ASTM D1509-18(2023)

Standard Test Methods for Carbon Black-Heating Loss

SIGNIFICANCE AND USE
4.1 In addition to determining the heating loss (primarily moisture content) of carbon black, these drying conditions are used to prepare samples prior to performing other carbon black tests.  
4.2 When larger samples are prepared for other tests, use an open vessel of suitable dimensions so that the depth of the black is no more than 10 mm during conditioning.  
4.3 Carbon black is hygroscopic. The amount of moisture absorbed is related to the surface area of the black and to the relative humidity, ambient temperature, and time to which the material is exposed.
SCOPE
1.1 These test methods cover the determination of the heating loss of carbon black at 125°C. This heating loss consists primarily of moisture, but other volatile materials may also be lost. These test methods are not applicable to treated carbon blacks that contain added volatile materials, if moisture loss is to be measured.  
1.2 These test methods may also be used for the determination of the heating loss of recovered carbon fillers (rCF/rCB) at 125°C. However, these materials were not included in the precision studies and therefore, the precision statements contained in this standard may not be valid for these materials.  
1.3 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.  
1.4 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.  
1.5 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-Dec-2022
• ICS: 83.040.20 - Rubber compounding ingredients
• Technical Committee: D24 - Carbon Black
• Drafting Committee: D24.31 - Non-Carbon Black Components of Carbon Black

Relations

• Refers: ASTM D1900-06(2015) - Standard Practice for Carbon Black—Sampling Bulk Shipments
• Effective Date: 01-Nov-2015
• Refers: ASTM D1799-03a(2014) - Standard Practice for Carbon Black—Sampling Packaged Shipments
• Effective Date: 01-Jun-2014
• Refers: ASTM D1900-06(2011) - Standard Practice for Carbon Black<char: emdash>Sampling Bulk Shipments
• Effective Date: 01-May-2011
• Refers: ASTM D1799-03a(2008) - Standard Practice for Carbon Black<span class='unicode'>&#x2014;</span>Sampling Packaged Shipments
• Effective Date: 01-Sep-2008
• Refers: ASTM D1900-06 - Standard Practice for Carbon Black-Sampling Bulk Shipments
• Effective Date: 01-Oct-2006
• Refers: ASTM D1799-03a - Standard Practice for Carbon Black&#8212;Sampling Packaged Shipments
• Effective Date: 01-Nov-2003
• Refers: ASTM D1799-03 - Standard Practice for Carbon Black&#8212;Sampling Packaged Shipments
• Effective Date: 10-Jun-2003
• Refers: ASTM D1799-02 - Standard Practice for Carbon Black&#8212;Sampling Packaged Shipments
• Effective Date: 10-Nov-2002
• Refers: ASTM D1799-93(1997) - Standard Practice for Carbon Black-Sampling Packaged Shipments
• Effective Date: 10-Nov-1997
• Refers: ASTM D1900-94(2002) - Standard Practice for Carbon Black&#8212;Sampling Bulk Shipments
• Effective Date: 15-Aug-1994

Overview

ASTM D1509-18(2023), Standard Test Methods for Carbon Black-Heating Loss, establishes reliable procedures for measuring the heating loss of carbon black at 125°C. The heating loss primarily reflects moisture content but may include other volatile components. These methods support quality control in carbon black production and use, as well as sample preparation for further testing. The standard is developed and maintained by ASTM International, and follows globally recognized guidelines for consistency and accuracy.

Key Topics

• Heating Loss Determination:
  The heating loss is quantified by weighing a carbon black sample before and after heating at 125°C, using either a convection-gravity oven or a moisture balance. The difference in mass represents the heating loss.

• Scope and Applicability:

  • Applicable to untreated carbon black and recovered carbon fillers (rCF/rCB).
  • Not intended for treated carbon blacks containing added volatile materials.
  • Results are reported in SI units and to the nearest 0.1%.

• Sample Preparation and Handling:

  • Samples must be conditioned in open vessels with a maximum depth of 10 mm for larger tests.
  • All samples should be stored in airtight containers and allowed to reach room temperature before testing to prevent moisture variation due to hygroscopicity.

• Significance in Testing:

  • Accurate determination of heating loss ensures consistent moisture content, critical for downstream testing and quality assessments.
  • The standardized drying protocol serves as a preparation step for various other carbon black analyses.

• Precision and Reporting:

  • Repeatability and reproducibility parameters enable laboratories to assess the confidence and comparability of results.
  • Detailed reporting is required, including sample identification and precise result values.

Applications

• Quality Control in Manufacturing:
  Used throughout the carbon black industry to monitor moisture and volatile loss, ensuring product consistency and compliance with technical specifications.

• Sample Conditioning for Further Testing:
  Proper drying of carbon black prior to additional analyses (such as surface area, structure, or chemical characteristics) improves accuracy and repeatability in laboratory environments.

• Recovered Carbon Fillers (rCF/rCB):
  The method extends to recovered carbon fillers, supporting recycling efforts and secondary material processing; however, stated precision limits may not directly apply.

• Moisture Sensitivity in End Products:
  Accurate heating loss determination is crucial for end-use products (including rubber and plastics) where residual moisture or volatile material can adversely affect performance or processability.

Related Standards

• ASTM D1799: Practice for Carbon Black-Sampling Packaged Shipments
  Guidance on representative sampling, necessary for ensuring test accuracy.

• ASTM D1900: Practice for Carbon Black-Sampling Bulk Shipments
  Procedures for bulk sampling, particularly applicable for large shipments.

