ASTM D6556-04

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: 31-Oct-2004
• 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 D6556-03 - Standard Test Method for Carbon Black—Total and External Surface Area by Nitrogen Adsorption
• Effective Date: 01-Nov-2004
• Replaced By: ASTM D6556-07 - Standard Test Method for Carbon Black-Total and External Surface Area by Nitrogen Adsorption
• Effective Date: 01-Oct-2007
• Referred By: ASTM D4122-17(2023) - Standard Practice for Carbon Black—Evaluation of an Industry Reference Black
• Effective Date: 01-Nov-2004
• Referred By: ASTM D3053-23 - Standard Terminology Relating to Carbon Black
• Effective Date: 01-Nov-2004
• Referred By: ASTM D7849-23 - Standard Classification for Nomenclature of Reference Materials of Committee D24
• Effective Date: 01-Nov-2004
• Referred By: ASTM D4821-20 - Standard Guide for Carbon Black—Validation of Test Method Precision and Bias
• Effective Date: 01-Nov-2004
• Referred By: ASTM D1765-23a - Standard Classification System for Carbon Blacks Used in Rubber Products
• Effective Date: 01-Nov-2004
• Referred By: ASTM D8325-20 - Standard Guide for Evaluation of Nuclear Graphite Surface Area and Porosity by Gas Adsorption Measurements
• Effective Date: 01-Nov-2004
• Referred By: ASTM D5817-20 - Standard Practice for Carbon Black, Pelleted—Reduction, Blending, and Drying of Gross Samples for Testing
• Effective Date: 01-Nov-2004
• Referred By: ASTM D6915-23 - Standard Practice for Carbon Black—Evaluation of Standard Reference Blacks
• Effective Date: 01-Nov-2004
• Referred By: ASTM D3849-22 - Standard Test Method for Carbon Black—Morphological Characterization of Carbon Black Using Electron Microscopy
• Effective Date: 01-Nov-2004

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:D6556–04
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 4. Significance and Use
1.1 This test method covers the determination of the total 4.1 This test method is used to measure the total and
surfaceareabytheBrunauer,Emmett,andTeller(B.E.T.NSA) external surface area of carbon blacks based on multipoint
theory of multilayer gas adsorption behavior using multipoint nitrogen adsorption. The NSA measurement is based on the
determinations and the external surface area based on the B.E.T. theory and it includes the total surface area, inclusive of
statistical thickness surface area method. micropores, pore diameters less than 2 nm (20 Å).The external
1.2 The values stated in SI units are to be regarded as the surface area, based on the statistical thickness method (STSA),
standard. The values given in parentheses are for information is defined as the specific surface area that is accessible to
only. rubber.
1.3 This standard does not purport to address all of the
5. Apparatus
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro- 5.1 MultipointStatic-VolumetricGasAdsorptionApparatus,
with Dewar flasks and all other accessories required for
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use. (The minimum operation.
5.2 Sample Cells, that when attached to the adsorption
safety equipment should include protective gloves, sturdy eye
and face protection). apparatus, will maintain isolation of the sample from the
–5 3
atmosphere equivalent to a helium leak rate of <10 cm /min,
2. Referenced Documents
per atmosphere of pressure difference.
2
2.1 ASTM Standards: 5.3 Balance, Analytical, with 0.1 mg sensitivity.
D 1799 Practice for Carbon Black—Sampling Packaged 5.4 Heating Mantle or Equivalent, capable of maintaining a
Shipments temperature of 300 6 10°C.
D 1900 Practice for Carbon Black—Sampling Bulk Ship- 5.5 Oven, Gravity Convection, capable of maintaining a
ments temperature of 125 6 10°C.
D 4483 Practice for Evaluating Precision for Test Method
6. Reagents
Standards in the Rubber and Carbon Black Manufacturing
Industries 6.1 Liquid Nitrogen, 98 % or higher purity.
6.2 Ultra-High Purity Nitrogen Gas, cylinder or other
3. Summary of Test Method
source of prepurified nitrogen gas.
3.1 The total and external surface areas are measured by 6.3 Ultra-High Purity Helium Gas, cylinder or other source
evaluating the amount of nitrogen adsorbed, at liquid nitrogen of prepurified helium gas.
temperature, by a carbon black at several partial pressures of
7. Sampling
nitrogen. The adsorption data is used to calculate the NSAand
STSA values. 7.1 Samples may be taken in accordance with Practices
D 1799 and D 1900.
1
This test method is under the jurisdiction ofASTM Committee D24 on Carbon 8. Sample Preparation Procedure
Black and is the direct responsibility of Subcommittee D24.21 on Carbon Black
8.1 Dry a portion of carbon black at 125°C for 1 h. If the
Surface Area and Related Properties.
carbon black is known to be substantially free of moisture, or
Current edition approved Nov. 1, 2004. Published November 2004. Originally
approved in 2000. Last previous edition approved in 2003 as D 6556-03.
subsequent preparation steps are known to be adequate for
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
moisture removal, then this step may be omitted.
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.
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D6556–04
8.2 Condition an empty sample cell for a minimum of 10 9.2 FilltheDewarwithliquidnitrogen(LN2)andallowitto
min at the same conditions intended for degassing the sample. reach temperature equilibrium. The Dewar should be refilled
Weigh the empty sample cell to the nearest 0.1 mg and record
approximately once per hour or between each analysis. The
the mass. time required to reach equilibrium is dependent upon Dewar
8.3 Weigh approximately 0.4 g of the carbon black into the
size and quality.
sample cell.
9.2.1 Small Dewar (<1 L)—Fill and cover the Dewar for a
minimum of 2 h prior to use.The Dewar should be cleaned
...