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ASTM D3765-03a

(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
31-Oct-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 D3765-03 - Standard Test Method for Carbon Black—CTAB (Cetyltrimethylammonium Bromide) Surface Area
Effective Date
01-Nov-2003
Replaced By
ASTM D3765-04 - Standard Test Method for Carbon Black—CTAB (Cetyltrimethylammonium Bromide) Surface Area (Withdrawn 2007)
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-Nov-2003

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ASTM D3765-03a - Standard Test Method for Carbon Black—CTAB (Cetyltrimethylammonium Bromide) Surface AreaASTM D3765-03a - Standard Test Method for Carbon Black—CTAB (Cetyltrimethylammonium Bromide) Surface Area
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ASTM D3765-03a - Standard Test Method for Carbon Black—CTAB (Cetyltrimethylammonium Bromide) Surface Area
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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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 3765 – 03a
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 equilibration is achieved by using mechanical stirring and
ultrasonic vibration. Titration with dioctyl sodium sulfosucci-
1.1 This test method covers the measurement of specific
4
nate (Aerosol OT ) solution to a turbidity maximum end point
surface area of carbon black exclusive of area contained in
is used to determine the unadsorbed CTAB after removal of the
micropores too small to admit hexadecyltrimethyl ammonium
colloidally dispersed carbon black by ultrafiltration. All results
bromide (cetyltrimethyl ammonium bromide, commonly re-
are scaled by using the Industry Tint Reference Black (ITRB)
ferred to as CTAB). However, it should be noted that the
as a primary standard and taking its accessible surface area to
preferred method for measuring external surface area is STSA
3 2 2
be exactly 83.0 3 10 m /kg (83.0 m /g).
(Test Method D 6556).
3.2 Titration of the unadsorbed CTAB with Aerosol OT
1.2 The values stated in SI units are to be regarded as the
solution is accomplished by the following:
standard. The values given in parentheses are for information
3.2.1 Part A—Automatic Titration.
only.
3.2.2 Part B—Manual Turbidity Titration.
1.3 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the
4. Significance and Use
responsibility of the user of this standard to establish appro-
4.1 The CTAB molecule is relatively large; so it is not
priate safety and health practices and determine the applica-
adsorbed in micropores or on surface roughness. Thus, the
bility of regulatory limitations prior to use.
CTAB surface area reflects only the surface of the carbon black
2. Referenced Documents that is available for interaction with rubber molecules.
2.1 ASTM Standards:
5. Apparatus
2
D 1193 Specification for Reagent Water
5.1 Analytical Balance, 0.1-mg sensitivity.
D 1799 Practice for Carbon Black—Sampling Packaged
5
3 5.2 Ultrasonic Cleaning Bath, modified to incorporate
Shipments
integral magnetic stirring and vial holder to properly position
D 1900 Practice for Carbon Black—Sampling Bulk Ship-
3 two sample vials. (If desired, a separate ultrasonic cleaning
ments
bath and a separate magnetic stirrer may be used.)
D 4483 Practice for Determining Precision for Test Method
3 5.3 Magnetic Spinbars, chemically resistant covered (poly-
Standards in the Rubber and Carbon Black Industries
chlorotrifluoroethylene or TFE-fluorocarbon), 6.4 or 4.8-mm
1 3
3. Summary of Test Method ( ⁄4 or ⁄16-in.) diameter, and length nearly equal to the diameter
3
of 50 or 100-cm Berzelius beakers, glass vials, or other glass
3.1 The isotherm for adsorption of an aqueous solution of
vessels.
CTAB on carbon black has a long horizontal plateau corre-
5.4 Microfiltration Membrane Filter Disks, mixed cellulose
sponding to a monolayer coverage of the substrate surface from
6
ester or cellulose nitrate, 47-mm diameter, 0.1 μm pore size .
which the adsorbate is not sterically excluded. The CTAB
5.5 Filter Holder.
adsorption by carbon black is independent of residual tars and
functional groups containing hydrogen and oxygen, etc. Rapid
1 4
This test method is under the jurisdiction of ASTM Committee D24 on Carbon Aerosol OT is a registered trademark of the American Cyanamid Co., Process
Black and is the direct responsibility of Subcommittee D24.21 on Adsorptive Chemicals Dept., Wayne, NJ 07470.
5
Properties of Carbon Black. This equipment is no longer commercially available. As an alternative, the
Current edition approved Nov. 1, 2003. Published December 2003. Originally sample vial to be immersed in the ultrasonic bath may be fixed to an automatic
approved in 1979. Last previous edition approved in 2003 as D 3765 – 03. shaker in order to assure proper agitation during the ultrasonic treatment.
2 6
Annual Book of ASTM Standards, Vol 11.01. Membrane filter disks of hydrophilic polysulfone, pore size 0.2 μm, also have
3
Annual Book of ASTM Standards, Vol 09.01. been found to be suitable.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
1

---------------------- Page: 1 ----------------------
D 3765 – 03a
FIG. 1 Pressure Filtration Manifold
3
5.6 Sampling Cylinder, 30-cm stainless steel, double end 5.24 Polyethylene Tubing (do not use vinyl tubing).
1
with 6.4-mm ( ⁄4-in.) NPT female openings, suit
...

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