Designation: D 1603 – 01

Standard Test Method for

Carbon Black In Olefin Plastics1
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 3. Terminology
1.1 This test method covers the determination of the carbon 3.1 Definitions—For definitions of technical terms pertain-
black content in polyethylene, polypropylene, and polybuty- ing to plastics used in this specification, see Terminology
lene plastics. Its use with acrylic or other polar monomer D 883.
modifications which might affect the accuracy is not recom-
mended. Determinations of carbon black are made gravimetri- 4. Significance and Use
cally after pyrolysis of the sample under nitrogen. This test 4.1 The information provided by this test method is useful
method is not applicable to compositions that contain nonvola- for control purposes and is required for calculation of optical
tile pigments or fillers other than carbon black. absorptivity.
1.1.1 This test method is not applicable to materials con-
taining brominated flame retardant additives at the end. 5. Apparatus
1.2 The values stated in SI units are to be regarded as the 5.1 Electric Furnace, at least 20 cm (7.9 in.) long suitable
standard. The values in parentheses are given for information for use with the tubing described in 5.2.
only. 5.2 High Temperature Glass Combustion Tube, 5 of appro-
1.3 This standard does not purport to address all of the priate diameter and approximately twice as long as the furnace
safety concerns, if any, associated with its use. It is the described in 5.1.
responsibility of the user of this standard to establish appro- 5.3 Stoppers—Two rubber or neoprene stoppers, to fit the
priate safety and health practices and determine the applica- tube described in 5.2, unless the tube is fitted with ground
bility of regulatory limitations prior to use. joints and mating connectors.
5.4 Glass Tubing, approximately 10 mm (0.39 in.) in
NOTE 1—This test method is similar to ISO 6964-1986(E) in title only.
The technical content is significantly different.
diameter, of sufficient amount, and matching rubber or plastic
tubing for connections.
2. Referenced Documents 5.5 Combustion Boat, approximately 8 by 1.9 by 1.3 cm
2.1 ASTM Standards: (3.15 by 0.75 by 0.51 in.). Glazed porcelain, quartz high-silica
D 883 Terminology Relating to Plastics2 glass, or platinum is suitable.
E 177 Practice for Use of the Terms Precision and Bias in NOTE 2—A loose-fitting cover for the combustion boat is optional. If
ASTM Test Methods3 used, it shall be considered a part of the boat and handled and weighed
2.2 ISO Standard: with it.
ISO 6964-1986(E) Polyolefin Pipes and Fittings— 5.6 Iron-Constantan Thermocouple, and a potentiometer or
Determination of Carbon Black by Calcination and millivoltmeter suitable for determining temperatures in the
Pyrolysis—Test Method and Basic Specification4 range 300 to 700°C (572 to 1292°F).
5.7 Flow Meter, 6 suitable for measuring gas flow at rates of
1
1 to 10 L/min.
This test method is under the jurisdiction of ASTM Committee D20 on Plastics
and is the direct responsibility of Subcommittee D20.70 on Analytical Methods 5.8 Traps, three glass traps with removable ground-glass
(Section D20.70.01). connected heads and 10-mm (0.39–in.) diameter inner and
In 1993, the scope was revised to clarify limitations related to use of this test connecting tubes.
method with materials containing brominated additives and to include an ISO
equivalency statement. Keywords were also added. NOTE 3—Only one trap is required if the entire apparatus train is placed
Current edition approved March 10, 2001. Published June 2001. Originally in a fume hood. None is required if in addition, nitrogen of sufficient
published as D 1603 – 58. Last previous edition D 1603 – 94.
2
Annual Book of ASTM Standards, Vol 08.01.
3
Annual Book of ASTM Standards, Vol 14.02.
4 5
ISO/IEC Selected Standards for Testing Plastics, Second Edition, published by Pyrex, Vycor, or equivalent tubing has been found satisfactory for this purpose.
6
ASTM. Also, available from American National Standards Institute, 11 W. 42nd St., Precision Bore Rotometer Tube No. 2B-25, available from the Fischer & Porter
13th Floor, New York, NY 10036. Co., County Line Road, Warminster, PA 18974 has been found satisfactory.

Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.

1
 D 1603
purity is used and produced by the alternative means provided in Section tinsel, foil, or wire, and maintained in a furnace at a tempera-
6. ture around 500°C (932°F).
5.9 Drying Tube—A U-shaped drying tube, having an inside 6.3.4 The need for the procedures described is eliminated if
diameter of 20 mm (0.79 in.) or larger, fitted with ground glass gas having an oxygen content of less than 0.002 % (20 ppm) is
or neoprene stoppers. used.
5.10 Glass Wool. 6.4 Trichloroethylene, technical grade (Note 4).
5.11 Desiccator, with desiccant.
5.12 Bunsen Burner. 7. Procedure
5.13 Balance—An analytical balance having a sensitivity of
NOTE 5—The procedure below assumes that the combustion tube can
0.0001 g. be easily removed from the furnace. If this is not the case, alternate
5.14 Weights—A set of Class S weights for use with the methods of inserting and removing sample boats are acceptable as long as
balance (if required). the temperature, purge time, and flow rate requirements are met.

6. Reagents and Materials 7.1 Assemble the apparatus as shown in Fig. 1. Both cold
traps following the combustion tube shall contain trichloroet-
6.1 Carbon Dioxide, Solid (Dry Ice). hylene, but only the first need be cooled with solid carbon
NOTE 4—The solid carbon dioxide and the trichloroethylene are not dioxide. Alternatively, the entire apparatus may be placed in a
required if the entire apparatus train is placed in a fume hood. fume hood and the two traps following the combustion tube
6.2 Desiccant, such as anhydrous calcium chloride (CaCl2). omitted. Fill the drying tube with anhydrous CaCl2 or other
6.3 Nitrogen, prepurified, having oxygen content below suitable desiccant. Hold between loose plugs of glass wool.
0.01 %. As a safeguard against accidental leakage, contamina- 7.2 Heat a clean combustion boat to red heat in a bunsen
tion, or inadequate purity, the gas shall be further purified by flame; then transfer the boat to the desiccator and allow it to
one of the following procedures: cool over fresh desiccant for not less than 30 min.
6.3.1 Passage of the nitrogen through a glass trap inserted 7.3 Remove the boat from the desiccator and weigh it to
ahead of the drying tube (seeFig. 1 ), filled approximately one nearest 0.0001 g (w1). Immediately place 1.0 6 0.1 g of the
third full of potassium hydroxide - pyrogallol solution made to ethylene plastic under test in the boat and quickly weigh to the
contain 5 g of pyrogallol and 50 g of KOH in 100 mL of water. nearest 0.0001 g (w2).
Technical grade, or better, reagents are satisfactory. 7.4 Heat the furnace to a constant temperature of 600°C
6.3.2 Insertion of a plug, or roll, of clean copper tinsel, foil, (1112°F).
or wire 7.5 to 10 cm (3 to 4 in.) long into the combustion tube 7.5 With the combustion tube removed from the furnace,
ahead of the sample (see Fig. 1) so that it is completely within adjust the rate of nitrogen flow through the tube to 1.7 6 0.3
the heated region of the furnace. Take care to prevent chan- L/min. Open the inlet end of the combustion tube, quickly
neling of the nitrogen through the plug. The extent of black- place the combustion boat with the sample into the tube
ening of the copper may be taken as a guide for determining positioned so the boat will be at the proper temperature when
when the plug should be renewed. in the furnace. Close the inlet to the tube and allow the nitrogen
6.3.3 Passage of the nitrogen through a combustion tube to flow for a minimum of 5 min to purge oxygen from the
filled to a length of 15 cm (6 in.) or greater with clean copper system prior to placing the tube in the furnace. If the furnace is

