ASTM D4527-2018 Standard Test Method for Carbon Black&x2014 Solvent Extractables.pdf
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1、Designation: D4527 99 (Reapproved 2016)D4527 18Standard 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 rev
2、ision. A 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 measuring carbon black solvent extractables.1.1.1 This test method determines the to
3、tal material extracted from carbon black by toluene under specified conditions. Theprocedure is also applicable to other solvents such as cyclohexane, etc.1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.1.3 This standard d
4、oes not purport to address all of the safety concerns, if any, associated with its use. It is the responsibilityof the user of this standard to establish appropriate safety safety, health, and healthenvironmental practices and determine theapplicability of regulatory limitations prior to use. For a
5、specific precautionary statement, see Section 7.1.4 This international standard was developed in accordance with internationally recognized principles on standardizationestablished in the Decision on Principles for the Development of International Standards, Guides and Recommendations issuedby the W
6、orld Trade Organization Technical Barriers to Trade (TBT) Committee.2. Referenced Documents2.1 ASTM Standards:2D3051D4483 Practice for Carbon BlackStating the Precision of ASTM Test MethodsEvaluating Precision for Test MethodStandards in the Rubber and Carbon Black Manufacturing Industries (Withdraw
7、n 1990)D3396 Practice for Carbon Black Measuring the Precision of ASTM Test Methods (Withdrawn 1990)33. Summary of Test Method3.1 A specimen of carbon black is extracted for 48 h (or other specified time) in a Soxhlet extractor, the solvent removed bycontrolled temperature evaporation, and the extra
8、cted residue determined gravimetrically. If the carbon black extractables are tobe subjected to additional analysis, see Section 7.4. Significance and Use4.1 The carbon black extract test procedure provides a uniform and precise method for the gravimetric determination oforganic-solvent extractables
9、 on carbon black.Accuracy and precision are acceptable for most specification or regulatory purposes,or both. However, carbon black with very low extract (less than 0.02 %) may require a more rigorous extraction procedure. Theactual chemical composition of the extract can vary significantly with the
10、 type and origin of the carbon black.5. Apparatus5.1 Soxhlet Extraction Apparatus, with interchangeable ground joints, 40 mm I.D. extraction tube, and 250-cm3 flask.35.2 Extraction Thimble, glass, 35-mm diameter by 90-mm height, with coarse porosity fritted disc.4 When filled with 50 cm3of toluene,
11、drainage time for the first 40 cm3 should not exceed 95 s. Discard thimbles taking longer.1 This test method is under the jurisdiction of ASTM Committee D24 on Carbon Black and is the direct responsibility of Subcommittee D24.31 on Non-Carbon BlackComponents of Carbon Black.Current edition approved
12、June 1, 2016June 1, 2018. Published July 2016July 2018. Originally approved in 1985. Last previous edition approved in 20112016 asD4527 99 (2011).(2016). DOI: 10.1520/D4527-99R16.10.1520/D4527-18.2 For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at
13、serviceastm.org. For Annual Book of ASTM Standardsvolume information, refer to the standards Document Summary page on the ASTM website.3 Fisher Scientific No. 9-556B available from Fisher Scientific Co., 203 FisherAve., Pittsburgh, PA15219, has been found satisfactory. The use of Kontas K-586100 (gl
14、assjacketed) available from Kontas Glass Co., 8000 Spruce St., Vineland, NJ 08360, simplifies insulating the apparatus and reduces the possibility of breakage.4 Fisher Scientific 9-653B available from Fisher Scientific Co., has been found satisfactory.This document is not an ASTM standard and is int
15、ended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Becauseit may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the curr
16、ent versionof the standard as published by ASTM is to be considered the official document.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States15.3 Heater, for extraction flask, with adjustable heat input. A hot plate extraction heater or h
17、emispherical heating mantle ispreferred.5.4 Filter Funnel, glass fritted disc type, with medium porosity fritted disc.5.5 Filter Flask, 125 or 250 cm3.5.6 Water Bath, or other suitable warming means for evaporating solvent from extract at a controlled temperature of 40 to 50C.5.7 Container, suitable
18、 for final solvent removal and weighing of residue. A lightweight aluminum dish 63 by 17.5 mm, aTFE-fluorocarbon cup or a 50-cm3 glass beaker is suggested.55.8 Vacuum Oven, gravity-convection type, capable of temperature regulation within 61C at 125C and temperatureuniformity within 65C.5.9 Oven, gr
19、avity-convection type, capable of temperature regulation within61C at 125C and temperature uniformity within65C.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 10 ppm (preferably less than 2 ppm
20、).66.2 Nitrogen.6.3 Glass wool, extracted with toluene, air-dried, followed by drying in a convection oven at 125C for 1 h. Store in a closedcontainer until ready to use.6.4 Aluminum Foil.7. Precautions7.1 For safety reasons, conduct the extraction and solvent evaporation in an approved fume hood. C
21、arbon blacks may containpolynuclear aromatic compounds, some of which are carcinogens. These compounds, when present, are so strongly bound to thecarbon black that they are biologically inactive. However, they may be removed by extraction with toluene or other appropriatesolvents. Avoid skin contact
22、 with solvent extracts from such carbon blacks.7.2 For most pelleted blacks, the depth of 60 mm in the thimble should provide a sample of 15 to 25 g. Unpelleted blacks shouldbe predensified sufficiently that this depth will require a sample of at least 10 g.7.3 Do not use joint lubricant on the grou
23、nd joints. To minimize vapor loss by leakage, the joints may be sealed withTFE-fluorocarbon inserts or wrapped with TFE-fluorocarbon laboratory tape.7.4 New thimbles should be washed before use by suction with hot HCl and then rinsed with distilled or deionized water toremove loose particles of fore
24、ign matter such as dust. Thimbles are conveniently cleaned by back washing under suction withappropriate media (water, acetone, etc.). If the fritted disc becomes fouled with carbon black, it may be necessary to burn it outby slowly heating the thimble from room temperature to 500C in a muffle furna
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