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ASTM D6556-16

(Test Method)

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

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

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4.2 CTAB Surface Area (formerly Test Method D3765) has been withdrawn.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
31-Dec-2015
ICS
71.060.10 - Chemical elements
Technical Committee
D24 - Carbon Black
Drafting Committee
D24.21 - Carbon Black Surface Area and Related Properties
Current Stage
Ref Project

Relations

Replaced By
ASTM D6556-17 - Standard Test Method for Carbon Black—Total and External Surface Area by Nitrogen Adsorption
Effective Date
01-Oct-2017

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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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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 − 16
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.Anumber 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
3.1 The total and external surface areas are measured by
1.1 This test method covers the determination of the total
evaluating the amount of nitrogen adsorbed, at liquid nitrogen
surfaceareabytheBrunauer,Emmett,andTeller(B.E.T.NSA)
temperature, by a carbon black at several partial pressures of
theory of multilayer gas adsorption behavior using multipoint
nitrogen. The adsorption data is used to calculate the NSAand
determinations and the external surface area based on the
STSA values.
statistical thickness surface area method.
1.2 The values stated in SI units are to be regarded as the
4. Significance and Use
standard. The values given in parentheses are for information
4.1 This test method is used to measure the total and
only.
external surface area of carbon blacks based on multipoint
1.3 This standard does not purport to address all of the
nitrogen adsorption. The NSA measurement is based on the
safety concerns, if any, associated with its use. It is the
B.E.T.theoryanditincludesthetotalsurfacearea,inclusiveof
responsibility of the user of this standard to establish appro-
micropores,porediameterslessthan2nm(20Å).Theexternal
priate safety and health practices and determine the applica-
surfacearea,basedonthestatisticalthicknessmethod(STSA),
bility of regulatory limitations prior to use. (The minimum
is defined as the specific surface area that is accessible to
safety equipment should include protective gloves, sturdy eye
rubber.
and face protection).
4.2 CTAB SurfaceArea (formerly Test Method D3765) has
been withdrawn. The CTAB value may be estimated from the
2. Referenced Documents
STSA value using Eq 1. The equation is based on a linear
2
2.1 ASTM Standards:
regressionoftheSTSAandCTABmeasuredvaluesoftheSRB
D1799 Practice for Carbon Black—Sampling Packaged
5 standards.
Shipments
CTAB 5 STSA*1.017012.6434 (1)
D1900Practice for Carbon Black—Sampling Bulk Ship-
ments
5. Apparatus
D3765Test Method for Carbon Black—CTAB (Cetyltrim-
ethylammonium Bromide) Surface Area (Withdrawn 5.1 MultipointStatic-VolumetricGasAdsorptionApparatus,
3
2007) with Dewar flasks and all other accessories required for
D4483Practice for Evaluating Precision for Test Method operation.
StandardsintheRubberandCarbonBlackManufacturing
5.2 Sample Cells, that when attached to the adsorption
Industries
apparatus, will maintain isolation of the sample from the
–5 3
atmosphere equivalent to a helium leak rate of <10 cm /min,
per atmosphere of pressure difference.
1
This test method is under the jurisdiction ofASTM Committee D24 on Carbon
5.3 Balance, Analytical, with 0.1 mg sensitivity.
Black and is the direct responsibility of Subcommittee D24.21 on Carbon Black
Surface Area and Related Properties.
5.4 Heating Mantle or Equivalent, capable of maintaining a
Current edition approved Jan. 1, 2016. Published February 2016. Originally
temperature of 300 6 10°C.
approved in 2000. Last previous edition approved in 2014 as D6556–14. DOI:
10.1520/D6556-16.
5.5 Oven, Gravity Convection, capable of maintaining a
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
temperature of 125 6 10°C.
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website.
6. Reagents
3
The last approved version of this historical standard is referenced on
www.astm.org. 6.1 Liquid Nitrogen, 98% or higher purity.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

---------------------- Page: 1 ----------------------
D6556 − 16
6.2 Ultra-High Purity Nitrogen Gas, cylinder or other 8.5.3 Place a heating mantle or other source of heat around
1
source of prepurified nitrogen gas. the sample cell and degas the sample at 300 6 10°C for ⁄2 h
orlongerasrequiredtoobtainandholdapressurelessthan1.4
6.3 Ultra-High Purity Helium Gas, cylinder or other source
Pa (10 µm Hg).
of prepurified helium gas.
NOTE 3—Attention! One-half hour vacuum degassing may be inad-
equate for some grades and may result in statistically different results to
7. Sampling
flow degassing.
7.1 Samples may be taken in accordance with Practices
8.5.4 Once the typical degassing times have been
D1799 and D1900.
determined, future samples can be degassed on the bas
...

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 − 14 D6556 − 16
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
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).
2. Referenced Documents
2
2.1 ASTM Standards:
D1799 Practice for Carbon Black—Sampling Packaged Shipments
D1900 Practice for Carbon Black—Sampling Bulk Shipments
3
D3765 Test Method for Carbon Black—CTAB (Cetyltrimethylammonium Bromide) Surface Area (Withdrawn 2007)
D4483 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 NSA and 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 D3765) 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 5 STSA*1.017012.6434 (1)
5. Apparatus
5.1 Multipoint Static-Volumetric Gas Adsorption Apparatus, 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.
1
This test method is under the jurisdiction of ASTM 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 June 1, 2014Jan. 1, 2016. Published July 2014February 2016. Originally approved in 2000. Last previous edition approved in 20102014 as
D6556 – 10.D6556 – 14. DOI: 10.1520/D6556-14.10.1520/D6556-16.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
3
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

---------------------- Page: 1 ----------------------
D6556 − 16
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.
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 D1799 and D1900.
8. Sample Preparation Procedure
8.1 Dry a
...

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