ASTM D6556-09

Standard Test Method for Carbon Black-Total and External Surface Area by Nitrogen Adsorption

SIGNIFICANCE AND USE
This test method is used to measure the total and external surface area of carbon blacks based on multipoint nitrogen adsorption. The NSA measurement is based on the B.E.T. theory and it includes the total surface area, inclusive of micropores, pore diameters less than 2 nm (20 Å). The external surface area, based on the statistical thickness method (STSA), is defined as the specific surface area that is accessible to rubber.
CTAB Surface Area (formerly Test Method D 3765) has been withdrawn. The CTAB value may be estimated from the STSA value using Eq 1. The equation is based on a linear regression of the STSA and CTAB measured values of the SRB 5 standards.
SCOPE
1.1 This test method covers the determination of the total surface area by the Brunauer, Emmett, and Teller (B.E.T. NSA) theory of multilayer gas adsorption behavior using multipoint determinations and the external surface area based on the statistical thickness surface area method.
1.2 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.
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. (The minimum safety equipment should include protective gloves, sturdy eye and face protection).

General Information

• Status: Historical
• Publication Date: 14-Feb-2009
• ICS: 71.060.10 - Chemical elements
• Technical Committee: D24 - Carbon Black
• Drafting Committee: D24.21 - Carbon Black Surface Area and Related Properties

Relations

• Replaces: ASTM D6556-07 - Standard Test Method for Carbon Black-Total and External Surface Area by Nitrogen Adsorption
• Effective Date: 15-Feb-2009
• Replaced By: ASTM D6556-10 - Standard Test Method for Carbon Black-Total and External Surface Area by Nitrogen Adsorption
• Effective Date: 01-Aug-2010
• Referred By: ASTM D3849-22 - Standard Test Method for Carbon Black—Morphological Characterization of Carbon Black Using Electron Microscopy
• Effective Date: 15-Feb-2009
• Referred By: ASTM D7849-23 - Standard Classification for Nomenclature of Reference Materials of Committee D24
• Effective Date: 15-Feb-2009
• Referred By: ASTM D6915-23 - Standard Practice for Carbon Black—Evaluation of Standard Reference Blacks
• Effective Date: 15-Feb-2009
• Referred By: ASTM D8325-20 - Standard Guide for Evaluation of Nuclear Graphite Surface Area and Porosity by Gas Adsorption Measurements
• Effective Date: 15-Feb-2009
• Referred By: ASTM D4821-20 - Standard Guide for Carbon Black—Validation of Test Method Precision and Bias
• Effective Date: 15-Feb-2009
• Referred By: ASTM D3053-23 - Standard Terminology Relating to Carbon Black
• Effective Date: 15-Feb-2009
• Referred By: ASTM D1765-23a - Standard Classification System for Carbon Blacks Used in Rubber Products
• Effective Date: 15-Feb-2009
• Referred By: ASTM D4122-17(2023) - Standard Practice for Carbon Black—Evaluation of an Industry Reference Black
• Effective Date: 15-Feb-2009
• Referred By: ASTM D5817-20 - Standard Practice for Carbon Black, Pelleted—Reduction, Blending, and Drying of Gross Samples for Testing
• Effective Date: 15-Feb-2009

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:D6556–09
Standard Test Method for
Carbon Black—Total and External Surface Area by Nitrogen
1
Adsorption
This standard is issued under the fixed designation D6556; 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 temperature, by a carbon black at several partial pressures of
nitrogen. The adsorption data is used to calculate the NSAand
1.1 This test method covers the determination of the total
STSA values.
surfaceareabytheBrunauer,Emmett,andTeller(B.E.T.NSA)
theory of multilayer gas adsorption behavior using multipoint
4. Significance and Use
determinations and the external surface area based on the
4.1 This test method is used to measure the total and
statistical thickness surface area method.
external surface area of carbon blacks based on multipoint
1.2 The values stated in SI units are to be regarded as the
nitrogen adsorption. The NSA measurement is based on the
standard. The values given in parentheses are for information
B.E.T. theory and it includes the total surface area, inclusive of
only.
micropores, pore diameters less than 2 nm (20 Å).The external
1.3 This standard does not purport to address all of the
surface area, based on the statistical thickness method (STSA),
safety concerns, if any, associated with its use. It is the
is defined as the specific surface area that is accessible to
responsibility of the user of this standard to establish appro-
rubber.
priate safety and health practices and determine the applica-
4.2 CTAB SurfaceArea (formerly Test Method D3765) has
bility of regulatory limitations prior to use. (The minimum
been withdrawn. The CTAB value may be estimated from the
safety equipment should include protective gloves, sturdy eye
STSA value using Eq 1. The equation is based on a linear
and face protection).
regressionoftheSTSAandCTABmeasuredvaluesoftheSRB
2. Referenced Documents 5 standards.
2
2.1 ASTM Standards: CTAB 5STSA * 1.0170 1 2.6434 (1)
D1799 Practice for Carbon Black—Sampling Packaged
5. Apparatus
Shipments
D1900 Practice for Carbon Black—Sampling Bulk Ship- 5.1 MultipointStatic-VolumetricGasAdsorptionApparatus,
ments with Dewar flasks and all other accessories required for
D3765 Test Method for Carbon Black—CTAB (Cetyltrim- operation.
3
ethylammonium Bromide) Surface Area 5.2 Sample Cells, that when attached to the adsorption
D4483 Practice for Evaluating Precision for Test Method apparatus, will maintain isolation of the sample from the
–5 3
Standards in the Rubber and Carbon Black Manufacturing atmosphere equivalent to a helium leak rate of <10 cm /min,
Industries per atmosphere of pressure difference.
5.3 Balance, Analytical, with 0.1 mg sensitivity.
3. Summary of Test Method
5.4 Heating Mantle or Equivalent, capable of maintaining a
3.1 The total and external surface areas are measured by temperature of 300 6 10°C.
evaluating the amount of nitrogen adsorbed, at liquid nitrogen
5.5 Oven, Gravity Convection, capable of maintaining a
temperature of 125 6 10°C.
1
This test method is under the jurisdiction ofASTM Committee D24 on Carbon
6. Reagents
Black and is the direct responsibility of Subcommittee D24.21 on Carbon Black
6.1 Liquid Nitrogen, 98 % or higher purity.
Surface Area and Related Properties.
Current edition approved Feb. 15, 2009. Published March 2009. Originally
6.2 Ultra-High Purity Nitrogen Gas, cylinder or other
approved in 2000. Last previous edition approved in 2007 as D6556 – 07. DOI:
source of prepurified nitrogen gas.
10.1520/D6556-09.
2
6.3 Ultra-High Purity Helium Gas, cylinder or other source
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM of prepurified helium gas.
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website.
3
Withdrawn. The last approved version of this historical standard is referenced
on www.astm.org.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
1

