ASTM D1603-20

Standard Test Method for Carbon Black Content in Olefin Plastics

SIGNIFICANCE AND USE
4.1 The information provided by this test method is useful for manufacturing quality control, technical service, and research purposes; and is required by various material specifications and for the calculation of optical absorptivity.  
4.2 Test Method D4218 is available for determining the carbon black content of polyethylene compounds if so desired.
SCOPE
1.1 This test method covers the determination of the carbon black content in polyethylene, polypropylene, and polybutylene plastics. Its use with acrylic or other polar monomer modifications which might affect the accuracy is not recommended. Determinations of carbon black content are made gravimetrically after pyrolysis of the sample under nitrogen. This test method is not applicable to compositions that contain nonvolatile pigments or fillers other than carbon black.  
1.1.1 This test method is not applicable to materials containing brominated flame retardant additives at the end.  
1.2 The values stated in SI units are to be regarded as standard. The values in parentheses are given 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, health, and environmental practices and determine the applicability of regulatory limitations prior to use.
Note 1: This standard and ISO 6964-1986(E) address the same subject matter, but differ in technical content.  
1.4 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

General Information

• Status: Published
• Publication Date: 31-Jan-2020
• ICS: 83.080.10 - Thermosetting materials
• Technical Committee: D20 - Plastics
• Drafting Committee: D20.70 - Analytical Methods

Relations

• Replaces: ASTM D1603-14 - Standard Test Method for Carbon Black Content in Olefin Plastics
• Effective Date: 01-Feb-2020
• Refers: ASTM D883-24 - Standard Terminology Relating to Plastics
• Effective Date: 01-Feb-2024
• Refers: ASTM D883-23 - Standard Terminology Relating to Plastics
• Effective Date: 01-Nov-2023
• Refers: ASTM E456-13a(2022)e1 - Standard Terminology Relating to Quality and Statistics
• Effective Date: 01-Apr-2022
• Refers: ASTM D883-20 - Standard Terminology Relating to Plastics
• Effective Date: 01-Jan-2020
• Refers: ASTM D883-19c - Standard Terminology Relating to Plastics
• Effective Date: 01-Aug-2019
• Refers: ASTM D883-19a - Standard Terminology Relating to Plastics
• Effective Date: 15-Apr-2019
• Refers: ASTM D883-19 - Standard Terminology Relating to Plastics
• Effective Date: 01-Feb-2019
• Refers: ASTM D883-18a - Standard Terminology Relating to Plastics
• Effective Date: 01-Dec-2018
• Refers: ASTM D883-18 - Standard Terminology Relating to Plastics
• Effective Date: 01-Nov-2018
• Refers: ASTM E456-13A(2017)e3 - Standard Terminology Relating to Quality and Statistics
• Effective Date: 01-Oct-2017
• Refers: ASTM E2935-17 - Standard Practice for Conducting Equivalence Testing in Laboratory Applications
• Effective Date: 01-Oct-2017
• Refers: ASTM E456-13A(2017)e1 - Standard Terminology Relating to Quality and Statistics
• Effective Date: 01-Oct-2017
• Refers: ASTM D883-17 - Standard Terminology Relating to Plastics
• Effective Date: 15-Aug-2017
• Refers: ASTM E2935-16 - Standard Practice for Conducting Equivalence Testing in Laboratory Applications
• Effective Date: 15-Nov-2016

Overview

ASTM D1603-20: Standard Test Method for Carbon Black Content in Olefin Plastics is a globally recognized test procedure developed by ASTM International. This method is designed for accurate determination of carbon black content in polyethylene, polypropylene, and polybutylene plastics by gravimetric analysis after pyrolysis of samples under nitrogen. Carbon black is widely used as a pigment and for its UV-protection properties in olefin plastics, making this standard essential for the plastics manufacturing industry, quality control laboratories, and materials research.

The information provided by ASTM D1603-20 is instrumental for manufacturing quality control, technical support, research and development, and for compliance with various material specifications. It is also critical in calculating the optical absorptivity of plastic materials.

Note: This method is not recommended for plastics with acrylic or other polar monomer modifications and is not suitable for materials containing nonvolatile pigments, fillers other than carbon black, or brominated flame retardant additives.

