1、Designation: D 4527 99 (Reapproved 2004)Standard Test Method forCarbon BlackSolvent Extractables1This standard is issued under the fixed designation D 4527; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revision.
2、 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 procedure for measuringcarbon black solvent extractables.1.1.1 This test method determines the total ma
3、terial ex-tracted from carbon black by toluene under specified condi-tions. The procedure is also applicable to other solvents such ascyclohexane, etc.1.2 The values stated in SI units are to be regarded as thestandard. The values given in parentheses are for informationonly.1.3 This standard does n
4、ot 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 to use. For a specificprecautionary statement,
5、 see Section 7.2. Referenced Documents2.1 ASTM Standards:2D 3051 Practice for Carbon BlackStating the Precision ofASTM Test Methods3D 3396 Practice for Carbon BlackMeasuring the Preci-sion of ASTM Test Methods33. Summary of Test Method3.1 A specimen of carbon black is extracted for 48 h (orother spe
6、cified time) in a Soxhlet extractor, the solvent re-moved by controlled temperature evaporation, and the ex-tracted residue determined gravimetrically. If the carbon blackextractables are to be subjected to additional analysis, seeSection 7.4. Significance and Use4.1 The carbon black extract test pr
7、ocedure provides auniform and precise method for the gravimetric determinationof organic-solvent extractables on carbon black. Accuracy andprecision are acceptable for most specification or regulatorypurposes, or both. However, carbon black with very low extract(less than 0.02 %) may require a more
8、rigorous extractionprocedure. The actual chemical composition of the extract canvary significantly with the type and origin of the carbon black.5. Apparatus5.1 Soxhlet Extraction Apparatus, with interchangeableground joints, 40 mm I.D. extraction tube, and 250-cm3flask.45.2 Extraction Thimble, glass
9、, 35-mm diameter by 90-mmheight, with coarse porosity fritted disc.5When filled with 50cm3of toluene, drainage time for the first 40 cm3should notexceed 95 s. Discard thimbles taking longer.5.3 Heater, for extraction flask, with adjustable heat input.A hot plate extraction heater or hemispherical he
10、ating mantle ispreferred.5.4 Filter Funnel, glass fritted disc type, with mediumporosity fritted disc.5.5 Filter Flask, 125 or 250 cm3.5.6 Water Bath, or other suitable warming means for evapo-rating solvent from extract at a controlled temperature of 40 to50C.5.7 Container, suitable for final solve
11、nt removal and weigh-ing of residue. A lightweight aluminum dish 63 by 17.5 mm, aTFE-fluorocarbon cup or a 50-cm3glass beaker is suggested.65.8 Vacuum Oven, gravity-convection type, capable of tem-perature regulation within 61C at 125C and temperatureuniformity within 65C.5.9 Oven, gravity-convectio
12、n type, capable of temperatureregulation within 61C at 125C and temperature uniformitywithin 65C.5.10 Desiccator.5.11 Analytical Balance, with a sensitivity of 60.1 mg.1This test method is under the jurisdiction of ASTM Committee D24 on CarbonBlack and is the direct responsibility of Subcommittee D2
13、4.31 on Non-CarbonBlack Components of Carbon Black.Current edition approved July 1, 2004. Published July 2004. Originally approvedin 1985. Last previous edition approved in 1999 as D 4527 99.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serv
14、iceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.3Withdrawn.4Fisher Scientific No. 9-556B available from Fisher Scientific Co., 203 FisherAve., Pittsburgh, PA 15219, has been found satisfactory. The use of KontasK-58610
15、0 (glass jacketed) available from Kontas Glass Co., 8000 Spruce St.,Vineland, NJ 08360, simplifies insulating the apparatus and reduces the possibilityof breakage.5Fisher Scientific 9-653B available from Fisher Scientific Co., has been foundsatisfactory.6Fisher Scientific No. 8-732-5C (aluminum dish
16、) available from Fisher Scien-tific Co., and Ventron No. 2034 (teflon cup) available from Ventron InstrumentCorp., Cahn Division, 16707 S. Carmenita Rd., Cerritos, CA 90701, have beenfound to be satisfactory.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 194