FIG. 1 Assembly of Apparatus

2
 D 1603
controlled by an external thermocouple, adjust the thermo- ~ Wr 2 W o !
Carbon black, % 5 W 3 100 (1)
couple so that the weld is in proximity to the boat. Insert the s

copper plug, if this is used (see 6.3.2). Quickly place the tube
where:
into the furnace, close the furnace, and allow heating to Wr = w3 - w1 = mass of residue (g) after burning in nitro-
proceed for at least 15 min. gen,
NOTE 6—The exact temperature of heating is not critical in the range
Wo = w4 - w1 = mass of residue (g) afterburning in air, and
500 to 700°C (932 to 1292°F), although a heating time as long as 30 min
Ws = w2 - w1 = mass of sample(g).
is desirable at the lower temperature. If desired, the sample may be put in
the furnace at 300°C (572°F) or less and the temperature of the furnace 9. Report
then programmed for sample heating to 350°C (662°F) in 10 min, 450°C
9.1 Report the following information:
(842°F) in another 10 min, and 500°C (932°F) after a total of 30 min,
finally heating at 500°C (932°F) for an additional 15 min. 9.1.1 Identity of the sample,
NOTE 7—If the combustion tube and furnace are of adequate size, 9.1.2 The individual values calculated as described in Sec-
several sample boats may be tested simultaneously if they are positioned tion 7, and
in the furnace within the area which meets the temperature requirements.
9.1.3 The average of the values reported in 9.1.2.
7.6 Move the tube or furnace so that the boat is no longer in
7
the heated zone of the furnace and allow 5 min for cooling, 10. Precision and Bias
while maintaining the flow of nitrogen. Remove the copper 10.1 The interlaboratory precision, exclusive of sampling
plug, if present, and the boat through the inlet end of the tube error, was determined by an interlaboratory study with seven
and allow it to cool in the desiccator for at least 30 min. Take laboratories to be 60.156 % (3S) as defined in Practice E 177,
care that the boat does not become contaminated from any over the range 2.5 to 3.0 % carbon black, and 60.309 % (3S)
deposits on the walls of the tube. Then quickly reweigh the over the range 35 to 55 % carbon black.
boat and its contents to the nearest 0.0001 g (w3).
7.7 If carbon black measurements are to be made at values 11. Keywords
less than 1 %, then the sample boat with the residue of the tube
furnace burn shall be placed in a muffle furnace for approxi- 11.1 carbon black; gravimetric; plastics; polyolefins
mately 10 min to oxidize the carbon black. This is to correct for
the presence of residual inorganic matter in the sample. After
heating, cool the sample boat in a desiccator until it is at room
temperature. Weigh the boat plus contents to the nearest 0.0001
g (w4).
7.8 Make all determinations in duplicate.

8. Calculation 7
Supporting data for this test method is available from ASTM Headquarters.
8.1 Calculate the carbon black content as follows: Request RR: D20-1027.

SUMMARY OF CHANGES

This section identifies the location of selected changes to this test method. For the convenience of the user,
Committee D20 has highlighted those changes that may impact the use of this test method. This section may also
include descriptions of the changes or reasons for the changes, or both.

D1603 - 01: (5) Inserted Note 5, renumbered old Note 5 to 6 and added
(1) Changed or added inch/pound units in parentheses. Note 7.
(2) Added Terminology section. (6) Added w1, w2, w3, and w4 weight (mass) references in text
(3) Revised some parts of Apparatus section to reflect currently and to table in Calculations section.
available equipment.
(7) Added Summary of Changes section.
(4) Revised Procedure to reflect use of current equipment and
laboratory practices.

3
 D 1603
ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentioned
in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk
of infringement of such rights, are entirely their own responsibility.

This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and
if not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standards
and should be addressed to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of the
responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should
make your views known to the ASTM Committee on Standards, at the address shown below.

This standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,
United States. Individual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the above
address or at 610-832-9585 (phone), 610-832-9555 (fax), or service@[Link] (e-mail); or through the ASTM website
([Link]).