ASTM D4527-1999(2016) Standard Test Method for Carbon Black&x2014 Solvent Extractables《碳黑的标准试验方法&x2014 溶剂可萃取物》.pdf
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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 Referenced Documents2.1 ASTM Standards:2D3051 Practice for Carbon BlackStating the Precision ofASTM Test Methods (Withdrawn 1990)3D3396 Practice for Carbon Black Measuring the Precisionof ASTM Test Methods (Withdrawn 1990)33.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
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