ASTM D4072-23

Standard Test Method for Toluene-Insoluble (TI) Content of Tar and Pitch

SIGNIFICANCE AND USE
5.1 This test method is useful for evaluating and characterizing tars and pitches and as one element in establishing the uniformity of shipments or sources of supply.
SCOPE
1.1 This test method covers the determination of toluene-insoluble matter (TI) in tar and pitch.  
1.2 Since this test method is empirical, strict adherence to all details of the procedure is necessary.  
1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
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. For specific hazard information, see Section 8.  
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: 30-Sep-2023
• ICS: 75.140 - Waxes, bituminous materials and other petroleum products
• Technical Committee: D02 - Petroleum Products, Liquid Fuels, and Lubricants
• Drafting Committee: D02.05 - Properties of Fuels, Petroleum Coke and Carbon Material

Relations

• Replaces: ASTM D4072-98(2018) - Standard Test Method for Toluene-Insoluble (TI) Content of Tar and Pitch
• Effective Date: 01-Oct-2023
• Refers: ASTM D4296-24 - Standard Practice for Sampling Pitch
• Effective Date: 01-Mar-2024
• Refers: ASTM D4175-23a - Standard Terminology Relating to Petroleum Products, Liquid Fuels, and Lubricants
• Effective Date: 15-Dec-2023
• Refers: ASTM D95-23 - Standard Test Method for Water in Petroleum Products and Bituminous Materials by Distillation
• Effective Date: 01-Oct-2023
• Refers: ASTM D4175-23e1 - Standard Terminology Relating to Petroleum Products, Liquid Fuels, and Lubricants
• Effective Date: 01-Jul-2023
• Refers: ASTM D4175-23 - Standard Terminology Relating to Petroleum Products, Liquid Fuels, and Lubricants
• Effective Date: 01-Jul-2023
• Refers: ASTM D4296-18 - Standard Practice for Sampling Pitch
• Effective Date: 01-Dec-2018
• Refers: ASTM D95-13(2018) - Standard Test Method for Water in Petroleum Products and Bituminous Materials by Distillation
• Effective Date: 01-Oct-2018
• Referred By: ASTM D4312-20 - Standard Test Method for Toluene-Insoluble (TI) Content of Tar and Pitch (Short Method)
• Effective Date: 01-Oct-2023
• Referred By: ASTM D2764-20 - Standard Test Method for Dimethylformamide-Insoluble (DMF-I) Content of Tar and Pitch
• Effective Date: 01-Oct-2023
• Referred By: ASTM D146/D146M-04(2020) - Standard Test Methods for Sampling and Testing Bitumen-Saturated Felts and Woven Fabrics for Roofing and Waterproofing
• Effective Date: 01-Oct-2023

Overview

ASTM D4072-23: Standard Test Method for Toluene-Insoluble (TI) Content of Tar and Pitch is an important ASTM International standard in the field of petroleum products and carbon materials. This empirical test method is designed specifically for the determination of the toluene-insoluble matter (TI) in tars and pitches. Accurate measurement of TI content is critical for evaluating and characterizing the quality of tar and pitch, as well as for establishing the uniformity of supply shipments.

The method strictly requires adherence to the detailed procedure to ensure the reliability and repeatability of results. Results are expressed in SI units and are used for technical, industrial, and procurement purposes, particularly in sectors utilizing tar and pitch for production processes.

Key Topics

• Toluene-Insoluble (TI) Content: The main focus is on measuring the matter in tar and pitch that is not soluble in toluene, which can impact material performance and quality.
• Sample Preparation: Detailed guidelines for selecting, handling, and preparing representative samples from shipments are provided to avoid bias and ensure accurate analysis.
• Test Procedure:
  • Digestion and extraction with hot toluene using a specialized apparatus and thimble
  • Precise washing, drying, and weighing processes to determine insoluble residue
  • Calculation of TI percentage and, if needed, correction to a dry-tar basis by measuring water content
• Precision and Bias: Repeatability and reproducibility data help laboratories assess data quality and compliance with international standards.
• Safety and Environmental Cautions: Includes guidance for laboratory safety, handling hazardous chemicals such as toluene and hydrochloric acid, and directions for developing appropriate health and safety practices.

