Standard Test Method for Carbon Black—Oil Absorption Number of Compressed Sample

SCOPE
1.1 This test method covers the procedure for the mechanical compression of a carbon black sample and the determination of the oil absorption number of the compressed sample.  
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.

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Publication Date
09-Dec-2001
Technical Committee
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ASTM D3493-00a - Standard Test Method for Carbon Black—Oil Absorption Number of Compressed Sample
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NOTICE: This standard has either been superseded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
Designation: D 3493 – 00a
Standard Test Method for
Carbon Black—Oil Absorption Number of Compressed
Sample
This standard is issued under the fixed designation D 3493; 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 to one of a semiplastic agglomeration, with an accompanying
increase in viscosity. This increased viscosity is transmitted to
1.1 This test method covers the procedure for the mechani-
the torque-sensing system of the absorptometer. When the
cal compression of a carbon black sample and the determina-
viscosity of the mixture reaches a predetermined torque level,
tion of the oil absorption number of the compressed sample.
the absorptometer and buret will simultaneously shut off. The
1.2 The values stated in SI units are to be regarded as the
volume of oil added is read from the direct reading buret. The
standard. The values given in parentheses are for information
volume of oil per unit mass of carbon black is the oil
only.
absorption number. Referee testing between suppliers and
1.3 This standard does not purport to address all of the
users should use DBP oil until such time that precision data is
safety concerns, if any, associated with its use. It is the
available for paraffin oil.
responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica-
4. Significance and Use
bility of regulatory limitations prior to use.
4.1 The oil absorption number of a carbon black is related to
2. Referenced Documents the processing and vulcanizate properties of rubber compounds
containing the carbon black.
2.1 ASTM Standards:
4.2 The difference between the regular oil absorption num-
D 1799 Practice for Carbon Black—Sampling Packaged
2 ber and the oil absorption number of compressed sample is
Shipments
some measure of the stability of the structure of the carbon
D 1900 Practice for Carbon Black—Sampling Bulk Ship-
2 black.
ments
D 2414 Test Method for Carbon Black—n-Dibutyl Phtha-
5. Apparatus
late Absorption Number
5.1 Balance, analytical, 0.01-g sensitivity.
D 3324 Practice for Carbon Black—Improving Test Repro-
5.2 Oven, gravity-convection type, capable of maintaining
ducibility Using ASTM Reference Blacks
125°C 65°C.
D 4483 Practice for Determining Precision for Test Method
5.3 Carbon Black Press, capable of compressing a 25 g
Standards in the Rubber and Carbon Black Industries
sample to 165 MPa (24 000psi).
E 691 Practice for Conducting an Interlaboratory Study to
5.4 Absorptometer, equipped with a constant-rate buret
Determine the Precision of a Test Method
3 3
which delivers 67 6 0.4 mm /s (4 6 0.024 cm /min).
3. Summary of Test Method 5.5 Spatula, rubber, 100-mm.
5.6 Sieve, 850 μm (U.S. No. 20), approximately 125-mm
3.1 A sample of carbon black is compressed four times in a
(5-in.) diameter with receiver pan.
compression cylinder at a pressure of 165 MPa (24 000 psi)
5.7 Brush, approximately 40-mm (1.5-in.), stiff bristle.
and then tested in an absorptometer to determine the oil
5.8 Desiccator.
absorption number.
3.2 n -Dibutyl phthalate or paraffin oil is added by means of
6. Reagent and Standards
a constant-rate buret to the compressed sample of carbon black
6.1 Purity of Reagents—Reagent grade chemicals shall be
in the mixer chamber of an absorptometer. As the sample
used in all tests. Unless otherwise indicated, it is intended that
absorbs the oil, the mixture changes from a free-flowing state
All apparatus is to be operated and maintained in accordance with the
