1、Designation: D 4746 98 (Reapproved 2003)e1An American National StandardStandard Test Method forDetermination of Quinoline Insolubles (QI) in Tar and Pitchby Pressure Filtration1This standard is issued under the fixed designation D 4746; the number immediately following the designation indicates the
2、year oforiginal adoption or, in the 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.e1NOTEWarning notes were editorially moved into the standard te
3、xt in November 2003.1. Scope1.1 This test method covers the determination of thequinoline-insoluble matter (QI) in tar and pitch by pressurefiltration and gives results comparable to those obtained byTest Method D 2318.1.2 Since this test method is empirical, strict adherence toall details of the pr
4、ocedure is necessary.1.3 This standard does not purport 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 t
5、o use. Specific precau-tionary statements are given in Section 7.2. Referenced Documents2.1 ASTM Standards:2D70 Test Method for Density of Semi-Solid BituminousMaterials (Pycnometer Method)D95 Test Method for Water in Petroleum Products andBituminous Materials by DistillationD 329 Specification for
6、AcetoneD 850 Test Method for Distillation of Industrial AromaticHydrocarbons and Related MaterialsD 2318 Test Method for Quinoline-Insoluble (QI) Contentof Tar and PitchD 4296 Practice for Sampling PitchE1 Specification for ASTM Thermometers3. Summary of Test Method3.1 The sample is digested in hot
7、quinoline and filteredthrough a heated pressure filter. The insoluble material iswashed with hot, fresh quinoline and with cold acetone, 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 theunifo
8、rmity of shipments and sources of supply.5. Apparatus5.1 Pressure Filtration VesselThe pressure filtration ves-sel3(see Fig. 1) is a stainless steel (304) jacketed block heatedby steam or cooled with water, sealed by a lid, flat gasket, andclamp. The interior of the block is designed to accept a 3A2
9、Berlin porcelain filtration crucible (see 5.4). The crucible issealed within the block by the use of three O-rings, a cruciblesealing collar, and an adjustable plunger.5.1.1 The seal is accomplished when the sealing lid isplaced on top of the block and clamped. The adjustable plungerapplies a force
10、to the crucible sealing collar, which in turnpushes downward on the crucible and simultaneously com-presses O-ring gaskets, forming a seal between surfaces of thecrucible and the wall of the block. The filtration of material isaccomplished by nitrogen (10 to 30 psig) introduced throughthe lid of the
11、 pressure filter. The filtrate exits from the draintube at the bottom of the block. The filtrate is disposed into aBuchner flask, attached to drain tube by a No. 7 rubber stopper.A vacuum hose is attached to the Buchner flask and placed ina 100-mL beaker containing water to indicate the exit ofnitro
12、gen when the filtration is completed.5.2 Beaker,50mL.5.3 Buchner Flask, 500.5.4 Filtering Crucible, porcelain, with a medium-porositybottom, top outer diameter 134 in. (45 mm), bottom outerdiameter 1.2 in. (30 mm), height 2 in. (50 mm).5.5 Analytical Balance.5.6 Desiccator.5.7 Thermometer, 0 to 300F
13、 (150C).5.8 Drying Oven, maintained at 221F (105C).1This test method is under the jurisdiction 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. 18,
14、 2003. Published November 2003. Originallyapproved in 1987. Last previous edition approved in 1998 as D 474698.2For 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 s
15、tandards Document Summary page onthe ASTM website.3The sole source of supply of the pressure filtration vessel known to thecommittee at this time is Koppers Co., Inc., 1005 Wm. Pitt Way, Pittsburgh, PA15238. If you are aware of alternative suppliers, please provide this information toASTM Headquarte
16、rs.Your comments will receive careful consideration at a meetingof the responsible technical committee,1which you may attend.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.5.9 Mortar and Pestle.5.10 Two Wash Bottles, 500 mL.5.11 Ste
17、am Bath.6. Reagents6.1 QuinolineRefined, meeting the following require-ments:6.1.1 The quinoline shall be distilled from 5 to 95 % withina range of 2F (1C) that shall include the temperature of459.3F (237.4C) after corrections for barometric pressureand emergent steam have been applied. The distilla
18、tion shall becarried out in accordance with Method D 850 using a total-immersion thermometer with a range from 383 to 581F (195to 305C), graduated in 1F (0.5C) and conforming to therequirements for thermometer 69C as described in Specifica-tion E1.6.1.2 The quinoline shall have a specific gravity at
19、 15.5/15.5C of 1.092 to 1.098, as determined by Test Method D70,or other method of 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 an all-glassapparatus, dis
20、carding the first 5 % and collecting the next 90 %.If the quinoline contains suspended matter but is clear, light incolor, and contains less than 0.5 % water, filter the quinolinethrough a crucible containing5gofcelite filter aid.6.1.4 Store the quinoline in a tightly closed, dark bottle.6.2 1 + 1 H
21、ydrochloric Acid SolutionAdd equal volumeconcentrated hydrochloric acid to distilled water. (WarningCorrosive.)6.3 Acetone, meeting Specification D 329.(WarningFlammable (Health Hazard).)7. Safety Precautions7.1 Fumes of the solvents should be removed by means ofproper hoods from all working areas.
