ASTM D4527-99(2004)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
Designation:D4527–99 (Reapproved 2004)
Standard Test Method for
Carbon Black—Solvent Extractables
This standard is issued under the fixed designation D4527; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope 4. Significance and Use
1.1 This test method covers the procedure for measuring 4.1 The carbon black extract test procedure provides a
carbon black solvent extractables. uniform and precise method for the gravimetric determination
1.1.1 This test method determines the total material ex- of organic-solvent extractables on carbon black.Accuracy and
tracted from carbon black by toluene under specified condi- precision are acceptable for most specification or regulatory
tions.Theprocedureisalsoapplicabletoothersolventssuchas purposes,orboth.However,carbonblackwithverylowextract
cyclohexane, etc. (less than 0.02 %) may require a more rigorous extraction
1.2 The values stated in SI units are to be regarded as the procedure. The actual chemical composition of the extract can
standard. The values given in parentheses are for information vary significantly with the type and origin of the carbon black.
only.
5. Apparatus
1.3 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the 5.1 Soxhlet Extraction Apparatus, with interchangeable
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ground joints, 40 mm I.D. extraction tube, and 250-cm flask.
responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica- 5.2 Extraction Thimble, glass, 35-mm diameter by 90-mm
height, with coarse porosity fritted disc. When filled with 50
bility of regulatory limitations prior to use. For a specific
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precautionary statement, see Section 7. cm of toluene, drainage time for the first 40 cm should not
exceed 95 s. Discard thimbles taking longer.
2. Referenced Documents
5.3 Heater, for extraction flask, with adjustable heat input.
2.1 ASTM Standards: Ahotplateextractionheaterorhemisphericalheatingmantleis
D3051 Recommended Practice for Carbon Black—Stating preferred.
the Precision of ASTM Test Methods 5.4 Filter Funnel, glass fritted disc type, with medium
D3396 Recommended Practice for Carbon Black— porosity fritted disc.
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Measuring the Precision of ASTM Test Methods 5.5 Filter Flask, 125 or 250 cm .
5.6 WaterBath, or other suitable warming means for evapo-
3. Summary of Test Method
rating solvent from extract at a controlled temperature of 40 to
3.1 A specimen of carbon black is extracted for 48 h (or 50°C.
other specified time) in a Soxhlet extractor, the solvent re-
5.7 Container, suitable for final solvent removal and weigh-
moved by controlled temperature evaporation, and the ex- ing of residue.Alightweight aluminum dish 63 by 17.5 mm, a
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tracted residue determined gravimetrically. If the carbon black
TFE-fluorocarbon cup or a 50-cm glass beaker is suggested.
extractables are to be subjected to additional analysis, see 5.8 Vacuum Oven, gravity-convection type, capable of tem-
Section 7.
perature regulation within 61°C at 125°C and temperature
uniformity within 65°C.
This test method is under the jurisdiction ofASTM Committee D24 on Carbon
Black and is the direct responsibility of Subcommittee D24.31 on Non-Carbon Fisher Scientific No. 9-556B available from Fisher Scientific Co., 203 Fisher
Black Components of Carbon Black. Ave., Pittsburgh, PA 15219, has been found satisfactory. The use of Kontas
Current edition approved July 1, 2004. Published July 2004. Originally approved K-586100 (glass jacketed) available from Kontas Glass Co., 8000 Spruce St.,
in 1985. Last previous edition approved in 1999 as D4527 – 99. DOI: 10.1520/ Vineland, NJ 08360, simplifies insulating the apparatus and reduces the possibility
D4527-99R04. of breakage.
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For referenced ASTM standards, visit the ASTM website, www.astm.org, or Fisher Scientific 9-653B available from Fisher Scientific Co., has been found
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM satisfactory.
Standards volume information, refer to the standard’s Document Summary page on Fisher Scientific No. 8-732-5C (aluminum dish) available from Fisher Scien-
the ASTM website. tific Co., and Ventron No. 2034 (teflon cup) available from Ventron Instrument
Withdrawn. The last approved version of this historical standard is referenced Corp., Cahn Division, 16707 S. Carmenita Rd., Cerritos, CA 90701, have been
on www.astm.org. found to be satisfactory.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D4527–99 (2004)
5.9 Oven, gravity-convection type, capable of temperature 7.7 Two or three glass beads may be added to the extraction
regulation within 61°C at 125°C and temperature uniformity flask to promote smooth boiling. Do not use porous boiling
within 65°C. chips.
5.10 Desiccator. 7.8 An extraction must be discarded if there is any visible
5.11 Analytical Balance, with a sensitivity of 60.1 mg. carbon black in the extraction flask or if the thimble does not
drain properly and overflows at any time during the extraction.
6. Reagents and Materials 7.9 The nitrogen should be delivered through a glass or
metal tip. Do not allow plastic or rubber to contact the solvent.
6.1 Toluene, having a residue after evaporation less than 10
7.10 To protect from dust, a loose cover over the evapora-
ppm (preferably less than 2 ppm).
tion vessel is recommended.
6.2 Nitrogen.
7.11 Solvent evaporation may be conducted in a vacuum
6.3 Glass wool, extracted with toluene, air-dried, followed
evaporator, if available.
by drying in a convection oven at 125°C for 1 h. Store in a
7.12 Any further analysis of the extracted material typically
closed container until ready to use.
requires that it be in solution. Complete re-solution of the dry
6.4 Aluminum Foil.
extract may be difficult or impossible. Therefore, if further
analysis is to be performed, an additional sample of the carbon
7. Precautions
black should be extracted and solvent removal carried only to
7.1 For safety reasons, conduct the extraction and solvent
the desired reduced volume. It is recommended that exposure
evaporation in an approved fume hood. Carbon blacks may
to strong light, especially sunlight, be avoided during extrac-
contain polynuclear aromatic compounds, some of which are
tion and subsequent handling, and that the extract be blanketed
carcinogens. These compounds, when present, are so strongly
with inert gas (nitrogen) if retained for any length of time.
bound to the carbon black that they are biologically inactive.
7.13 It has been found that there may be significant varia-
However, they may be removed by extraction with toluene or
tion in the amount of residue found in different bottles of
other appropriate solvents. Avoid skin contact with solvent
toluene bearing the same lot number. Consequently, blanks
extracts from such carbon blacks.
should be run on each bottle.
7.2 For most pelleted blacks, the depth of 60 mm in the
thimble should
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