ASTM D6556-03

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

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: 09-Jul-2003
• 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 D6556-02a - Standard Test Method for Carbon Black—Total and External Surface Area by Nitrogen Adsorption
• Effective Date: 10-Jul-2003
• Replaced By: ASTM D6556-04 - Standard Test Method for Carbon Black-Total and External Surface Area by Nitrogen Adsorption
• Effective Date: 01-Nov-2004
• Referred By: ASTM D4122-17(2023) - Standard Practice for Carbon Black—Evaluation of an Industry Reference Black
• Effective Date: 10-Jul-2003
• Referred By: ASTM D7849-23 - Standard Classification for Nomenclature of Reference Materials of Committee D24
• Effective Date: 10-Jul-2003
• Referred By: ASTM D6915-23 - Standard Practice for Carbon Black—Evaluation of Standard Reference Blacks
• Effective Date: 10-Jul-2003
• Referred By: ASTM D8325-20 - Standard Guide for Evaluation of Nuclear Graphite Surface Area and Porosity by Gas Adsorption Measurements
• Effective Date: 10-Jul-2003
• Referred By: ASTM D5817-20 - Standard Practice for Carbon Black, Pelleted—Reduction, Blending, and Drying of Gross Samples for Testing
• Effective Date: 10-Jul-2003
• Referred By: ASTM D4821-20 - Standard Guide for Carbon Black—Validation of Test Method Precision and Bias
• Effective Date: 10-Jul-2003
• Referred By: ASTM D3849-22 - Standard Test Method for Carbon Black—Morphological Characterization of Carbon Black Using Electron Microscopy
• Effective Date: 10-Jul-2003
• Referred By: ASTM D3053-23 - Standard Terminology Relating to Carbon Black
• Effective Date: 10-Jul-2003
• Referred By: ASTM D1765-23a - Standard Classification System for Carbon Blacks Used in Rubber Products
• Effective Date: 10-Jul-2003

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: D 6556 – 03
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 (e) indicates an editorial change since the last revision or reapproval.
1. Scope nitrogen adsorption. The NSA measurement is based on the
B.E.T. theory and it includes the total surface area, inclusive of
1.1 This test method covers the determination of the total
micropores, pore diameters less than 2 nm (20 Å). The external
surface area by the Brunauer, Emmett, and Teller (B.E.T. NSA)
surface area, based on the statistical thickness method (STSA),
theory of multilayer gas adsorption behavior using multipoint
is defined as the specific surface area that is accessible to
determinations and the external surface area based on the
rubber.
statistical thickness surface area method.
1.2 The values stated in SI units are to be regarded as the
5. Apparatus
standard. The values given in parentheses are for information
5.1 Multipoint Static-Volumetric Gas Adsorption Apparatus,
only.
with Dewar flasks and all other accessories required for
1.3 This standard does not purport to address all of the
operation.
safety concerns, if any, associated with its use. It is the
5.2 Sample Cells that, when attached to the adsorption
responsibility of the user of this standard to establish appro-
apparatus, will maintain isolation of the sample from the
priate safety and health practices and determine the applica-
–5 3
atmosphere equivalent to a helium leak rate of <10 cm /min,
bility of regulatory limitations prior to use. (The minimum
per atmosphere of pressure difference.
safety equipment should include protective gloves, sturdy eye
5.3 Balance, Analytical, with 0.1 mg sensitivity.
and face protection).
5.4 Heating Mantle or Equivalent, capable of maintaining a
2. Referenced Documents temperature of 300 6 10°C.
5.5 Oven, Gravity Convection, capable of maintaining a
2.1 ASTM Standards:
temperature of 125 6 10°C.
D 1799 Practice for Carbon Black—Sampling Packaged
2
Shipments
6. Reagents
D 1900 Practice for Carbon Black—Sampling Bulk Ship-
2 6.1 Liquid nitrogen, 98 % or higher purity.
ments
6.2 Ultra-high purity nitrogen gas, cylinder or other source
D 4483 Practice for Determining Precision for Test Method
2 of prepurified nitrogen gas.
Standards in the Rubber and Carbon Black Industries
6.3 Ultra-high purity helium gas, cylinder or other source of
3. Summary of Test Method prepurified helium gas.
3.1 The total and external surface areas are measured by
7. Sampling
evaluating the amount of nitrogen adsorbed, at liquid nitrogen
7.1 Samples may be taken in accordance with Practice
temperature, by a carbon black at several partial pressures of
D 1799 and Practice D 1900.
nitrogen. The adsorption data is used to calculate the NSA and
STSA values.
8. Sample Preparation Procedure
4. Significance and Use 8.1 Dry a portion of carbon black at 125°C for 1 h. If the
carbon black is known to be substantially free of moisture, or
4.1 This test method is used to measure the total and
subsequent preparation steps are known to be adequate for
external surface area of carbon blacks based on multipoint
moisture removal, then this step may be omitted.
8.2 Condition an empty sample cell for a minimum of 10
1
This test method is under the jurisdiction of ASTM Committee D24 on Carbon minutes at the same conditions intended for degassing the
Black and is the direct responsibility of Subcommittee D24.21 on Adsorptive
sample. Weigh the empty sample cell to the nearest 0.1 mg and
Properties of Carbon Black.
record the mass.
Current edition approved July 10, 2003. Published August 2003. Originally
approved in 2000. Last previous edition approved in 2002 as D 6556-02a.
2
Annual Book of ASTM Standards, Vol 09.01.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
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D6556–03
8.3 Weigh approximately 0.4 g of the carbon black into the 9.4 Determine the free space of the sample cell by measure-
sample cell. ment with helium or by calculation using an assumed carbon
3
black density of 1.9 g/cm .
NOTE 1—For carbon black powder samples, add enough carbon black
9.5 Obtain a minimum of five data points evenly spaced in
to give a depth of approximately 2 in. in straight wall sample tubes, or
the 0.1 to 0.5 relative pressure (P/P ) range. For some tread
approximately 0.4 g for bulb-type sample cells.
o
carbon blacks, particularly N100 and N200 series, it is neces-
8.4 Flow Degassing:
sary to me
...