22、The working area shouldbe kept free of sparks and flames. Quinoline fumes should notbe inhaled, and prolonged contact with skin should be avoided.7.2 Observe proper laboratory procedures for handling anddiluting hydrochloric acid.8. Bulk Sampling8.1 Samples from shipments shall be taken in accordanc
23、ewith Practice D 4296 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 Hard PitchIf the solid bulk sample contains freewater, air dry a representative portion in
24、a forced draft oven at122F (50C).9.2 Soft Pitch (Softening Point 140F (60C)If thepresence of water is indicated by surface foam on heating,maintain a representative portion of the bulk sample at atemperature between 257 and 302F (125 and 150C) in anopen container until the surface is free of foam. T
25、ake care notto overheat, and remove the heat source immediately when thefoam subsides.9.3 TarA wet tar sample can 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 sample.9.3.2 As an alternative to dehy
26、dration, the water content ofthe tar is determined by Test Method D95and, if the watercontent is less than 10 weight %, the QI content is corrected toa dry-tar basis (see 13.2). This alternative method applies onlyto stable emulsions of water in tar, that is, no water separateswhen the tar sample is
27、 left undisturbed for 24 h at roomtemperature.10. Preparation of Working Sample10.1 Pitch that is sufficiently hard at room temperature shallbe finely pulverized in a mortar. Crush this sample so that allof it will pass the 250-m (No. 60) sieve. Soft pitches and tarsshall be warmed and well agitated
28、 before sampling.10.2 The amount of sample to be taken for the test shall besuch that the final quantity of quinoline insoluble (QI) shall benot less than 0.1 g. As a guide, the following sample sizes arerecommended:Sample Size, gCrude coke oven tar 5.0Horizontal retort tars 2.5Fiber pitch 5.0Other
29、pitches 2.5Distilled tars 2.5Vertical retort tars 10.0 to 25.010.2.1 When the sample contains 15 % QI or if the softeningpoint is greater than 248F (120C), the amount used fortesting should be reduced, but to not less than 0.5 g.FIG. 1 Pressure FilterD 4746 98 (2003)e1211. Crucible Preparation11.1 I
30、f 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 for1hatabout 1472F (800C).Cool the crucible slowly by placing it in a drying oven for 1 ha
31、fter removal from the furnace to prevent cracking and place itin a desiccator while still warm.11.2 After the crucible has been used for six determinations,remove any residual ash from pores in the filtering area byboiling in1+1hydrochloric acid solution. Refer to 6.2. Thenboil the crucible in disti
32、lled water, thoroughly back wash withdistilled water, dry, and ignite as in 11.1.12. Procedure12.1 Weigh the recommended amount of sample (usually2.5 g) into a 50-mL beaker and record weight (W1).12.2 Add 2.0 mL of refined quinoline per gram of sample tobeaker.12.3 Place thermometer 0 to 300F (150C)
33、 (6 in. length)into solution and heat on steam bath to 167 6 10F (75 6 5C)for not less than 15 nor more than 20 min. Closely inspect thethermometer and bottom of the beaker for undissolved pitchand stir so that all of the pitch is brought into solution.12.4 Place gaskets into the pressure vessel.12.