Key Topics

• Scope and Applicability
  • Applicable to polyethylene, polypropylene, and polybutylene plastics.
  • Not recommended for plastics with polar monomer modifications, nonvolatile fillers, or brominated flame retardants.
• Test Method Principle
  • Carbon black content is determined gravimetrically after the sample undergoes pyrolysis in a nitrogen atmosphere.
• Significance of Testing
  • Ensures consistency and quality in polymer products.
  • Helps verify material compliance with international specifications.
• Precision and Reproducibility
  • Repeatability and reproducibility have been studied across multiple laboratories to ensure reliable results.
• Safety and Compliance
  • Users are responsible for observing proper safety, health, and environmental practices.
  • Standard developed in line with internationally recognized principles, including those of the WTO Technical Barriers to Trade Committee.
• Reference to Alternatives
  • ASTM D4218 provides an alternative method for determining carbon black content in polyethylene compounds.

Applications

ASTM D1603-20 is widely adopted in industries that manufacture or utilize olefin-based plastics, ensuring the accurate measurement of carbon black content for:

• Manufacturing Quality Control:
  • Verifying that finished products meet desired performance and appearance specifications.
  • Preventing under- or over-addition of carbon black, which affects UV resistance and material properties.
• Research and Development:
  • Supporting material scientists in the evaluation and optimization of polymer formulations.
  • Assisting in the design of new products and comparison of competitive materials.
• Technical Service and Compliance:
  • Supporting infrastructure, automotive, and packaging sectors by validating material properties required by regulatory and customer specifications.
• Calculation of Optical Absorptivity:
  • Essential for assessing the effectiveness of carbon black in shielding against UV degradation.

Related Standards

• ASTM D4218: Test Method for Determination of Carbon Black Content in Polyethylene Compounds by the Muffle-Furnace Technique.
• ISO 6964: Polyolefin Pipes and Fittings - Determination of Carbon Black by Calcination and Pyrolysis - Test Method and Basic Specification.
• ASTM D883: Terminology Relating to Plastics.
• ASTM E691: Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method.

Summary

ASTM D1603-20 provides a robust and standardized approach to quantifying carbon black in olefin plastics, ensuring manufacturers and testing laboratories can uphold product quality, consistency, and compliance with industry and international requirements. This test method is critical for anyone involved with polyolefin materials where carbon black content must be tightly controlled for optimal performance and durability.

Standards Content (Sample)

