ASTM D4527-99(2016)

Standard Test Method for Carbon Black—Solvent Extractables

SIGNIFICANCE AND USE
4.1 The carbon black extract test procedure provides a uniform and precise method for the gravimetric determination of organic-solvent extractables 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. The actual chemical composition of the extract can vary significantly with the type and origin of the carbon black.
SCOPE
1.1 This test method covers the procedure for measuring carbon black solvent extractables.  
1.1.1 This test method determines the total material extracted from carbon black by toluene under specified conditions. The procedure 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 does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. For a specific precautionary statement, see Section 7.

General Information

• Status: Historical
• Publication Date: 31-May-2016
• ICS: 83.040.20 - Rubber compounding ingredients
• Technical Committee: D24 - Carbon Black
• Drafting Committee: D24.31 - Non-Carbon Black Components of Carbon Black

Relations

• Replaces: ASTM D4527-99(2011) - Standard Test Method for Carbon Black<char: emdash>Solvent Extractables
• Effective Date: 01-Jun-2016

Standards Content (Sample)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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 2016)
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
procedure. The actual chemical composition of the extract can
1.2 The values stated in SI units are to be regarded as
vary significantly with the type and origin of the carbon black.
standard. No other units of measurement are included in this
standard.
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
3 4
responsibility of the user of this standard to establish appro-
ground joints, 40 mm I.D. extraction tube, and 250-cm flask.
priate safety and health practices and determine the applica-
5.2 Extraction Thimble, glass, 35-mm diameter by 90-mm
bility of regulatory limitations prior to use. For a specific
height, with coarse porosity fritted disc. When filled with 50
precautionary statement, see Section 7.
3 3
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,forextractionflask,withadjustableheatinput.A
2.1 ASTM Standards:
hot plate extraction heater or hemispherical heating mantle is
D3051 Practice for Carbon Black—Stating the Precision of
preferred.
ASTM Test Methods (Withdrawn 1990)
D3396 PracticeforCarbonBlack—MeasuringthePrecision
5.4 Filter Funnel, glass fritted disc type, with medium
of ASTM Test Methods (Withdrawn 1990)
porosity fritted disc.
5.5 Filter Flask, 125 or 250 cm .
3. Summary of Test Method
3.1 A specimen of carbon black is extracted for 48 h (or 5.6 WaterBath, or other suitable warming means for evapo-
other specified time) in a Soxhlet extractor, the solvent re-
rating solvent from extract at a controlled temperature of 40 to
moved by controlled temperature evaporation, and the ex- 50°C.
tracted residue determined gravimetrically. If the carbon black
5.7 Container, suitable for final solvent removal and weigh-
extractables are to be subjected to additional analysis, see
ing of residue.Alightweight aluminum dish 63 by 17.5 mm, a
Section 7.
3 6
TFE-fluorocarbon cup or a 50-cm glass beaker is suggested.
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
CurrenteditionapprovedJune1,2016.PublishedJuly2016.Originallyapproved K-586100 (glass jacketed) available from Kontas Glass Co., 8000 Spruce St.,
in 1985. Last previous edition approved in 2011 as D4527 – 99 (2011). DOI: Vineland, NJ 08360, simplifies insulating the apparatus and reduces the possibility
10.1520/D4527-99R16. of breakage.
2 5
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 [e-mail]. 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
The last approved version of this historical standard is referenced on Corp., Cahn Division, 16707 S. Carmenita Rd., Cerritos, CA 90701, have been
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 (2016)
5.8 Vacuum Oven, gravity-convection type, capable of tem- of carbon black. If this is not feasible, the glassware must be
perature regulation within 61°C at 125°C and temperature extracted before use in accordance with 7.6.
uniformity within 65°C.
7.6 New glassware, including thimbles, must be extracted,
5.9 Oven, gravity-convection type, capable of temperature
repeatedly if necessary, with toluene or other solvent until the
regulation within 61°C at 125°C and temperature uniformity
blank is acceptable (preferably less than 0.3 mg/150 cm
within 65°C.
solvent).
5.10 Desiccator.
7.7 Two or three glass beads may be added to the extraction
flask to promote smooth boiling. Do not use porous boiling
5.11 Analytical Balance, with a sensitivity of 60.1 mg.
chips.
6. Reagents and Materials
7.8 An extraction must be discarded if there is any visible
6.1 Toluene, having a residue after evaporation less than 10
carbon black in the extraction flask or if the thimble does not
ppm (preferably less than 2 ppm).
drain properly and overflows at any time during the extraction.
6.2 Nitrogen.
7.9 The nitrogen should be delivered through a glass or
metal tip. Do not allow plastic or rubber to contact the solvent.
6.3 Glass wool, extracted with toluene, air-dried, followed
by drying in a convection oven at 125°C for 1 h. Store in a
7.10 To protect from dust, a loose cover over the evapora-
closed container until ready to use.
tion vessel is recommended.
6.4 Aluminum Foil.
7.11 Solvent evaporation may be conducted in a vacuum
evaporator, if available.
7. Precautions
7.12 Any further analysis of the extracted material typically
7.1 For safety reasons, conduct the extraction and solvent
requires that it be in solution. Complete re-solution of the dry
evaporation in an approved fume hood. Carbon blacks may
extract may be difficult or impossible. Therefore, if further
contain polynuclear aromatic compounds, some of which are
analysis is to be performed, an additional sample of the carbon
carcinogens. These compounds, when present, are so strongly
black should be extracted and solvent removal carried only to
bound to the carbon black that they are biologically inactive.
the desired reduced volume. It is recommended that exposure
However, they may be removed by extraction with toluene or
to strong light, especially sunlight, be avoided during extrac-
other appropriate solvents. Avoid skin contact with solvent
tion and subsequent handling, and that the extract be blanketed
extracts from such carbon blacks.
with inert gas (nitrogen) if retained for any length of time.
7.2 For most pellete
...

