1、Designation: D4527 99 (Reapproved 2016)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 Referenced Documents2.1 ASTM Standards:2D3051 Practice for Carbon BlackStating the Precision ofASTM Test Methods (Withdrawn 1990)3D3396 Practice for Carbon Black Measuring the Precisionof ASTM Test Methods (Withdrawn 1990)33. Summary of Test Method3.1 A specimen of carbon black is extr
6、acted for 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 c
7、arbon black 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
8、0.02 %) may 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.
9、2 Extraction 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
10、heater or 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
11、, suitable 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.61This test method is under the jurisdiction of ASTM Committee D24 on CarbonBlack and is the direct responsibility of Subcommittee D24.
12、31 on Non-CarbonBlack Components of Carbon Black.Current edition approved June 1, 2016. Published July 2016. Originally approvedin 1985. Last previous edition approved in 2011 as D4527 99 (2011). DOI:10.1520/D4527-99R16.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact
13、ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.3The last approved version of this historical standard is referenced onwww.astm.org.4Fisher Scientific No. 9-556B available from Fisher Scien
14、tific Co., 203 FisherAve., Pittsburgh, PA 15219, has been found satisfactory. The use of KontasK-586100 (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
15、 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 (teflon cup) available from Ventron InstrumentCorp., Cahn Division, 16707 S. Carmenita Rd., Cerritos, CA 90701, have beenfound to be sat
16、isfactory.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States15.8 Vacuum Oven, gravity-convection type, capable of tem-perature regulation within 61C at 125C and temperatureuniformity within 65C.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 polynuclea
19、r 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 carb
20、on 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 lea
21、kage, 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 conve
22、niently 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 of
23、 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 cm3so
25、lvent).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 carried
28、 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 signi
29、ficant 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 di
30、mensions 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 wool
31、 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 aluminu
32、m 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 extrac
33、tion flask into a cleanfilter flask using moderate suction, rinsing the extraction flaskand filter funnel with several small portions of toluene.7Distilled-in-glass toluene available from Burdick and Jackson, 1953 T.S.Harvey, Muskegan, MI 49442 and Photrex grade available from J.T. BauerChemical Co.
34、, 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 (2016)28.5 Evaporate the contents of the filter flask at 40 to 50Cuntil approximately
35、 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 container, rinsing the flask withseveral small portions of toluene. Continue evaporation toesse
36、ntially 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-conductive support or equivalent should be used. Slowlyreduce 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 BW3100 (1)whe
39、re: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 0.0
40、1 %.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 fiv
41、elaboratories 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 isexc
42、lusively 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 (Multil
43、aboratory)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. Keywords12.
44、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 advi
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47、 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. Individ
48、ual 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 Copyright Clearance Center, 222Rosewood Drive, Danvers, MA 01923, Tel: (978) 646-2600; http:/ 99 (2016)3
