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ASTM D3765-03

(Test Method)

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

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

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), and the CTAB method is being maintained by ASTM International in order to allow time for laboratories to obtain the proper instrumentation.
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
Historical
Publication Date
09-Jun-2003
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 D3765-02 - Standard Test Method for Carbon Black—CTAB (Cetyltrimethylammonium Bromide) Surface Area
Effective Date
10-Jun-2003
Replaced By
ASTM D3765-03a - Standard Test Method for Carbon Black—CTAB (Cetyltrimethylammonium Bromide) Surface Area
Effective Date
01-Nov-2003
Referred By
ASTM D6556-21 - Standard Test Method for Carbon Black—Total and External Surface Area by Nitrogen Adsorption
Effective Date
10-Jun-2003

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ASTM D3765-03 - Standard Test Method for Carbon Black—CTAB (Cetyltrimethylammonium Bromide) Surface AreaASTM D3765-03 - Standard Test Method for Carbon Black—CTAB (Cetyltrimethylammonium Bromide) Surface Area
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ASTM D3765-03 - Standard Test Method for Carbon Black—CTAB (Cetyltrimethylammonium Bromide) Surface Area
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Standards Content (Sample)

NOTICE: This standard has either been superceded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
Designation: D 3765 – 03
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 functional groups containing hydrogen and oxygen, etc. Rapid
equilibration is achieved by using mechanical stirring and
1.1 This test method covers the measurement of specific
ultrasonic vibration. Titration with dioctyl sodium sulfosucci-
surface area of carbon black exclusive of area contained in
4
nate (Aerosol OT ) solution to a turbidity maximum end point
micropores too small to admit hexadecyltrimethyl ammonium
is used to determine the unadsorbed CTAB after removal of the
bromide (cetyltrimethyl ammonium bromide, commonly re-
colloidally dispersed carbon black by ultrafiltration. All results
ferred to as CTAB). However, it should be noted that the
are scaled by using the Industry Tint Reference Black (ITRB)
preferred method for measuring external surface area is STSA
as a primary standard and taking its accessible surface area to
(Test Method D 6556), and the CTAB method is being
3 2 2
be exactly 83.0 3 10 m /kg (83.0 m /g).
maintained by ASTM International in order to allow time for
3.2 Titration of the unadsorbed CTAB with Aerosol OT
laboratories to obtain the proper instrumentation.
solution is accomplished by the following:
1.2 The values stated in SI units are to be regarded as the
3.2.1 Part A—Automatic Titration.
standard. The values given in parentheses are for information
3.2.2 Part B—Manual Turbidity Titration.
only.
1.3 This standard does not purport to address all of the
4. Significance and Use
safety concerns, if any, associated with its use. It is the
4.1 The CTAB molecule is relatively large; so it is not
responsibility of the user of this standard to establish appro-
adsorbed in micropores or on surface roughness. Thus, the
priate safety and health practices and determine the applica-
CTAB surface area reflects only the surface of the carbon black
bility of regulatory limitations prior to use.
that is available for interaction with rubber molecules.
2. Referenced Documents
5. Apparatus
2.1 ASTM Standards:
2
5.1 Analytical Balance, 0.1-mg sensitivity.
D 1193 Specification for Reagent Water
5
5.2 Ultrasonic Cleaning Bath, modified to incorporate
D 1799 Practice for Carbon Black—Sampling Packaged
3
integral magnetic stirring and vial holder to properly position
Shipments
two sample vials. (If desired, a separate ultrasonic cleaning
D 1900 Practice for Carbon Black—Sampling Bulk Ship-
3 bath and a separate magnetic stirrer may be used.)
ments
5.3 Magnetic Spinbars, chemically resistant covered (poly-
D 4483 Practice for Determining Precision for Test Method
3 chlorotrifluoroethylene or TFE-fluorocarbon), 6.4 or 4.8-mm
Standards in the Rubber and Carbon Black Industries
1 3
( ⁄4 or ⁄16-in.) diameter, and length nearly equal to the diameter
3
3. Summary of Test Method of 50 or 100-cm Berzelius beakers, glass vials, or other glass
vessels.
3.1 The isotherm for adsorption of an aqueous solution of
5.4 Microfiltration Membrane Filter Disks, mixed cellulose
CTAB on carbon black has a long horizontal plateau corre-
ester or cellulose nitrate, 47-mm diameter.
sponding to a monolayer coverage of the substrate surface from
5.5 Filter Holder.
which the adsorbate is not sterically excluded. The CTAB
3
5.6 Sampling Cylinder, 30-cm stainless steel, double end
adsorption by carbon black is independent of residual tars and
1
with 6.4-mm ( ⁄4-in.) NPT female openings, suitable for 0.7-
MPa (100-psi) pressure.
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 Adsorptive
4
Properties of Carbon Black. Aerosol OT is a registered trademark of the American Cyanamid Co., Process
Current edition approved June 10, 2003. Published June 2003. Originally Chemicals Dept., Wayne, NJ 07470.
5
approved in 1979. Last previous edition approved in 2002 as D 3765 – 02. This equipment is no longer commercially available. As an alternative, the
2
Annual Book of ASTM Standards, Vol 11.01. sample vial to be immersed in the ultrasonic bath may be fixed to an automatic
3
Annual Book of ASTM Standards, Vol 09.01. shaker in order to assure proper agitation during the ultrasonic treatment.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
1

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