Applications

The ASTM D4072-23 test method is widely applicable in:

• Quality Control in Manufacturing: Used by producers and buyers of tar and pitch to monitor product uniformity and quality prior to shipment or use in industrial processes.
• Material Characterization: Enables chemical and physical property assessment, which is essential for downstream applications in industries such as metallurgical coke production, aluminum smelting, and carbon electrode manufacturing.
• Supply Chain Management: Ensures consistency of raw material batches, supporting procurement processes and regulatory compliance.
• Research and Development: Laboratories involved in the study of petroleum-based materials and alternative carbon sources rely on standardized TI measurements for comparative analysis and innovation.

Related Standards

To support effective implementation, ASTM D4072-23 references several related ASTM standards:

• ASTM D95: Test Method for Water in Petroleum Products and Bituminous Materials by Distillation.
• ASTM D850: Test Method for Distillation of Industrial Aromatic Hydrocarbons and Related Materials.
• ASTM D4175: Terminology Relating to Petroleum Products, Liquid Fuels, and Lubricants.
• ASTM D4296: Practice for Sampling Pitch.
• ASTM E11: Specification for Woven Wire Test Sieve Cloth and Test Sieves.

These referenced standards provide critical definitions, sampling methodologies, and supporting measurement techniques necessary for comprehensive analysis.

---

Keywords: ASTM D4072-23, toluene-insoluble content, TI content, tar, pitch, petroleum products, quality control, material characterization, industrial standards, laboratory testing.