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D6556–09
7. Sampling 8.5.5 Go directly to Section 9 and continue the remaining
steps of the procedure.
7.1 Samples may be taken in accordance with Practices
D1799 and D1900.
9. Measurement Procedure
8. Sample Preparation Procedure
9.1 Refertotheuser’smanualorspecificinstructionsforthe
8.1 Dry a portion of carbon black at 125°C for 1 h. If the
multipoint gas adsorption analyzer to be used, and become
carbon black is known to be substantially free of moisture, or
thoroughly familiar with the procedures
...

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:D6556–07 Designation:D6556–09
Standard Test Method for
Carbon Black—Total and External Surface Area by Nitrogen
1
Adsorption
This standard is issued under the fixed designation D 6556; 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 ThistestmethodcoversthedeterminationofthetotalsurfaceareabytheBrunauer,Emmett,andTeller(B.E.T.NSA)theory
of multilayer gas adsorption behavior using multipoint determinations and the external surface area based on the statistical
thickness surface area method.
1.2 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.
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. (The minimum safety equipment should include protective gloves, sturdy eye and face protection).
2. Referenced Documents
2
2.1 ASTM Standards:
D 1799 Practice for Carbon BlackSampling Packaged Shipments
D 1900 Practice for Carbon BlackSampling Bulk Shipments
D 3765 Test Method for Carbon BlackCTAB (Cetyltrimethylammonium Bromide) Surface Area
D 4483 Practice for Evaluating Precision for Test Method Standards in the Rubber and Carbon Black Manufacturing Industries
3. Summary of Test Method
3.1 The total and external surface areas are measured by evaluating the amount of nitrogen adsorbed, at liquid nitrogen
temperature, by a carbon black at several partial pressures of nitrogen.The adsorption data is used to calculate the NSAand STSA
values.
4. Significance and Use
4.1 This test method is used to measure the total and external surface area of carbon blacks based on multipoint nitrogen
adsorption. The NSA measurement is based on the B.E.T. theory and it includes the total surface area, inclusive of micropores,
pore diameters less than 2 nm (20 Å). The external surface area, based on the statistical thickness method (STSA), is defined as
the specific surface area that is accessible to rubber.
4.2 CTAB Surface Area (formerly Test Method D 3765) has been withdrawn. The CTAB value may be estimated from the
STSA value using Eq 1. The equation is based on a linear regression of the STSA and CTAB measured values of the SRB 5
standards.
CTAB 5STSA * 1.0170 1 2.6434 (1)
5. Apparatus
5.1 Multipoint Static-Volumetric GasAdsorptionApparatus, with Dewar flasks and all other accessories required for operation.
5.2 Sample Cells, that when attached to the adsorption apparatus, will maintain isolation of the sample from the atmosphere
–5 3
equivalent to a helium leak rate of <10 cm /min, per atmosphere of pressure difference.
5.3 Balance, Analytical, with 0.1 mg sensitivity.
5.4 Heating Mantle or Equivalent, capable of maintaining a temperature of 300 6 10°C.
5.5 Oven, Gravity Convection, capable of maintaining a temperature of 125 6 10°C.
1
This test method is under the jurisdiction ofASTM Committee D24 on Carbon Black and is the direct responsibility of Subcommittee D24.21 on Carbon Black Surface
Area and Related Properties.
Current edition approved Oct. 1, 2007. Published November 2007. Originally approved in 2000. Last previous edition approved in 2004 as D6556–04.
Current edition approved Feb. 15, 2009. Published March 2009. Originally approved in 2000. Last previous edition approved in 2007 as D 6556 – 07.
2
For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at [e-mail]. ForAnnualBookofASTMStandards
volume information, refer to the standard’s Document Summary page on the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
1

---------------------- Page: 1 ----------------------
D6556–09
6. Reagents
6.1 Liquid Nitrogen, 98 % or higher purity.
6.2 Ultra-High Purity Nitrogen Gas, cylinder or other source of prepurified nitrogen gas.
6.3 Ultra-High Purity Helium Gas, cylinder or other source of prepurified helium gas.
7. Sampling
7.1 Samples may be taken in accordance with Practices D 1799 and D 1900.
8. Sample Preparation Procedure
8.1 Dry a portion of carbon black at 125°C for 1 h. If the carbon
...