This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
Designation:D1603 −20
Standard Test Method for
Carbon Black Content in Olefin Plastics
This standard is issued under the fixed designation D1603; 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 (´) indicates an editorial change since the last revision or reapproval.
This standard has been approved for use by agencies of the U.S. Department of Defense.
1. Scope* D4218 Test Method for Determination of Carbon Black
Content in Polyethylene Compounds By the Muffle-
1.1 This test method covers the determination of the carbon
Furnace Technique
black content in polyethylene, polypropylene, and polybuty-
E456 Terminology Relating to Quality and Statistics
lene plastics. Its use with acrylic or other polar monomer
E691 Practice for Conducting an Interlaboratory Study to
modifications which might affect the accuracy is not recom-
Determine the Precision of a Test Method
mended. Determinations of carbon black content are made
E2935 Practice for Conducting Equivalence Testing in
gravimetrically after pyrolysis of the sample under nitrogen.
Laboratory Applications
This test method is not applicable to compositions that contain
2.2 ISO Standard:
nonvolatile pigments or fillers other than carbon black.
ISO 6964-1986(E) Polyolefin Pipes and Fittings—
1.1.1 This test method is not applicable to materials con-
Determination of Carbon Black by Calcination and
taining brominated flame retardant additives at the end.
Pyrolysis—Test Method and Basic Specification
1.2 The values stated in SI units are to be regarded as
3. Terminology
standard. The values in parentheses are given for information
only.
3.1 Terms used in this standard are defined in accordance
with Terminology D883, unless otherwise specified. For terms
1.3 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the relating to precision and bias and associated issues, the terms
used in this standard are defined in accordance with Terminol-
responsibility of the user of this standard to establish appro-
priate safety, health, and environmental practices and deter- ogy E456.
mine the applicability of regulatory limitations prior to use.
4. Significance and Use
NOTE1—ThisstandardandISO6964-1986(E)addressthesamesubject
4.1 The information provided by this test method is useful
matter, but differ in technical content.
for manufacturing quality control, technical service, and re-
1.4 This international standard was developed in accor-
search purposes; and is required by various material specifica-
dance with internationally recognized principles on standard-
tions and for the calculation of optical absorptivity.
ization established in the Decision on Principles for the
4.2 Test Method D4218 is available for determining the
Development of International Standards, Guides and Recom-
carbon black content of polyethylene compounds if so desired.
mendations issued by the World Trade Organization Technical
Barriers to Trade (TBT) Committee.
5. Apparatus
5.1 Electric Furnace, at least 20 cm (7.9 in.) long suitable
2. Referenced Documents
for use with the tubing described in 5.2.
2.1 ASTM Standards:
5.2 High Temperature Glass Combustion Tube , of appro-
D883 Terminology Relating to Plastics
priate diameter and approximately twice as long as the furnace
described in 5.1.
1 5.3 Stoppers—Two rubber or neoprene stoppers, to fit the
This test method is under the jurisdiction ofASTM Committee D20 on Plastics
and is the direct responsibility of Subcommittee D20.70 on Analytical Methods
tube described in 5.2, unless the tube is fitted with ground
(Section D20.70.01).
joints and mating connectors.
Current edition approved Feb. 1, 2020. Published March 2020. Originally
approved in 1958. Last previous edition approved in 2014 as D1603 - 14. DOI:
10.1520/D1603-20. ISO/IEC Selected Standards for Testing Plastics, Second Edition, published by
For referenced ASTM standards, visit the ASTM website, www.astm.org, or ASTM. Also available from American National Standards Institute (ANSI), 25 W.
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM 43rd St., 4th Floor, New York, NY 10036.
Standards volume information, refer to the standard’s Document Summary page on Borosilicate, high-silica, or equivalent glass tubing has been found satisfactory
the ASTM website. for this purpose.
*A Summary of Changes section appears at the end of this standard
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D1603−20
5.4 Glass Tubing, approximately 10 mm (0.39 in.) in 5.13 Balance—An analytical balance having a sensitivity of
diameter, of sufficient amount, and matching rubber or plastic 0.0001 g.
tubing for connections.
6. Reagents and Materials
5.5 Combustion Boat, approximately 8 by 1.9 by 1.3 cm
(3.15 by 0.75 by 0.51 in.). Glazed porcelain, quartz high-silica
6.1 Carbon Dioxide, Solid (Dry Ice).
glass, or platinum is suitable.
NOTE 5—The solid carbon dioxide and the trichloroethylene are not
NOTE 2—A loose-fitting cover for the combustion boat is optional. If
required if the entire apparatus train is placed in a fume hood.
used, it shall be considered a part of the boat and handled and weighed
with it.
6.2 Desiccant, such as anhydrous calcium chloride (CaCl ).
5.6 Iron-Constantan Thermocouple, and a potentiometer or
6.3 Nitrogen, prepurified, having oxygen content below
millivoltmeter suitable for determining temperatures in the
0.01 %. As a safeguard against accidental leakage,
range 300 to 700°C (572 to 1292°F).
contamination, or inadequate purity, the gas shall be further
5.7 Flow Meter, suitable for measuring gas flow at rates of
purified by one of the following procedures:
1 to 10 L/min.
6.3.1 Passage of the nitrogen through a glass trap inserted
5.8 Traps, three glass traps with removable ground-glass
ahead of the drying tube (see Fig. 1), filled approximately one
connected heads and 10-mm (0.39-in.) diameter inner and
third full of potassium hydroxide - pyrogallol solution made to
connecting tubes.
contain5gof pyrogallol and 50 g of KOH in 100 mLof water.
NOTE 3—Only one trap is required if the entire apparatus train is placed Technical grade, or better, reagents are satisfactory.
in a fume hood. None is required if in addition, nitrogen of sufficient
6.3.2 Insertion of a plug, or roll, of clean copper tinsel, foil,
purity is used and produced by the alternative means provided in Section
or wire 7.5 to 10 cm (3 to 4 in.) long into the combustion tube
6.
ahead of the sample (see Fig. 1) so that it is completely within
5.9 DryingTube—AU-shaped drying tube, having an inside
the heated region of the furnace. Take care to prevent chan-
diameter of 20 mm (0.79 in.) or larger, fitted with ground glass
neling of the nitrogen through the plug. The extent of black-
or neoprene stoppers.
ening of the copper may be taken as a guide for determining
5.10 Glass Wool.
when the plug should be renewed.
5.11 Desiccator, with desiccant.
6.3.3 Passage of the nitrogen through a combustion tube
filled to a length of 15 cm (6 in.) or greater with clean copper
5.12 BunsenBurnerorMuffleFurnace—Electricresistance-
heated or microwave-heated furnace capable of heating the tinsel, foil, or wire, and maintained in a furnace at a tempera-
combustion boat to red heat. ture around 500°C (932°F).
6.3.4 The need for the procedures described is eliminated if
NOTE 4—When an electric furnace is used, position it in a well-
ventilated hood. When a microwave furnace is used, position it within or gas having an oxygen content of less than 0.002 % (20 ppm) is
adjacenttoahoodandtheexhausttubeventedintothehoodtopreventthe
used.
breathingofbyproductsofanycombustion.Anairflowrateof2.8m /min
through the microwave oven is recommended. 6.4 Trichloroethylene, tec
...