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: D4072 − 23
Standard Test Method for
Toluene-Insoluble (TI) Content of Tar and Pitch
This standard is issued under the fixed designation D4072; 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.
1. Scope* E11 Specification for Woven Wire Test Sieve Cloth and Test
Sieves
1.1 This test method covers the determination of toluene-
insoluble matter (TI) in tar and pitch.
3. Terminology
1.2 Since this test method is empirical, strict adherence to
3.1 Definitions:
all details of the procedure is necessary.
3.1.1 For definitions of terms used in this test method, refer
1.3 The values stated in SI units are to be regarded as
to Terminology D4175.
standard. No other units of measurement are included in this
standard.
4. Summary of Test Method
1.4 This standard does not purport to address all of the
4.1 The sample is digested, then extracted with hot toluene
safety concerns, if any, associated with its use. It is the
in an alundum thimble. The insoluble matter is dried and
responsibility of the user of this standard to establish appro-
weighed.
priate safety, health, and environmental practices and deter-
mine the applicability of regulatory limitations prior to use.
5. Significance and Use
For specific hazard information, see Section 8.
5.1 This test method is useful for evaluating and character-
1.5 This international standard was developed in accor-
izing tars and pitches and as one element in establishing the
dance with internationally recognized principles on standard-
uniformity of shipments or sources of supply.
ization established in the Decision on Principles for the
Development of International Standards, Guides and Recom-
6. Apparatus
mendations issued by the World Trade Organization Technical
6.1 Extraction Apparatus, Flask with metal cap condenser
Barriers to Trade (TBT) Committee.
as shown in Fig. 1.
2. Referenced Documents
6.2 Extraction Thimble, Alundum AN 485 coarse (formerly
2.1 ASTM Standards: RA 98), 30 mm in diameter by 80 mm in height with flat
D95 Test Method for Water in Petroleum Products and
bottom.
Bituminous Materials by Distillation
6.3 Thimble Cover, Paper cone, made by wetting with water
D362 Specification for Industrial Grade Toluene (Withdrawn
a 70 mm filter paper normally folded in a small glass funnel,
1989)
and drying the funnel in an oven with the paper cone in place.
D850 Test Method for Distillation of Industrial Aromatic
6.4 Sieves, U.S. Standard 600 μm (No. 30) and 250 μm (No.
Hydrocarbons and Related Materials
60), conforming to Specification E11.
D4175 Terminology Relating to Petroleum Products, Liquid
Fuels, and Lubricants
6.5 Heater, having a minimum capacity of 300 W per unit.
D4296 Practice for Sampling Pitch
7. Reagents
This test method is under the jurisdiction of ASTM Committee D02 on 7.1 Toluene, Industrial Pure, meeting Specification D362.
Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of
(Warning—Flammable.)
Subcommittee D02.05 on Properties of Fuels, Petroleum Coke and Carbon Material.
Current edition approved Oct. 1, 2023. Published October 2023. Originally 7.2 Concentrated Hydrochloric Acid. (Warning—
approved in 1981. Last previous edition approved in 2018 as D4072 – 18. DOI:
Corrosive.)
10.1520/D4072-23.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
8. Hazards
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
Standards volume information, refer to the standard’s Document Summary page on
8.1 Since toluene is a toxic and flammable substance, all
the ASTM website.
working areas should be efficiently hooded and kept free of
The last approved version of this historical standard is referenced on
www.astm.org. sparks and flames.
*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
D4072 − 23
crusher and a mullite mortar and pestle. No particle in the
representative sample shall be larger than 5 mm in any dimen-
sion. Crush this sample so that all of it will pass the 250 μm
(No. 60) sieve. Store the sieved working sample in a tightly
closed container and use within 24 h (see 11.4).
11.2 Soft Pitch—If the pitch is too soft to grind and too
sticky to mix, heat a representative portion of the dry sample to
the lowest temperature that will permit passage through the
600 μm (No. 30) sieve. Do not exceed 10 min for this melting
period. Pass the heated sample through the 600 μm sieve to
remove foreign matter.
11.3 Tar—Heat a representative portion of the tar to the
lowest temperature that will permit passage through the
600 μm (No. 30) sieve: then filter through this sieve to remove
foreign matter.
FIG. 1 Extraction Apparatus
11.4 Discard working samples 24 h after crushing and
sieving as changes in composition sometimes occur in pulver-
8.2 Observe proper laboratory procedures for handling and
ized pitch.
diluting hydrochloric acid.
12. Preparation of Extraction Thimble
9. Bulk Sampling
12.1 Dry the clean thimble in an oven at 105 °C 6 5 °C for
9.1 Samples from shipments shall be taken in accordance
45 min, cool in a desiccator, and weigh to the nearest 0.5 mg.
with Practice D4296, and shall be free of foreign substances.
Record the mass.
Thoroughly mix the sample immediately before removing a
12.1.1 After each use, ignite the thimble at 700 °C to 800 °C
representative portion for the determination or for dehydration.
for a few hours. Cool the thimble slowly by placing in a drying
oven for 1 h after removal from the furnace to prevent
10. Dehydration of Sample
cracking. Before reuse, condition the thimble as described in
10.1 Hard Pitch—If the solid bulk sample contains free
12.1.
water, air-dry a representative portion in a forced draft oven at 12.1.2 After repeated use, boil the thimble in 1 + 1 hydro-
50 °C.
chloric acid. (Add equal volume of concentrated hydrochloric
acid to distilled water.) to remove residual ash from the pores.
10.2 Soft Pitch—If the presence of water is indicated by
Then boil the thimble in distilled water and wash with water.
surface foam on heating, maintain a representative portion of
After drying at 105 °C, ignite and condition the thimble as
the bulk sample of a temperature between 125 °C and 150 °C
described in 12.1 and 12.1.1.
in an open container until the surface is free of foam. Take care
not to overheat and remove heat source immediately when
13. Procedure
foam subsides.
13.1 The mass of sample taken for analysis shall yield
10.3 Tar—Dehydrate a representative portion of the bulk
between 150 mg and 250 mg of matter insoluble in toluene
sample at atmospheric pressure using a simple sidearm distil-
(TI), unless this would require less than the minimum accept-
lation apparatus similar to the one in Test Method D850 and
able sample mass of 1 g, in which case 1 g shall be used.
stop the distillation when the temperature reaches 170 °C.
13.2 Place the required amount of sample in a tared 150 mL
Separate any oil from the water that has distilled over (if
beaker and weigh to the nearest 0.5 mg. Pour 60 mL of toluene
crystals are present, warm sufficiently to ensure their solution)
into the beaker, stirring continuously while introducing the
and thoroughly mix the oil with the residual tar in the still after
toluene, to ensure complete mixture of the sample and toluene
the latter has cooled to a moderate temperature.
and thorough dispersion of the insoluble matter (see 8.1). Place
10.3.1 As an alternative to dehydration, the water content of
the beaker o
...