• ASTM D4483: Practice for Evaluating Precision for Test Method Standards in the Rubber and Carbon Black Manufacturing Industries
  Essential reference for understanding and evaluating test method variability and precision.

Practical Value

ASTM D1509-18(2023) is widely used in the carbon black industry to quantify heating loss, primarily moisture content, ensuring materials meet stringent quality requirements. The standard supports laboratories and manufacturers by offering repeatable and reliable test methods, promoting comparability across production batches and testing facilities. Consistent moisture measurement helps safeguard product quality and optimizes further material testing processes.

Keywords: carbon black, heating loss, moisture content, volatile materials, ASTM D1509, standardized test methods, sample preparation, quality control, recovered carbon fillers (rCF/rCB)

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: D1509 − 18 (Reapproved 2023)
Standard Test Methods for
Carbon Black—Heating Loss
This standard is issued under the fixed designation D1509; 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 D1900 Practice for Carbon Black—Sampling Bulk Ship-
ments
1.1 These test methods cover the determination of the
D4483 Practice for Evaluating Precision for Test Method
heating loss of carbon black at 125°C. This heating loss
Standards in the Rubber and Carbon Black Manufacturing
consists primarily of moisture, but other volatile materials may
Industries
also be lost. These test methods are not applicable to treated
carbon blacks that contain added volatile materials, if moisture
3. Summary of Test Method
loss is to be measured.
3.1 A carbon black sample is weighed before and after
1.2 These test methods may also be used for the determi-
heating for 1 h at 125°C. The observed difference in mass is the
nation of the heating loss of recovered carbon fillers (rCF/rCB)
heating loss.
at 125°C. However, these materials were not included in the
precision studies and therefore, the precision statements con-
4. Significance and Use
tained in this standard may not be valid for these materials.
4.1 In addition to determining the heating loss (primarily
1.3 The values stated in SI units are to be regarded as the
moisture content) of carbon black, these drying conditions are
standard. The values given in parentheses are for information
used to prepare samples prior to performing other carbon black
only.
tests.
1.4 This standard does not purport to address all of the
4.2 When larger samples are prepared for other tests, use an
safety concerns, if any, associated with its use. It is the
open vessel of suitable dimensions so that the depth of the
responsibility of the user of this standard to establish appro-
black is no more than 10 mm during conditioning.
priate safety, health, and environmental practices and deter-
4.3 Carbon black is hygroscopic. The amount of moisture
mine the applicability of regulatory limitations prior to use.
absorbed is related to the surface area of the black and to the
1.5 This international standard was developed in accor-
relative humidity, ambient temperature, and time to which the
dance with internationally recognized principles on standard-
material is exposed.
ization established in the Decision on Principles for the
Development of International Standards, Guides and Recom-
Method A—Convection–Gravity Oven Method
mendations issued by the World Trade Organization Technical
Barriers to Trade (TBT) Committee.
5. Apparatus
5.1 Oven, gravity-convection type, capable of temperature
2. Referenced Documents
regulation of within 61°C at 125°C and temperature unifor-
2.1 ASTM Standards:
mity within 65°C.
D1799 Practice for Carbon Black—Sampling Packaged
5.2 Weighing Bottle, low-form, 30 mm in height and 60 mm
Shipments
in diameter, equipped with a ground-glass stopper.
5.3 Analytical Balance, having a sensitivity of 0.1 mg.
5.4 Desiccator.
These test methods are under the jurisdiction of ASTM Committee D24 on
Carbon Black and are the direct responsibility of Subcommittee D24.31 on
Non-Carbon Black Components of Carbon Black.
6. Sampling
Current edition approved Jan. 1, 2023. Published February 2023. Originally
6.1 Samples shall be taken in accordance with Practices
approved in 1957. Last previous edition approved in 2018 as D1509 – 18. DOI:
10.1520/D1509-18R23.
D1799 or D1900.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
6.1.1 Place the samples of carbon black in airtight sample
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
containers. Allow the closed container to reach room tempera-
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. ture before starting the test.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D1509 − 18 (2023)
7. Procedure 10. Precision and Bias
7.1 Dry the weighing bottle and the stopper, with the
10.1 This precision and bias statement has been prepared in
stopper removed, in the specified oven set at 125°C for 30 min.
accordance with Practice D4483. Refer to Practice D4483 for
Place the bottle and stopper in the desiccator and allow to cool
terminology and other statistical details.
to room temperature. Weigh the bottle with stopper to the
10.2 Precision—The precision results in this precision and
nearest 0.1 mg.
bias section give an estimate of the precision of this test
7.2 Weigh 2 g of carbon black into the weighing bottle to the
method with the materials (rubbers, carbon blacks, etc.) used in
nearest 0.1 mg.
the particular interlaboratory program described in 10.3 –
10.3.2. The precision parameters should not be used for
7.3 Place the weighing bottle, sample, and stopper in the
acceptance or rejection testing of any group of materials
specified oven set at 125°C for 1 h with the stopper removed.
without documentation that they are applicable to those par-
7.4 Replace the stopper and transfer the bottle and contents
ticular materials and the specific testing protocols of the test
to the desiccator. Remove the stopper and allow to cool to
method.
room temperature. Replace the stopper on the weighing bottle
and reweigh to the nearest 0.1 mg. 10.3 Convection-Gravity Oven—Test Method A—A Type 1
interlaboratory precision program was conducted in 1994. Both
NOTE 1—Keep the stopper on the weighing bottle when transferring to
...