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ASTM D3765-04

(Test Method)

Standard Test Method for Carbon Black—CTAB (Cetyltrimethylammonium Bromide) Surface Area (Withdrawn 2007)

Standard Test Method for Carbon Black—CTAB (Cetyltrimethylammonium Bromide) Surface Area (Withdrawn 2007)

SCOPE
1.1 This test method covers the measurement of specific surface area of carbon black exclusive of area contained in micropores too small to admit hexadecyltrimethyl ammonium bromide (cetyltrimethyl ammonium bromide, commonly referred to as CTAB). However, it should be noted that the preferred method for measuring external surface area is STSA (Test Method D 6556).
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.
WITHDRAWN RATIONALE
This test method covers the measurement of specific surface area of carbon black exclusive of area contained in micropores too small to admit hexadecyltrimethyl ammonium bromide (cetyltrimethyl ammonium bromide, commonly referred to as CTAB).
Formerly under the jurisdiction of Committee D24 on Carbon Black, this test method was withdrawn in August 2007 because the preferred method for measuring external surface area is STSA (Test Method D 6556).
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.

General Information

Status
Withdrawn
Publication Date
31-May-2004
Withdrawal Date
27-Aug-2007
ICS
83.040.20 - Rubber compounding ingredients
Technical Committee
D24 - Carbon Black
Drafting Committee
D24.21 - Carbon Black Surface Area and Related Properties
Current Stage
Ref Project

Relations

Replaces
ASTM D3765-03a - Standard Test Method for Carbon Black—CTAB (Cetyltrimethylammonium Bromide) Surface Area
Effective Date
01-Jun-2004
Referred By
ASTM D6556-21 - Standard Test Method for Carbon Black—Total and External Surface Area by Nitrogen Adsorption
Effective Date
01-Jun-2004

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ASTM D3765-04 - Standard Test Method for Carbon Black—CTAB (Cetyltrimethylammonium Bromide) Surface Area (Withdrawn 2007)ASTM D3765-04 - Standard Test Method for Carbon Black—CTAB (Cetyltrimethylammonium Bromide) Surface Area (Withdrawn 2007)
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ASTM D3765-04 - Standard Test Method for Carbon Black—CTAB (Cetyltrimethylammonium Bromide) Surface Area (Withdrawn 2007)
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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:D3765–04
Standard Test Method for
Carbon Black—CTAB (Cetyltrimethylammonium Bromide)
1
Surface Area
This standard is issued under the fixed designation D 3765; 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 adsorption by carbon black is independent of residual tars and
functional groups containing hydrogen and oxygen, and the
1.1 This test method covers the measurement of specific
like. Rapid equilibration is achieved by using mechanical
surface area of carbon black exclusive of area contained in
stirring and ultrasonic vibration. Titration with dioctyl sodium
micropores too small to admit hexadecyltrimethyl ammonium
3
sulfosuccinate (Aerosol OT ) solution to a turbidity maximum
bromide (cetyltrimethyl ammonium bromide, commonly re-
end point is used to determine the unadsorbed CTAB after
ferred to as CTAB). However, it should be noted that the
removal of the colloidally dispersed carbon black by ultrafil-
preferred method for measuring external surface area is STSA
tration. All results are scaled by using the Industry Tint
(Test Method D 6556).
Reference Black (ITRB) as a primary standard and taking its
1.2 The values stated in SI units are to be regarded as the
3 2
accessible surface area to be exactly 83.0 3 10 m /kg (83.0
standard. The values given in parentheses are for information
2
m /g).
only.
3.2 Titration of the unadsorbed CTAB with Aerosol OT
1.3 This standard does not purport to address all of the
solution is accomplished by the following:
safety concerns, if any, associated with its use. It is the
3.2.1 Part A—Automatic Titration.
responsibility of the user of this standard to establish appro-
3.2.2 Part B—Manual Turbidity Titration.
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use.
4. Significance and Use
2. Referenced Documents 4.1 The CTAB molecule is relatively large; so it is not
2
adsorbed in micropores or on surface roughness. Thus, the
2.1 ASTM Standards:
CTABsurfaceareareflectsonlythesurfaceofthecarbonblack
D 1193 Specification for Reagent Water
that is available for interaction with rubber molecules.
D 1799 Practice for Carbon Black—Sampling Packaged
Shipments
5. Apparatus
D 1900 Practice for Carbon Black—Sampling Bulk Ship-
5.1 Analytical Balance, 0.1-mg sensitivity.
ments
4
5.2 Ultrasonic Cleaning Bath, modified to incorporate
D 4483 Practice for Determining Precision for Test Method
integral magnetic stirring and vial holder to properly position
Standards in the Rubber and Carbon Black Industries
two sample vials. (If desired, a separate ultrasonic cleaning
D 6556 Test Method for Carbon Black—Total and External
bath and a separate magnetic stirrer may be used.)
Surface Area by Nitrogen Adsorption
5.3 Magnetic Spinbars, chemically resistant, covered (poly-
3. Summary of Test Method chlorotrifluoroethylene or TFE-fluorocarbon), 6.4 or 4.8-mm
1 3
( ⁄4 or ⁄16-in.) diameter, and length nearly equal to the diameter
3.1 The isotherm for adsorption of an aqueous solution of
3
of 50 or 100-cm Berzelius beakers, glass vials, or other glass
CTAB on carbon black has a long horizontal plateau corre-
vessels.
spondingtoamonolayercoverageofthesubstratesurfacefrom
5.4 Microfiltration Membrane Filter Disks, mixed cellulose
which the adsorbate is not sterically excluded. The CTAB
5
ester or cellulose nitrate, 47-mm diameter, 0.1-µm pore size .
5.5 Filter Holder.
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
3
Surface Area and Related Properties. Aerosol OT is a registered trademark of the American Cyanamid Co., Process
Current edition approved June 1, 2004. Published June 2004. Originally Chemicals Dept., Wayne, NJ 07470.
4
approved in 1979. Last previous edition approved in 2003 as D 3765 – 03a. This equipment is no longer commercially available. As an alternative, the
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or sample vial to be immersed in the ultrasonic bath may be fixed to an automatic
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM shaker in order to assure proper agitation during the ultrasonic treatment.
5
Standards volume information, refer to the standard’s Document Summary page on Membrane filter disks of hydrophilic polysulfone, pore size 0.2 µm, also have
the ASTM website. been found to be suitable.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
1

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