ASTM D1603-94

NOTICE: This standard has either been superseded and replaced by a new version or discontinued.
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Designation: D 1603 – 94
AMERICAN SOCIETY FOR TESTING AND MATERIALS
100 Barr Harbor Dr., West Conshohocken, PA 19428
Reprinted from the Annual Book of ASTM Standards. Copyright ASTM
Standard Test Method for
Carbon Black In Olefin Plastics
This standard is issued under the fixed designation D 1603; 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 4. Apparatus
1.1 This test method covers the determination of the carbon 4.1 Electric Furnace, at least 20 cm (8 in.) long suitable for
black content in polyethylene, polypropylene, and polybuty- use with the tubing described in 4.2.
lene plastics. Its use with acrylic or other polar monomer 4.2 Tubing,, 2.9 cm ( ⁄8 in.) in diameter, approximately
modifications which might affect the accuracy is not recom- twice as long as the furnace described in 4.1.
mended. Determinations of carbon black are made gravimetri- 4.3 Stoppers—Two rubber or neoprene stoppers, to fit the
cally after pyrolysis of the sample under nitrogen. This test tube described in 4.2, unless the tube is fitted with ground
method is not applicable to compositions that contain nonvola- joints and mating connectors.
tile pigments or fillers other than carbon black. 4.4 Glass Tubing, 10-mm, of sufficient amount, and match-
1.1.1 This test method is not applicable to materials con- ing rubber or plastic tubing for connections.
taining brominated flame retardant additives at the end. 4.5 Combustion Boat, approximately 8 by 1.9 by 1.3 cm
1 3 1
1.2 The values stated in SI units are to be regarded as the (3 ⁄2 by ⁄4 by ⁄2 in.). Glazed porcelain, quartz high-silica glass,
standard. The values in parentheses are given for information or platinum is suitable.
only.
NOTE 2—A loose-fitting cover for the combustion boat is optional. If
1.3 This standard does not purport to address all of the
used, it shall be considered a part of the boat and handled and weighed
safety concerns, if any, associated with its use. It is the
with it.
responsibility of the user of this standard to establish appro-
4.6 Iron-Constantan Thermocouple, and a potentiometer or
priate safety and health practices and determine the applica-
millivoltmeter suitable for determining temperatures in the
bility of regulatory limitations prior to use.
range 300 to 700 C.
NOTE 1—This test method is similar to ISO 6964-1986(E) in title only.
4.7 Flow Meter,, suitable for measuring gas flow at rates of
The technical content is significantly different.
1 to 10 L/min.
4.8 Traps, three glass traps with removable ground-glass
2. Referenced Documents
connected heads and 10-mm diameter inner and connecting
2.1 ASTM Standards:
tubes.
E 177 Practice for Use of the Terms Precision and Bias in
2 NOTE 3—Only one trap is required if the entire apparatus train is placed
ASTM Test Methods
in a fume hood. None is required if in addition, nitrogen of sufficient
2.2 ISO Standard:
purity is used and produced by the alternative means provided in Section
ISO 6964-1986(E) Polyolefin Pipes and Fittings—
5.
Determination of Carbon Black by Calcination and
4.9 Drying Tube—A U-shaped drying tube, having an inside
Pyrolysis—Test Method and Basic Specification
diameter of 20 mm or larger, fitted with ground glass or
neoprene stoppers.
3. Significance and Use
4.10 Glass Wool.
3.1 The information provided by this test method is useful
4.11 Desiccator, with desiccant.
for control purposes and is required for calculation of optical
4.12 Bunsen Burner.
absorptivity.
4.13 Balance—An analytical balance having a sensitivity of
0.0001 g.
This test method is under the jurisdiction of ASTM Committee D-20 on Plastics 4.14 Weights—A set of Class S weights for use with the
and is the direct responsibility of Subcommittee D20.70 on Analytical Methods
balance.
(Section D20.70.01).
In 1993, the scope was revised to clarify limitations related to use of this test
5. Reagents and Materials
method with materials containing brominated additives and to include an ISO
equivalency statement. Keywords were also added.
5.1 Carbon Dioxide, Solid (Dry Ice).
Current edition approved June 15, 1994. Published August 1994. Originally
published as D 1603 – 58. Last previous edition D 1603 – 76 (1988)e .
2 4
Annual Book of ASTM Standards, Vol 14.02. Pyrex, Vycor, or equivalent tubing has been found satisfactory for this purpose.
3 5
Available from American National Standards Institute, 11 W. 42nd St., 13th Precision Bore Rotometer Tube No. 2B-25, available from the Fischer & Porter
Floor, New York, NY 10036. Co., County Line Road, Warminster, PA 18974 has been found satisfactory.
D 1603
NOTE 4—The solid carbon dioxide and the trichloroethylene are not
cool over fresh desiccant for not less than 30 min.
required if the entire apparatus train is placed in a fume hood.
6.3 Remove the boat from the desiccator and weigh it to
nearest 0.0001 g. Immediately place 1.0 6 0.1 g of the ethylene
5.2 Desiccant, such as anhydrous calcium chloride (CaCl ).
plastic under test in the boat and quickly weigh to the nearest
5.3 Nitrogen, prepurified, having oxygen content below
0.0001 g.
0.01 %. As a safeguard against accidental leakage, conta
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