall not be considered suspect unless the determined percentagesdiffer 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 than 4 %.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 mo
