ASTM D5816-99

Standard Test Methods for Carbon Black-External Surface Area by Multipoint Nitrogen Adsorption (Withdrawn 2000)

SCOPE
1.1 These test methods cover the determination of the external surface area of carbon blacks by the statistical thickness surface area (STSA) 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.

General Information

• Status: Withdrawn
• Publication Date: 09-Sep-1999
• Technical Committee: D24 - Carbon Black
• Drafting Committee: D24.21 - Carbon Black Surface Area and Related Properties

Standards Content (Sample)

Designation: D 5816 – 99
Standard Test Methods for
Carbon Black—External Surface Area by Multipoint Nitrogen
1
Adsorption
This standard is issued under the fixed designation D 5816; 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 4.3 Analytical Balance, with 0.1 mg sensitivity.
4.4 Heating Mantle or Equivalent, capable of maintaining a
1.1 These test methods cover the determination of the
temperature of 300 6 10°C.
external surface area of carbon blacks by the statistical
4.5 Oven, Gravity Convection, capable of maintaining a
thickness surface area (STSA) method.
temperature of 125 6 5°C.
1.2 The values stated in SI units are to be regarded as the
standard. The values given in parentheses are for information
5. Reagents
only.
5.1 Liquid nitrogen, 98 % or higher purity.
1.3 This standard does not purport to address all of the
5.2 Ultra high-purity nitrogen gas, cylinder, or other source
safety concerns, if any, associated with its use. It is the
of prepurified nitrogen gas.
responsibility of the user of this standard to establish appro-
5.3 Ultra high-purity helium gas, cylinder, or other source
priate safety and health practices and determine the applica-
of prepurified helium gas.
bility of regulatory limitations prior to use.
6. Sampling
2. Referenced Documents
6.1 Samples shall be taken in accordance with Practice
2.1 ASTM Standards:
D 1799 and Practice D 1900.
D 1799 Practice for Carbon Black—Sampling Packaged
2
Shipments
7. Sample Preparation Procedure
D 1900 Practice for Carbon Black—Sampling Bulk Ship-
7.1 Dry a portion of the carbon black to be tested at 125°C
2
ments
for 1 h. If the carbon black is known to be substantially free of
D 4820 Test Methods for Carbon Black—Surface Area by
2 moisture, or subsequent preparation steps are known to be
Multipoint B.E.T. Nitrogen Adsorption
adequate for moisture removal, then this step may be omitted.
7.2 Weigh a sample cell to the nearest 0.1 mg and record the
3. Significance and Use
mass.
3.1 These test methods are used to measure the external
7.3 Weigh into the cell approximately 0.4 g of the carbon
surface area of carbon black. These techniques are based on the
black to be tested.
statistical thickness method using a carbon black model. The
external surface area is defined as the specific surface area that
NOTE 1—For carbon black powder samples, add enough carbon black
is accessible to rubber. The external surface area excludes the to give a depth of approximately 2 in. in straight wall sample tubes, or fill
˚
the sample bulb for bulb-type sample cells.
micropore area, pore diameters less than 20 A.
7.4 Flow Degassing:
4. Apparatus
7.4.1 Open the helium control valve and insert the delivery
4.1 Multipoint Static-Volumetric Gas Adsorption Apparatus,
tube into the sample tube, and allow to purge for a minimum of
with Dewar flasks and all other accessories required for
1 min.
operation.
7.4.2 Place a heating mantle or other source of heat around
4.2 Sample Cells that, when attached to the adsorption 1
the sample cell and degas the sample at 300 6 10°C for ⁄2 h
apparatus, will maintain isolation of the sample from the
or longer to ensure that all traces of moisture condensing in the
−5 3
atmosphere equivalent to a helium leak rate of <10 cm /min,
top of the tube are absent.
per atmosphere of pressure difference.
7.4.3 Once the typical degassing times have been deter-
mined, future samples can be degassed on the basis of time
alone, if desired, allowing a reasonable margin of excess time.
1
These test methods are under the jurisdiction of ASTM Committee D-24 on
1
Some samples will be found to require less than ⁄2 h, especially
Carbon Black and are the direct responsibility of Subcommittee D24.21 on
Adsorptive Properties of Carbon Black.
if moisture exposure has been minimal. In these cases, the
Current edition approved August 10, 1999. Published September 1999. Origi-
minimum time that gives a stable surface area may be used for
nally published as D 5816 – 95. Last previous edition D 5816 – 96.
2
degassing.
Annual Book of ASTM Standards, Vol 09.01.
Copyright © ASTM, 100 Barr Harbor Drive, West Conshohocken, PA 19428-2959, United States.
1

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D 5816
sample mass ~dried!5~mass of cell 1 sample!2~mass of cell!
7.4.4 After degassing, the sample tube may be moved
(1)
directly to the analyzer. Otherwise, remove the sample tube
from the heat source and continue the flow of purging gas until Record masses to nearest 0.1 mg.
9.3 Statistical Thickness Surface Area:
it is ready for analysis.
7.4.5 Go directly to Section 8 and continue the remaining 9.3.1 Calculate the total volume of nitrogen adsorbed per g
3
of carbon black to the nearest 0.0001 cm as follows:
steps
...