This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
Designation: D1603 − 14 D1603 − 20
Standard Test Method for
Carbon Black Content in Olefin Plastics
This standard is issued under the fixed designation D1603; 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 (´) indicates an editorial change since the last revision or reapproval.
This standard has been approved for use by agencies of the U.S. Department of Defense.
1. Scope*
1.1 This test method covers the determination of the carbon black content in polyethylene, polypropylene, and polybutylene
plastics. Its use with acrylic or other polar monomer modifications which might affect the accuracy is not recommended.
Determinations of carbon black content are made gravimetrically after pyrolysis of the sample under nitrogen. This test method
is not applicable to compositions that contain nonvolatile pigments or fillers other than carbon black.
1.1.1 This test method is not applicable to materials containing brominated flame retardant additives at the end.
1.2 The values stated in SI units are to be regarded as standard. The values in parentheses are given 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 safety, health, and healthenvironmental practices and determine the
applicability of regulatory limitations prior to use.
NOTE 1—This standard and ISO 6964-1986(E) address the same subject matter, but differ in technical content.
1.4 This international standard was developed in accordance with internationally recognized principles on standardization
established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued
by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
2. Referenced Documents
2.1 ASTM Standards:
D883 Terminology Relating to Plastics
D4218 Test Method for Determination of Carbon Black Content in Polyethylene Compounds By the Muffle-Furnace Technique
E177E456 Practice for Use of the Terms Precision and Bias in ASTM Test MethodsTerminology Relating to Quality and
Statistics
E691 Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method
E2935 Practice for Conducting Equivalence Testing in Laboratory Applications
2.2 ISO Standard:
ISO 6964-1986(E) Polyolefin Pipes and Fittings—Determination of Carbon Black by Calcination and Pyrolysis—Test Method
and Basic Specification
3. Terminology
3.1 Definitions—For definitions of technical Terms used in this standard are defined in accordance with Terminology D883terms
pertaining to plastics , unless otherwise specified. For terms relating to precision and bias and associated issues, the terms used
in this specification, see standard are defined in accordance with Terminology D883E456.
4. Significance and Use
4.1 The information provided by this test method is useful for manufacturing quality control, technical service, and research
purposes; and is required by various material specifications and for the calculation of optical absorptivity.
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 (Section
D20.70.01).
Current edition approved Aug. 1, 2014Feb. 1, 2020. Published August 2014March 2020. Originally approved in 1958. Last previous edition approved in 20122014 as
D1603 - 12.D1603 - 14. DOI: 10.1520/D1603-14.10.1520/D1603-20.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
ISO/IEC Selected Standards for Testing Plastics, Second Edition, published by ASTM. Also available from American National Standards Institute (ANSI), 25 W. 43rd
St., 4th Floor, New York, NY 10036.
*A Summary of Changes section appears at the end of this standard
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D1603 − 20
4.2 Test Method D4218 is available for determining the carbon black content of polyethylene compounds if so desired.
5. Apparatus
5.1 Electric Furnace, at least 20 cm (7.9 in.) long suitable for use with the tubing described in 5.2.
5.2 High Temperature Glass Combustion Tube , of appropriate diameter and approximately twice as long as the furnace
described in 5.1.
5.3 Stoppers—Two rubber or neoprene stoppers, to fit the tube described in 5.2, unless the tube is fitted with ground joints and
mating connectors.
5.4 Glass Tubing, approximately 10 mm (0.39 in.) in diameter, of sufficient amount, and matching rubber or plastic tubing for
connections.