This test method is under the jurisdiction of ASTM Committee D24 on Carbon
manufacturer’s directions for optimum performance.
Black and is the direct responsibility of Subcommittee D24.11 on Absorptive
Carbon black presses from the following companies have been found satisfac-
Properties of Carbon Black. tory for this test method: EG&G Engineering, P.O. Box 470710, Tulsa, OK
Current edition approved Nov. 10, 2000. Published January 2001. Originally 74147–0710 and Titan Specialties, Inc., P.O. Box 2316, Pampa, TX 79066-2316.
published as D 3493-76. Last previous edition D 3493-00. Available from C. W. Brabender Instruments, Inc., 50 E. Wesley St., South
Annual Book of ASTM Standards, Vol 09.01. Hackensack, NJ 07606 and from HITEC Luxembourg, 5 Rue de l’Eglise, L-1458
Annual Book of ASTM Standards, Vol 14.02. Luxembourg.
Copyright © ASTM, 100 Barr Harbor Drive, West Conshohocken, PA 19428-2959, United States.
D 3493
all reagents shall conform to the specifications of the Commit- 9.4.5 Raise the ram to a sufficient height to allow the bottom
tee on Analytical Reagents of the American Chemical Society, seal plate to be removed, then lower the ram in order to press
where such specifications are available. Other grades may be the piston and sample through the cylinder and into a sieve
used, provided it is first ascertained that the reagent is of screen fitted with a receiver pan.
sufficiently high purity to permit its use without lessening the 9.4.6 Wipe the piston, cylinder and seal in order to remove
accuracy of the determination. carbon black dust and reassemble the apparatus as described in
6.2 n-Dibutyl Phthalate, having a density of 1.042 to 1.047 9.4.1.
Mg/m at 25°C and a relative density of 1.045 to 1.050 at 25°C. 9.4.7 Pass the compressed carbon black through the sieve
6.3 Paraffin oil, having a kinematic viscosity of 10 to 34 screen into the receiver.
2 8
mm /s (cSt) at 40° C 9.4.8 Repeat 9.4.2-9.4.7, compressing the sample a total of
6.4 ASTM D-24 Standard Reference Blacks, SRB-5. four times. Retain the sample from 9.4.7 after the fourth
compression. Proceed to 9.6.
7. Sampling
9.5 Titan Press
9.5.1 Lower the cylinder piston by pressing the left hand
7.1 Samples shall be taken in accordance with Practices
lever downward then pour the carbon black sample into the
D 1799 and D 1900.
cylinder.
8. Calibration and Standardization 9.5.2 Close and latch the door of the press. Compress the
sample by operating the ram using a downward movement of
8.1 See Test Method D 2414.
the right hand lever, until the preset gauge pressure reaches
NOTE 1—If values are not obtained within the acceptable range, it will
approximately 11 MPa (1550 psi). Release immediately. The
be necessary to either vary the pressure of the hydraulic press until
exact pressure is determined by measuring the compressed oilA
acceptable values are obtained or follow Practice D 3324.
value of the SRB materials and making appropriate adjust-
9. Procedure ments. If the values are too high, the pressure is increased and
pressure is lowered if the values are too low.
9.1 Dry an adequate sample for1hina specified oven set
9.5.3 Raise the ram until it is level with the top of the
at 125°C. Cool the sample in a desiccator for a minimum of 30
conical collar placed on top of the cylinder.
min prior to testing.
9.5.4 Raise the cylinder piston until the compressed sample
9.2 Weigh 25 6 0.1 g of the sample.
is broken by contact with the raised ram. The conical collar will
9.3 Compress the sample using either the Chandler or Titan
retain the sample.
press.
9.5.5 Break up the sample with a spatula, lower the cylinder
9.4 Chandler Press
piston, and allow the sample to fall back into cylinder. If
9.4.1 Place the bottom seal plate and the compression
necessary, brush the inside of the collar to return all of the
cylinder in the hydraulic press. Move the handle of the seal
carbon black to the cylinder.
plate to check its position in the support plate. Rotate the
9.5.6 Repeat steps 9.5.2-9.5.5 an additional three times, for
cylinder to be certain that it fits on the seal plate.
a total of four compression cycles.
9.4.2 Place the carbon black sample in the compr
...

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