ASTM D4527-18

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, health, and environmental practices and determine the applicability of regulatory limitations prior to use. For a specific precautionary statement, see Section 7.  
1.4 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

General Information

• Status: Historical
• Publication Date: 31-May-2018
• ICS: 83.040.20 - Rubber compounding ingredients
• Technical Committee: D24 - Carbon Black
• Drafting Committee: D24.31 - Non-Carbon Black Components of Carbon Black

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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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 − 18
Standard Test Method for
1
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 3. Summary of Test Method
1.1 This test method covers the procedure for measuring 3.1 A specimen of carbon black is extracted for 48 h (or
carbon black solvent extractables. other specified time) in a Soxhlet extractor, the solvent re-
1.1.1 This test method determines the total material ex- moved by controlled temperature evaporation, and the ex-
tracted from carbon black by toluene under specified condi- tracted residue determined gravimetrically. If the carbon black
tions. The procedure is also applicable to other solvents such as extractables are to be subjected to additional analysis, see
cyclohexane, etc. Section 7.
1.2 The values stated in SI units are to be regarded as
4. Significance and Use
standard. No other units of measurement are included in this
4.1 The carbon black extract test procedure provides a
standard.
uniform and precise method for the gravimetric determination
1.3 This standard does not purport to address all of the
of organic-solvent extractables on carbon black. Accuracy and
safety concerns, if any, associated with its use. It is the
precision are acceptable for most specification or regulatory
responsibility of the user of this standard to establish appro-
purposes, or both. However, carbon black with very low extract
priate safety, health, and environmental practices and deter-
(less than 0.02 %) may require a more rigorous extraction
mine the applicability of regulatory limitations prior to use.
procedure. The actual chemical composition of the extract can
For a specific precautionary statement, see Section 7.
vary significantly with the type and origin of the carbon black.
1.4 This international standard was developed in accor-
5. Apparatus
dance with internationally recognized principles on standard-
ization established in the Decision on Principles for the
5.1 Soxhlet Extraction Apparatus, with interchangeable
Development of International Standards, Guides and Recom- 3 3
ground joints, 40 mm I.D. extraction tube, and 250-cm flask.
mendations issued by the World Trade Organization Technical
5.2 Extraction Thimble, glass, 35-mm diameter by 90-mm
Barriers to Trade (TBT) Committee.
4
height, with coarse porosity fritted disc. When filled with 50
3 3
cm of toluene, drainage time for the first 40 cm should not
2. Referenced Documents
exceed 95 s. Discard thimbles taking longer.
2
2.1 ASTM Standards:
5.3 Heater, for extraction flask, with adjustable heat input. A
D4483 Practice for Evaluating Precision for Test Method
hot plate extraction heater or hemispherical heating mantle is
Standards in the Rubber and Carbon Black Manufacturing
preferred.
Industries
5.4 Filter Funnel, glass fritted disc type, with medium
porosity fritted disc.
1
3
This test method is under the jurisdiction of ASTM Committee D24 on Carbon
5.5 Filter Flask, 125 or 250 cm .
Black and is the direct responsibility of Subcommittee D24.31 on Non-Carbon
Black Components of Carbon Black.
3
Current edition approved June 1, 2018. Published July 2018. Originally approved Fisher Scientific No. 9-556B available from Fisher Scientific Co., 203 Fisher
in 1985. Last previous edition approved in 2016 as D4527 – 99 (2016). DOI: Ave., Pittsburgh, PA 15219, has been found satisfactory. The use of Kontas
10.1520/D4527-18. K-586100 (glass jacketed) available from Kontas Glass Co., 8000 Spruce St.,
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or Vineland, NJ 08360, simplifies insulating the apparatus and reduces the possibility
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM of breakage.
4
Standards volume information, refer to the standard’s Document Summary page on Fisher Scientific 9-653B available from Fisher Scientific Co., has been found
the ASTM website. satisfactory.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

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D4527 − 18
5.6 Water Bath, or other suitable warming means for evapo- fritted disc becomes fouled with carbon black, it may be
rating solvent from extract at a controlled temperature of 40 to necessary to burn it out by slowly heating the thimble from
50°C. room temperature to 500°C in a muffle furnace. One hour is
usually sufficient. The use of chromic acid cleaning solution is
5.7 Container, suitable for final solvent removal and
...

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 2016) D4527 − 18
Standard Test Method for
1
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 safety, health, and healthenvironmental practices and determine the
applicability of regulatory limitations prior to use. For a specific precautionary statement, see Section 7.
1.4 This international standard was developed in accordance with internationally recognized principles on standardization
established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued
by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
2. Referenced Documents
2
2.1 ASTM Standards:
D3051D4483 Practice for Carbon Black—Stating the Precision of ASTM Test MethodsEvaluating Precision for Test Method
Standards in the Rubber and Carbon Black Manufacturing Industries (Withdrawn 1990)
3
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 3
5.1 Soxhlet Extraction Apparatus, with interchangeable ground joints, 40 mm I.D. extraction tube, and 250-cm flask.
4 3
5.2 Extraction Thimble, glass, 35-mm diameter by 90-mm height, with coarse porosity fritted disc. When filled with 50 cm
3
of toluene, drainage time for the first 40 cm 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 Black
Components of Carbon Black.
Current edition approved June 1, 2016June 1, 2018. Published July 2016July 2018. Originally approved in 1985. Last previous edition approved in 20112016 as
D4527 – 99 (2011).(2016). DOI: 10.1520/D4527-99R16.10.1520/D4527-18.
2
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.
3
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.
4
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
1

---------------------- Page: 1 ----------------------
D4527 − 18
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 f
...