5.5 Combustion Boat, approximately 8 by 1.9 by 1.3 cm (3.15 by 0.75 by 0.51 in.). Glazed porcelain, quartz high-silica glass,
or platinum is suitable.
NOTE 2—A loose-fitting cover for the combustion boat is optional. If used, it shall be considered a part of the boat and handled and weighed with it.
5.6 Iron-Constantan Thermocouple, and a potentiometer or millivoltmeter suitable for determining temperatures in the range
300 to 700°C (572 to 1292°F).
5.7 Flow Meter, suitable for measuring gas flow at rates of 1 to 10 L/min.
5.8 Traps, three glass traps with removable ground-glass connected heads and 10-mm (0.39-in.) diameter inner and connecting
tubes.
NOTE 3—Only one trap is required if the entire apparatus train is placed in a fume hood. None is required if in addition, nitrogen of sufficient purity
is used and produced by the alternative means provided in Section 6.
5.9 Drying Tube—A U-shaped drying tube, having an inside diameter of 20 mm (0.79 in.) or larger, fitted with ground glass or
neoprene stoppers.
5.10 Glass Wool.
5.11 Desiccator, with desiccant.
5.12 Bunsen Burner or Muffle Furnace—Electric resistance-heated or microwave-heated furnace capable of heating the
combustion boat to red heat.
NOTE 4—When an electric furnace is used, position it in a well-ventilated hood. When a microwave furnace is used, position it within or adjacent to
a hood and the exhaust tube vented into the hood to prevent the breathing of byproducts of any combustion. An air flow rate of 2.8 m /min through the
microwave oven is recommended.
5.13 Balance—An analytical balance having a sensitivity of 0.0001 g.
6. Reagents and Materials
6.1 Carbon Dioxide, Solid (Dry Ice).
NOTE 5—The solid carbon dioxide and the trichloroethylene are not required if the entire apparatus train is placed in a fume hood.
6.2 Desiccant, such as anhydrous calcium chloride (CaCl ).
6.3 Nitrogen, prepurified, having oxygen content below 0.01 %. As a safeguard against accidental leakage, contamination, or
inadequate purity, the gas shall be further purified by one of the following procedures:
6.3.1 Passage of the nitrogen through a glass trap inserted ahead of the drying tube (see Fig. 1), filled approximately one third
full of potassium hydroxide - pyrogallol solution made to contain 5 g of pyrogallol and 50 g of KOH in 100 mL of water. Technical
grade, or better, reagents are satisfactory.
6.3.2 Insertion of a plug, or roll, of clean copper tinsel, foil, or wire 7.5 to 10 cm (3 to 4 in.) long into the combustion tube ahead
of the sample (see Fig. 1) so that it is completely within the heated region of the furnace. Take care to prevent channeling of the
nitrogen through the plug. The extent of blackening of the copper may be taken as a guide for determining when the plug should
be renewed.
6.3.3 Passage of the nitrogen through a combustion tube filled to a length of 15 cm (6 in.) or greater with clean copper tinsel,
foil, or wire, and maintained in a furnace at a temperature around 500°C (932°F).
6.3.4 The need for the procedures described is eliminated if gas having an oxygen content of less than 0.002 % (20 ppm) is used.
6.4 Trichloroethylene, technical grade (Note 5).
Borosilicate, high-silica, or equivalent glass tubing has been found satisfactory for this purpose.
D1603 − 20
FIG. 1 Assembly of Apparatus
7. Sampling and Test Specs
7.1 The test specimens can be in a variety of forms which fit in the combustion boat but must satisfy the requirements of 8.3.
Soiled articles must be washed and printed articles are wiped clean with a suitable solvent.
8. Procedure
NOTE 6—The procedure below assumes that the combustion tube can be easily removed from the furnace. If this is not the case, alternate methods of
inserting and removing sample boats are acceptable as long as the temperature, purge time, and flow rate requirements are met.
8.1 Assemble the apparatus as shown in Fig. 1. Both cold traps following the combustion tube shall contain trichloroethylene,
but only the first need be cooled with solid carbon dioxide. Alternatively, the entire apparatus may be placed in a fume hood and
the two traps following the combustion tube omitted. Fill the drying tube with anhydrous CaCl or other suitable desiccant. Hold
between loose plugs of glass wool.
8.2 Heat a clean c
...