17、28-2959, United States.6. Reagents and Materials6.1 Toluene, having a residue after evaporation less than 10ppm (preferably less than 2 ppm).76.2 Nitrogen.6.3 Glass wool, extracted with toluene, air-dried, followedby drying in a convection oven at 125C for 1 h. Store in aclosed container until ready
18、 to use.6.4 Aluminum Foil.7. Precautions7.1 For safety reasons, conduct the extraction and solventevaporation in an approved fume hood. Carbon blacks maycontain polynuclear aromatic compounds, some of which arecarcinogens. These compounds, when present, are so stronglybound to the carbon black that
19、they are biologically inactive.However, they may be removed by extraction with toluene orother appropriate solvents. Avoid skin contact with solventextracts from such carbon blacks.7.2 For most pelleted blacks, the depth of 60 mm in thethimble should provide a sample of 15 to 25 g. Unpelletedblacks
20、should be predensified sufficiently that this depth willrequire a sample of at least 10 g.7.3 Do not use joint lubricant on the ground joints. Tominimize vapor loss by leakage, the joints may be sealed withTFE-fluorocarbon inserts or wrapped with TFE-fluorocarbonlaboratory tape.7.4 New thimbles shou
21、ld be washed before use by suctionwith hot HCl and then rinsed with distilled or deionized waterto remove loose particles of foreign matter such as dust.Thimbles are conveniently cleaned by back washing undersuction with appropriate media (water, acetone, etc.). If thefritted disc becomes fouled wit
22、h carbon black, it may benecessary to burn it out by slowly heating the thimble fromroom temperature to 500C in a muffle furnace. One hour isusually sufficient. The use of chromic acid cleaning solution isnot recommended. The permeability of the clean thimbleshould be checked periodically. Discard t
23、himbles with drainagetimes exceeding the 95 s specified under 5.2.7.5 To prevent contamination, it is recommended that allglassware used in this procedure be reserved for the extractionof carbon black. If this is not feasible, the glassware must beextracted before use in accordance with 7.6.7.6 New
24、glassware, including thimbles, must be extracted,repeatedly if necessary, with toluene or other solvent until theblank is acceptable (preferably less than 0.3 mg/150 cm3solvent).7.7 Two or three glass beads may be added to the extractionflask to promote smooth boiling. Do not use porous boilingchips
25、.7.8 An extraction must be discarded if there is any visiblecarbon black in the extraction flask or if the thimble does notdrain properly and overflows at any time during the extraction.7.9 The nitrogen should be delivered through a glass ormetal tip. Do not allow plastic or rubber to contact the so
26、lvent.7.10 To protect from dust, a loose cover over the evapora-tion vessel is recommended.7.11 Solvent evaporation may be conducted in a vacuumevaporator, if available.7.12 Any further analysis of the extracted material typicallyrequires that it be in solution. Complete re-solution of the dryextrac
27、t may be difficult or impossible. Therefore, if furtheranalysis is to be performed, an additional sample of the carbonblack should be extracted and solvent removal carried only tothe desired reduced volume. It is recommended that exposureto strong light, especially sunlight, be avoided during extrac
28、-tion and subsequent handling, and that the extract be blanketedwith inert gas (nitrogen) if retained for any length of time.7.13 It has been found that there may be significant varia-tion in the amount of residue found in different bottles oftoluene bearing the same lot number. Consequently, blanks
29、should be run on each bottle.8. Procedure8.1 Dry an adequate specimen of the carbon black for1hinthe gravity-convection oven set at 125C in an open containerof suitable dimensions so that the depth of the black is no morethan 10 mm. Cool and store the sample in a desiccator.8.2 Weigh, into a clean,
30、dry extraction thimble, sufficientdried carbon black to fill the thimble to a depth of approxi-mately 60 mm. Record the weight of black to 0.1 g. Place aplug of glass wool above the black. Insert the thimble into theextraction tube, place 150 cm3of toluene in the extractionflask, and assemble the ap
