Standard Test Method for Carbon Black-Morphological Characterization of Carbon Black Using Electron Microscopy

SCOPE
1.1 This test method covers the morphological characterization of carbon black primary aggregates from transmission electron microscope images. These measurements are used to derive the mean particle and aggregate size of carbon black in the dry (as manufactured) state, from CAB chip dispersion or removed from a rubber compound.
1.2 The values stated in SI units are to be regarded as the standard. The values 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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09-Nov-2002
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ASTM D3849-02 - Standard Test Method for Carbon Black-Morphological Characterization of Carbon Black Using Electron Microscopy
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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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 3849 – 02
Standard Test Method for
Carbon Black—Morphological Characterization of Carbon
1
Black Using Electron Microscopy
This standard is issued under the fixed designation D 3849; 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 black particle size is a distributional property; therefore, the
term particle size implies the mean value from multiple
1.1 This test method covers the morphological characteriza-
measurements.
tion of carbon black primary aggregates from transmission
3.1.1.2 carbon black aggregate—a discrete, rigid colloidal
electron microscope images. These measurements are used to
entity that is the smallest dispersible unit; it is composed of
derive the mean particle and aggregate size of carbon black in
extensively coalesced particles. Carbon black aggregate size is
the dry (as manufactured) state, from CAB chip dispersion or
a distributional property; therefore, the term aggregate size
removed from a rubber compound.
implies the mean value from multiple measurements.
1.2 The values stated in SI units are to be regarded as the
3.1.1.3 glow discharge—a plasma of ionized gas that is
standard. The values in parentheses are for information only.
formed in a high-voltage field at pressures of about 3 to 20 Pa
1.3 This standard does not purport to address all of the
-3
(25 to 150 3 10 torr). An alternating current (a-c) glow
safety concerns, if any, associated with its use. It is the
discharge using air is effective in cleaning and oxidizing the
responsibility of the user of this standard to establish appro-
surface of carbon substrates to improve the wetting character-
priate safety and health practices and determine the applica-
istics of polar vehicles containing pigment dispersions.
bility of regulatory limitations prior to use.
3.1.1.4 substrate—a thin film that is used to support elec-
2. Referenced Documents tron microscope specimens. Evaporated carbon films are com-
monly used because of relatively good mechanical strength,
2.1 ASTM Standards:
stability and conductivity.
D 3182 Practice for Rubber—Materials, Equipment, and
3.1.2 Aggregate Dimensional Properties from Image Analy-
Procedures for Mixing Standard Compounds and Prepar-
2
sis
ing Standard Vulcanized Sheets
3.1.2.1 area (A)—the two-dimensional projected area of the
D 3191 Test Methods for Carbon Black in SBR (Styrene-
2
carbon black aggregate image.
Butadiene Rubber)—Recipe and Evaluation Procedures
3.1.2.2 perimeter (P)—the total boundary length of an
D 3192 Test Methods for Carbon Black Evaluation in NR
2
aggregate.
(Natural Rubber)
3.1.2.3 volume (V)—an estimate of the volume of the
D 6556 Test Method for Carbon Black—Total and External
2
carbon black aggregate using stereological principles.
Surface Area by Nitrogen Adsorption
3.1.3 Image Analysis
3. Terminology
3.1.3.1 erosion—the process by which image features are
reduced in size by selectively removing pixels from their
3.1 Definitions:
periphery. It consists of examining each binary pixel and
3.1.1 General
changing it from ON to OFF if it has greater than a preset
3.1.1.1 carbon black particle—a small spheroidally shaped,
minimum of neighbors that are OFF. It serves a number of
paracrystalline, non-discrete component of an aggregate; it can
useful functions such as smoothing feature outlines and sepa-
only be separated from the aggregate by fracturing. Carbon
rating features touching each other.
3.1.3.2 dilation—the converse of erosion. This process is
1
accomplished by changing any OFF pixel to ON if it has
This test method is under the jurisdiction of ASTM Committee D24 on Carbon
Black and is the direct responsibility of Subcommittee D24.81 on Carbon Black
greater than a preset minimum of ON neighbors. This process
Microscopy and Morphology.
causes image features to grow in size, which fills in small
Current edition approved Nov. 10, 2002. Published December 2002. Originally
breaks in features, internal voids, or small indentations along
approved in 1980. Last previous edition approved in 2000 as D 3849 – 95a (2000).
2
Annual Book of ASTM Standards, Vol 09.01. the feature surface.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
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D3849–02
3.1.3.3 feature—areas within a single continuous boundary 5.8 Electrically Heated Tube Furnace, capable of being
that have gray-level ranges that allow them to be distinguished heated to 800 to 900°C under an inert environment, with the
from the background area outside the feature v
...

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