This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Because
it 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 current version
of the standard as published by ASTM is to be considered the official document.
Designation: D4527 − 99 (Reapproved 2011) D4527 − 99 (Reapproved 2016)
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
1.1 This test method covers the procedure for measuring carbon black solvent extractables.
1.1.1 This test method determines the total material extracted from carbon black by toluene under specified conditions. The
procedure 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 does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility
of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory
limitations prior to use. For a specific precautionary statement, see Section 7.
2. Referenced Documents
2.1 ASTM Standards:
D3051 Practice for Carbon Black—Stating the Precision of ASTM Test Methods (Withdrawn 1990)
D3396 Practice for Carbon Black— Measuring the Precision of ASTM Test Methods (Withdrawn 1990)
3. Summary of Test Method
3.1 A specimen of carbon black is extracted for 48 h (or other specified time) in a Soxhlet extractor, the solvent removed by
controlled temperature evaporation, and the extracted residue determined gravimetrically. If the carbon black extractables are to
be subjected to additional analysis, see Section 7.
4. Significance and Use
4.1 The carbon black extract test procedure provides a uniform and precise method for the gravimetric determination of
organic-solvent extractables 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. The
actual chemical composition of the extract can vary significantly with the type and origin of the carbon black.
5. Apparatus
3 4
5.1 Soxhlet Extraction Apparatus, with interchangeable ground joints, 40 mm I.D. extraction tube, and 250-cm flask.
5 3
5.2 Extraction Thimble, glass, 35-mm diameter by 90-mm height, with coarse porosity fritted disc. When filled with 50 cm
of toluene, drainage time for the first 40 cm should not exceed 95 s. Discard thimbles taking longer.
5.3 Heater, for extraction flask, with adjustable heat input. A hot plate extraction heater or hemispherical heating mantle is
preferred.
5.4 Filter Funnel, glass fritted disc type, with medium porosity fritted disc.
5.5 Filter Flask, 125 or 250 cm .
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 Black
Components of Carbon Black.
Current edition approved May 1, 2011June 1, 2016. Published July 2011July 2016. Originally approved in 1985. Last previous edition approved in 20042011 as D4527 – 99
(2004).(2011). DOI: 10.1520/D4527-99R11. 10.1520/D4527-99R16.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
The last approved version of this historical standard is referenced on www.astm.org.
Fisher Scientific No. 9-556B available from Fisher Scientific Co., 203 Fisher Ave., Pittsburgh, PA 15219, has been found satisfactory. The use of Kontas 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.
Fisher Scientific 9-653B available from Fisher Scientific Co., has been found satisfactory.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D4527 − 99 (2016)
5.6 Water Bath, or other suitable warming means for evaporating solvent from extract at a controlled temperature of 40 to 50°C.
5.7 Container, suitable for final solvent removal and weighing of residue. A lightweight aluminum dish 63 by 17.5 mm, a
3 6
TFE-fluorocarbon cup or a 50-cm glass beaker is suggested.
5.8 Vacuum Oven, gravity-convection type, capable of temperature regulation within 61°C at 125°C and temperature
uniformity within 65°C.
5.9 Oven, gravity-convection type, capable of temperature regulation within 61°C at 125°C and temperature uniformity within
65°C.
5.10 Desiccator.
5.11 Analytical Balance, with a sensitivity of 60.1 mg.
6. Reagents and Materials
6.1 Toluene, having a residue after evaporation less than 10 ppm (preferably less than 2 ppm).
6.2 Nitrogen.
6.3 Glass wool, extracted with toluene, air-dried, followed by drying in a convection oven at 125°C for 1 h. Store in a closed
container until ready to use.
6.4 Aluminum Foil.
7. Precautions
7.1 For safety reasons, conduct the extraction and solvent evaporation in an approved fume hood. Carbon blacks may contain
polynuclear aromatic compounds, some of which are carcinogens. These compounds, when present, are so strongly bound to the
carbon black that they are biologically inactive. However, they may be removed by extraction with toluene or other appropriate
solvents. Avoid skin contact 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 should
be predensified sufficiently that this depth will require a sample of at least 10 g.
7.3 Do not use joint lubricant on the ground joints. To minimize vapor loss by leakage, the joints may be sealed with
TFE-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 to
remove loose particles of foreign matter such as dust. Thimbles are conveniently cleaned by back washing under suction with
appropriate media (water, acetone, etc.). If the fritted disc becomes fouled with carbon black, it may be necessary to burn it out
by slowly heating the thimble from room temperature to 500°C in a muffle furnace. One hour is usually sufficient. The use of
chromic acid cleaning solution is not recommended. The permeability of the clean thimble should be checked periodically. Discard
thimbles with drainage times exceeding the 95 s specified under 5.2.
7.5 To prevent contamination, it is recommended that all glassware used in this procedure be reserved for the extraction of
carbon black. If this is not feasible, the glassware must be extracted 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 the blank
is acceptable (preferably less than 0.3 mg/150 cm solvent).
7.7 Two or three glass beads may be added to the extraction flask to promote smooth boili
...