1、Designation: D4527 99 (Reapproved 2011)Standard Test Method forCarbon BlackSolvent Extractables1This standard is issued under the fixed designation D4527; 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.1. Scope1.1 This test method covers the procedure for measuringcarbon black solvent extractables.1.1.1 This test method determines the total mater
3、ial 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 asstandard. No other units of measurement are included in thisstandard.1.3 This standard does not p
4、urport 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, see
5、 Section 7.2. Referenced Documents2.1 ASTM Standards:2D3051 Recommended Practice for Carbon BlackStatingthe Precision of ASTM Test Methods3D3396 Recommended Practice for Carbon BlackMeasuring the Precision of ASTM Test Methods33. Summary of Test Method3.1 A specimen of carbon black is extracted for
6、48 h (orother specified 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 blac
7、k extract test procedure 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 %) ma
8、y require a more 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 Extracti
9、on Thimble, glass, 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.Ahot plate extraction heater or
10、hemispherical heating 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
11、 for final solvent 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.1This test
12、method is under the jurisdiction of ASTM Committee D24 on CarbonBlack and is the direct responsibility of Subcommittee D24.31 on Non-CarbonBlack Components of Carbon Black.Current edition approved May 1, 2011. Published July 2011. Originally approvedin 1985. Last previous edition approved in 2004 as
13、 D4527 99 (2004). DOI:10.1520/D4527-99R11.2For 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.3Withdrawn. The las
14、t approved version of this historical standard is referencedon www.astm.org.4Fisher Scientific No. 9-556B available from Fisher Scientific Co., 203 FisherAve., Pittsburgh, PA 15219, has been found satisfactory. The use of KontasK-586100 (glass jacketed) available from Kontas Glass Co., 8000 Spruce S
15、t.,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) available from Fisher Scien-tific Co., and Ventron No. 2034 (te
16、flon 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 19428-2959, United States.5.9 Oven, gravity-convection type, capable
17、 of temperatureregulation within 61C at 125C and temperature uniformitywithin 65C.5.10 Desiccator.5.11 Analytical Balance, with a sensitivity of 60.1 mg.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,
18、 extracted with toluene, air-dried, followedby drying in a convection oven at 125C for 1 h. Store in aclosed container until ready 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 polynucle
19、ar aromatic compounds, some of which arecarcinogens. These compounds, when present, are so stronglybound to the carbon black that they are biologically inactive.However, they may be removed by extraction with toluene orother appropriate solvents. Avoid skin contact with solventextracts from such car
20、bon blacks.7.2 For most pelleted blacks, the depth of 60 mm in thethimble should provide a sample of 15 to 25 g. Unpelletedblacks 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 le
21、akage, the joints may be sealed withTFE-fluorocarbon inserts or wrapped with TFE-fluorocarbonlaboratory tape.7.4 New thimbles should 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 conv
22、eniently cleaned by back washing undersuction with appropriate media (water, acetone, etc.). If thefritted disc becomes fouled with 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 o
23、f chromic acid cleaning solution isnot recommended. The permeability of the clean thimbleshould be checked periodically. Discard thimbles 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
24、 the extractionof carbon black. If this is not feasible, the glassware must beextracted before use in accordance with 7.6.7.6 New 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 cm3s
25、olvent).7.7 Two or three glass beads may be added to the extractionflask to promote smooth boiling. Do not use porous boilingchips.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
26、 the extraction.7.9 The nitrogen should be delivered through a glass ormetal tip. Do not allow plastic or rubber to contact the solvent.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
27、.12 Any further analysis of the extracted material typicallyrequires that it be in solution. Complete re-solution of the dryextract may be difficult or impossible. Therefore, if furtheranalysis is to be performed, an additional sample of the carbonblack should be extracted and solvent removal carrie
28、d only tothe desired reduced volume. It is recommended that exposureto strong light, especially sunlight, be avoided during extrac-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 sign
29、ificant varia-tion in the amount of residue found in different bottles oftoluene bearing the same lot number. Consequently, blanksshould 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 d
30、imensions 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, 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 woo
31、l above the black. Insert the thimble into theextraction tube, place 150 cm3of toluene in the extractionflask, and assemble the apparatus (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 alumin
32、um foil loosely around the extractiontube and upper part of the flask to reduce heat loss. Terminatethe extraction with the extraction 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 extra
33、ction flask into a cleanfilter flask using moderate suction, rinsing the extraction flaskand filter funnel with several small portions 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 solut
34、ion to hasten evaporation(see 7.9-7.11).8.6 Transfer the remaining solution to the previously driedand weighed (to 0.1 mg) final container, rinsing the flask withseveral small portions of toluene. Continue evaporation toessentially dryness (see 7.12).8.7 To complete solvent removal to constant resid
35、ue mass,place the container in a vacuum oven at 40C. Setting thecontainer on the floor of the oven should be avoided; anon-conductive support or equivalent should be used. Slowly7Distilled-in-glass toluene available from Burdick and Jackson, 1953 T.S.Harvey, Muskegan, MI 49442 and Photrex grade avai
36、lable 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. Louis, MO 63134 has generally been found acceptable.D4527 99 (2011)2reduce the oven pressure to approximately 3.3
37、 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 for15 min, cool, and reweigh. Repeat as necessary until the massis constant. Subtract the original mass to
38、 obtain the mass ofresidue.8.8 Make duplicate blank determinations on each bottle oftoluene placed in use. Follow this procedure 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)
39、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 following 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
40、0.01 %.11. Precision and Bias11.1 These precision data are based on single tests of threesamples by five laboratories on two days. 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
41、fivelaboratories participated in the interlaboratory study.11.2 In test method statistical terminology, bias is thedifference between 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 is
42、exclusively defined by this test method. Bias, therefore, cannotbe determined.11.3 Repeatability (Single-Operator)The repeatabilityhas been estimated to be 60.06 percentage points. Two testresults are significantly different if their difference exceeds0.09 percentage points.11.4 Reproducibility (Mul
43、tilaboratory)The reproducibil-ity has been estimated to be 60.09 percentage points. Two testresults are significantly different if their difference exceeds0.13 percentage points.NOTE 2This precision statement was developed following the guide-lines presented in Practices D3051 and D3396.12. Keywords
44、12.1 carbon black; cyclohexane; extract; silica gel adsorbentaromatic/polar fractions; solvent extractables; tolueneASTM 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 a
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47、 If you feel that your comments have not received a fair hearing you shouldmake your views known to the ASTM Committee on Standards, 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. Indi
48、vidual 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). Permission rights to photocopy the standard may also be secured from the ASTM website (www.astm.org/COPYRIGHT/).D4527 99 (2011)3