34、5 Start to heat block with steam (see 5.1 and Fig. 2).12.6 Weigh a 3A2 Berlin crucible and record mass (W2).12.7 Place the preweighed crucible in the pressure vesseland then put crucible collar on (see 5.1 and Fig. 3).12.8 When the quinoline-pitch solution has completed theheating cycle (see 12.3),
35、pour the solution into the crucible,decanting it alongside the thermometer. Wash down the ther-mometer and beaker with 5 to 10 mL of quinoline and place onthe steam bath.12.9 Place the lid of the pressure filter with the adjustableplunger on the pressure vessel. The plunger shall be adjusted sothat
36、there is about18-to14-in. gap between the lid and the flatgasket (see Fig. 1) of block. To close, force down by hand andattach clamp.NOTE 1Sealing of the crucible is a trial-and-error process. Excessivepressure could cause the crucible to be pushed past the O-rings duringfiltration or not allow comp
37、lete sealing of the lid. Insufficient pressure ofthe plunger could cause leaks around the O-rings.12.10 Add 10 psig of nitrogen using the pressure controllerto pressurize the vessel to 10 psig with nitrogen. One may seeslight bubbling from the indicator before the filtrate can be seencoming from the
38、 drain. Once the filtrate is flowing, pressurecan be increased to 30 psig gradually. Nitrogen may bubbleslowly (caused by volume displacement in the collecting flask)through the water seal and may bubble fast when filtration iscompleted. When filtrate stops coming out of bottom, shut offnitrogen and
39、 remove lid.NOTE 2In some cases, nitrogen stops bubbling although there is nodraining of the filtrate. The filtration is actually completed, the quinolineinsolubles have compacted on the bottom (filter cake) of the crucible anddo not let nitrogen pass through. By increasing the pressure, nitrogen wi
40、lleventually break through the filter cake.12.11 Continue filtering the sample as described in 12.8 to12.10 until the filtrate is clear. This usually will take aboutthree washings of the beaker. When the third or last washing ispoured into the crucible, rinse the beaker with the wash bottle,allowing
41、 the solution to run into the crucible to remove anycarbon deposits. Filter the rinses.12.12 When the last filtration is complete, shut the steamand nitrogen off. Remove the lid and start cooling the blockwith water (it takes approximately 5 min to cool the block andcrucible).12.13 Once cool, fill t
42、he crucible to about three quarters ofits volume with acetone. Place lid on and follow 12.10 to filter.Perform this step three times.12.14 When acetone rinses are complete, shut off thenitrogen, remove the lid, remove the crucible, and wipe sideswith a paper towel containing acetone to remove any tr
43、aces ofquinoline. Place crucible in an oven at 221F (105C) for aminimum of 30 min, preferably 1 h. Remove, place in adesiccator, and allow to cool for 30 min.12.15 Weigh the crucible containing quinoline insolublesand record the mass (W3).NOTE 3For pitches yielding slow-filtering quinoline insoluble
44、s, ahigher pressure may be used of up to 50 but not to exceed 75 psig. Underthese conditions, a stainless steel disk with a18-in. hole is added to thebottom of the block. Under high pressure, the crucible can be forcedthrough O-rings. The stainless steel plate reduces the distance the cruciblewill t
45、ravel to a minimum and thus avoids breakage and sample loss.13. Calculation13.1 Calculate the quinoline-insoluble (QI) content as fol-lows:QI,%5 W32 W2!/W1# 3 100 (1)where:W3= mass of crucible with QI, g;W2= mass of the crucible, g; andW1= mass of the sample, g.13.2 If the QI was determined on a wet
46、 tar sample (see9.3.2), correct the QI value determined in 13.1 to a dry-tar basisas follows:QI, mass % dry basis!5QI, mass % wet basis! from 13.1100 2 water content of tar, mass %!3 100(2)14. Report14.1 Report the quinoline insoluble (QI) content to thenearest 0.1 %.15. Precision and Bias415.1 Repe
47、atabilityDuplicate values by the same operatorshall not be considered suspect unless they differ by more than0.2 %.15.2 ReproducibilityThe values reported by each of twolaboratories, representing the arithmetic average of duplicatedeterminations, shall not be considered suspect unless theydiffer by
48、more than 0.3 %.4Supporting data have been filed at ASTM International Headquarters and maybe obtained by requesting Research Report RR: D081002.D 4746 98 (2003)e13FIG. 2 Pressure Filter DimensionsD 4746 98 (2003)e1416. Keywords16.1 coal-tar insolubles; pitch; pressure filtration; QI;quinoline-insol
49、ubles; tarFIG. 3 Pressure Filter Tension Adjuster, Collar, and CapD 4746 98 (2003)e15ASTM 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 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 e
