ASTM D4527-99

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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Designation: D 4527 – 99
Standard Test Method for
Carbon Black—Solvent Extractables
This standard is issued under the fixed designation D 4527; 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 (e) indicates an editorial change since the last revision or reapproval.
1. Scope precision are acceptable for most specification or regulatory
purposes, or both. However, carbon black with very low extract
1.1 This test method covers the procedure for measuring
(less than 0.02 %) may require a more rigorous extraction
carbon black solvent extractables.
procedure. The actual chemical composition of the extract can
1.1.1 This test method determines the total material ex-
vary significantly with the type and origin of the carbon black.
tracted from carbon black by toluene under specified condi-
tions. The procedure is also applicable to other solvents such as
5. Apparatus
cyclohexane, etc.
5.1 Soxhlet Extraction Apparatus, with interchangeable
1.2 The values stated in SI units are to be regarded as the
ground joints, 40 mm I.D. extraction tube, and 250-cm flask.
standard. The values given in parentheses are for information
5.2 Extraction Thimble, glass, 35 mm diameter by 90 mm
only.
height, with coarse porosity fritted disc. When filled with 50
1.3 This standard does not purport to address all of the
3 3
cm of toluene, drainage time for the first 40 cm should not
safety concerns, if any, associated with its use. It is the
exceed 95 s. Discard thimbles taking longer.
responsibility of the user of this standard to establish appro-
5.3 Heater, for extraction flask, with adjustable heat input.
priate safety and health practices and determine the applica-
A hot plate extraction heater or hemispherical heating mantle is
bility of regulatory limitations prior to use. For a specific
preferred.
precautionary statement, see Section 7.
5.4 Filter Funnel, glass fritted disc type, with medium
2. Referenced Documents porosity fritted disc.
5.5 Filter Flask, 125 or 250 cm .
2.1 ASTM Standards:
5.6 Water Bath, or other suitable warming means for evapo-
D 3051 Practice for Carbon Black—Stating the Precision of
rating solvent from extract at a controlled temperature of 40 to
ASTM Test Methods
50°C.
D 3396 Practice for Carbon Black—Measuring the Preci-
5.7 Container, suitable for final solvent removal and weigh-
sion of ASTM Test Methods
ing of residue. A light weight aluminum dish 63 by 17.5 mm,
3 5
3. Summary of Test Method
a TFE-fluorocarbon cup or a 50-cm glass beaker is suggested.
5.8 Vacuum Oven, gravity-convection type, capable of tem-
3.1 A specimen of carbon black is extracted for 48 h (or
perature regulation within 61°C at 125°C and temperature
other specified time) in a Soxhlet extractor, the solvent re-
uniformity within 65°C.
moved by controlled temperature evaporation, and the ex-
5.9 Oven, gravity-convection type, capable of temperature
tracted residue determined gravimetrically. If the carbon black
regulation within 61°C at 125°C and temperature uniformity
extractables are to be subjected to additional analysis, see
within 65°C.
Section 7.
5.10 Desiccator.
4. Significance and Use
4.1 The carbon black extract test procedure provides a
Fisher Scientific No. 9-556B available from Fisher Scientific Co., 203 Fisher
uniform and precise method for the gravimetric determination
Ave., Pittsburgh, PA 15219, has been found satisfactory. The use of Kontas
of organic-solvent extractables on carbon black. Accuracy and
K-586100 (glass jacketed) available from Kontas Glass Co., 8000 Spruce St.,
Vineland, NJ 08360, simplifies insulating the apparatus and reduces the possibility
of breakage.
1 4
This test method is under the jurisdiction of ASTM Committee D-24 on Carbon Fisher Scientific 9-653B available from Fisher Scientific Co., has been found
Black and is the direct responsibility of Subcommittee D24.31 on Non-Carbon satisfactory.
Black Components of Carbon Black. Fisher Scientific No. 8-732-5C (aluminum dish) available from Fisher Scien-
Current edition approved May 10, 1999. Published June 1999. Originally tific Co., and Ventron No. 2034 (teflon cup) available from Ventron Instrument
published as D 4527 – 85. Last previous edition D 4527 – 93a (1998). Corp., Cahn Division, 16707 S. Carmenita Rd., Cerritos, CA 90701, have been
Annual Book of ASTM Standards, Vol 09.01. found to be satisfactory.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D 4527
5.11 Analytical Balance, with a sensitivity of 60.1 mg. 7.8 An extraction must be discarded if there is any visible
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
6.1 Toluene, having a residue after evaporation less than 10
metal tip. Do not allow plastic or rubber to contact the solvent.
ppm (preferably less than 2 ppm).
7.10 To protect from dust, a loose cover over the evapora-
6.2 Nitrogen.
tion vessel is recommended.
6.3 Glass wool, extracted with toluene, air-dried, followed
7.11 Solvent evaporation may be conducted in a vacuum
by drying in a convection oven at 125°C for 1 h. Store in a
evaporator, if available.
closed container until ready to use.
7.12 Any further analysis of the extracted material typically
6.4 Aluminum Foil.
requires that it be in solution. Complete re-solution of the dry
extract may be difficult or impossible. Therefore, if further
7. Precautions
analysis is to be performed, an additional sample of the carbon
7.1 For safety reasons, conduct the extraction and solvent
black should be extracted and solvent removal carried only to
evaporation in an approved fume hood. Carbon blacks may
the desired reduced volume. It is recommended that exposure
contain polynuclear aromatic compounds, some of which are
to strong light, especially sunlight, be avoided during extrac-
carcinogens. These compounds, when present, are so strongly
tion and subsequent handling, and that the extract be blanketed
bound to the carbon black that they are biologically inactive.
with inert gas (nitrogen) if retained for any length of time.
However, they may be removed by extraction with toluene or
7.13 It has been found that there may be significant varia-
other appropriate solvents. Avoid skin contact with solvent
tion in the amount of residue found in different bottles of
extracts from such carbon blacks.
toluene bearing the same lot number. Consequently, blanks
7.2 For most pelleted blacks, the depth of 60 mm in the
should be run on each bottle.
thimble should provide a sample of 15 to 25 g. Unpelleted
blacks should be predensified sufficiently that this depth
...