31、paratus (see 7.1-7.6).8.3 Extract continuously for 48 h (or other time if specified),heating so that the cycle time between siphonings is 4 to 5 min(see 7.7). Wrap aluminum foil loosely around the extractiontube and upper part of the flask to reduce heat loss. Terminatethe extraction with the extrac
32、tion cup nearly full to reduce thequantity of solvent to be subsequently evaporated from theresidue in the extraction flask (See 7.8).8.4 Filter the contents of the extraction flask into a cleanfilter flask using moderate suction, rinsing the extraction flaskand filter funnel with several small port
33、ions of toluene.8.5 Evaporate the contents of the filter flask at 40 to 50Cuntil approximately 10 cm3remains. Direct a stream of drynitrogen onto the surface of the solution to hasten evaporation(see 7.9-7.11).8.6 Transfer the remaining solution to the previously driedand weighed (to 0.1 mg) final c
34、ontainer, rinsing the flask withseveral small portions of toluene. Continue evaporation toessentially dryness (see 7.12).8.7 To complete solvent removal to constant residue mass,place the container in a vacuum oven at 40C. Setting thecontainer on the floor of the oven should be avoided; anon-conduct
35、ive support or equivalent should be used. Slowlyreduce the oven pressure to approximately 3.3 kPa andthereafter hold at that level. After a suitable time (usually 45min to 1 h), cool the container and contents to room tempera-ture in a desiccator and weigh to 0.1 mg. Return to the oven for7Distilled
36、-in-glass toluene available from Burdick and Jackson, 1953 T.S.Harvey, Muskegan, MI 49442 and Photrex grade available from J.T. BauerChemical Co., 223 Red School Ln., Phillipsburg, NJ 08865 are preferred products.Analytical reagent grade available from Mallinckrodt, Inc., 675-T McDonnell Blvd.,St. L
37、ouis, MO 63134 has generally been found acceptable.D 4527 99 (2004)215 min, cool, and reweigh. Repeat as necessary until the massis constant. Subtract the original mass to obtain the mass ofresidue.8.8 Make duplicate blank determinations on each bottle oftoluene placed in use. Follow this procedure
38、exactly but omitthe carbon black (see 7.13).9. Calculation9.1 Calculate the mass percent extractables to the nearest0.01 % as follows:Extractables, mass % 5R 2 BW3 100 (1)where:R = mass of residue, g,B = mass of residue from blank, g, andW = mass of carbon black sample, g.10. Report10.1 Report the f
39、ollowing information:10.1.1 Proper identification of the sample,10.1.2 The solvent used,10.1.3 The extraction time, and10.1.4 The result obtained, reported to the nearest 0.01 %.11. Precision and Bias11.1 These precision data are based on single tests of threesamples by five laboratories on two days
40、. The range of thesamples studied was from about 0.06 % to about 1.02 %.Precision is expressed in absolute terms.NOTE 1The precision is based on limited data in that only fivelaboratories participated in the interlaboratory study.11.2 In test method statistical terminology, bias is thedifference bet
41、ween an average test value and the reference ortrue test property value. Reference values do not exist for thistest method since the value or level of the test property isexclusively defined by this test method. Bias, therefore, cannotbe determined.11.3 Repeatability (Single-Operator)The repeatabili
42、tyhas been estimated to be 60.06 percentage points. Two testresults are significantly different if their difference exceeds0.09 percentage points.11.4 Reproducibility (Multilaboratory)The reproducibil-ity has been estimated to be 60.09 percentage points. Two testresults are significantly different i
43、f their difference exceeds0.13 percentage points.NOTE 2This precision statement was developed following the guide-lines presented in Practices D 3051 and D 3396.12. Keywords12.1 carbon black; cyclohexane; extract; silica gel adsorbentaromatic/polar fractions; solvent extractables; tolueneASTM Intern
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46、d 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 Stand
47、ards, at the address shown below.This standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,United States. Individual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the aboveaddress or at 610-832-9585 (phone), 610-832-9555 (fax), or serviceastm.org (e-mail); or through the ASTM website(www.astm.org).D 4527 99 (2004)3