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: D4072 − 98 (Reapproved 2018) D4072 − 23
Standard Test Method for
Toluene-Insoluble (TI) Content of Tar and Pitch
This standard is issued under the fixed designation D4072; 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.
1. Scope Scope*
1.1 This test method covers the determination of toluene-insoluble matter (TI) in tar and pitch.
1.2 Since this test method is empirical, strict adherence to all details of the procedure is necessary.
1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
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. For specific hazard information, see Section 78.
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.
2. Referenced Documents
2.1 ASTM Standards:
D95 Test Method for Water in Petroleum Products and Bituminous Materials by Distillation
D362 Specification for Industrial Grade Toluene (Withdrawn 1989)
D850 Test Method for Distillation of Industrial Aromatic Hydrocarbons and Related Materials
D4175 Terminology Relating to Petroleum Products, Liquid Fuels, and Lubricants
D4296 Practice for Sampling Pitch
E11 Specification for Woven Wire Test Sieve Cloth and Test Sieves
3. Terminology
3.1 Definitions:
3.1.1 For definitions of terms used in this test method, refer to Terminology D4175.
4. Summary of Test Method
4.1 The sample is digested, then extracted with hot toluene in an alundum thimble. The insoluble matter is dried and weighed.
This test method is under the jurisdiction of ASTM Committee D02 on Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of Subcommittee
D02.05 on Properties of Fuels, Petroleum Coke and Carbon Material.
Current edition approved Dec. 1, 2018Oct. 1, 2023. Published December 2018October 2023. Originally approved in 1981. Last previous edition approved in 20032018
as D4072 – 98 (2013).D4072 – 18. DOI: 10.1520/D4072-98R18.10.1520/D4072-23.
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.
The last approved version of this historical standard is referenced on www.astm.org.
*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
D4072 − 23
5. Significance and Use
5.1 This test method is useful for evaluating and characterizing tars and pitches and as one element in establishing the uniformity
of shipments or sources of supply.
6. Apparatus
6.1 Extraction Apparatus, Flask with metal cap condenser as shown in Fig. 1.
6.2 Extraction Thimble, Alundum AN 485 coarse (formerly RA 98), 30 mm in diameter by 80 mm in height with flat bottom.
6.3 Thimble Cover, Paper cone, made by wetting with water a 70 mm filter paper normally folded in a small glass funnel, and
drying the funnel in an oven with the paper cone in place.
6.4 Sieves, U.S. Standard 600 μm (No. 30) and 250 μm (No. 60), conforming to Specification E11.
6.5 Heater, having a minimum capacity of 300 W per unit.
7. Reagents
7.1 Toluene, Industrial Pure, meeting Specification D362. (Warning—Flammable.)
7.2 Concentrated Hydrochloric Acid. (Warning—Corrosive.)
8. Hazards
8.1 Since toluene is a toxic and flammable substance, all working areas should be efficiently hooded and kept free of sparks and
flames.
8.2 Observe proper laboratory procedures for handling and diluting hydrochloric acid.
9. Bulk Sampling
9.1 Samples from shipments shall be taken in accordance with Practice D4296, and shall be free of foreign substances. Thoroughly
mix the sample immediately before removing a representative portion for the determination or for dehydration.
10. Dehydration of Sample
10.1 Hard Pitch—If the solid bulk sample contains free water, air-dry a representative portion in a forced draft oven at 50 °C.
FIG. 1 Extraction Apparatus
D4072 − 23
10.2 Soft Pitch—If the presence of water is indicated by surface foam on heating, maintain a representative portion of the bulk
sample of a temperature between 125 °C and 150 °C in an open container until the surface is free of foam. Take care not to
overheat,overheat and remove heat source immediately when foam subsides.
10.3 Tar—Dehydrate a representative portion of the bulk sample at atmospheric pressure using a simple sidearm distillation
apparatus similar to the one in Test Method D850 and stop the distillation when the temperature reaches 170 °C. Separate any oil
from the water that has distilled over (if crystals are present, warm sufficiently to ensure their solution) and thoroughly mix the
oil with the residual tar in the still after the latter has cooled to a moderate temperature.
10.3.1 As an alternative to dehydration, the water content of the tar is determined by Test Method D95 and, if the water content
is less than 10 % by mass, the TI content is corrected to a dry-tar basis (see 13.214.2). This alternative method applies only to stable
emulsions of water in tar, that is, no water separates when the tar sample is left undisturbed for 24 h at room temperature.
11. Preparation of Working Sample
11.1 Hard Pitch—If the pitch can be crushed at room temperature, prepare a 20 g working sample by suitable crushing, mixing,
and quartering of a representative portion of the dry sample. The crushing can be done with a small jaw crusher and a mullite
mortar and pestle. No particle in the representative sample shall be larger than 5 mm in any dimension. Crush this sample so that
all of it will pass the 250 μm (No. 60) sieve. Store the sieved working sample in a tightly closed container and use within 24 h
(see 10.411.4).
11.2 Soft Pitch—If the pitch is too soft to grind and too sticky to mix, heat a representative portion of the dry sample to the lowest
temperature that will permit passage through the 600 μm (No. 30) sieve. Do not exceed 10 min for this melting period. Pass the
heated sample through the 600 μm sieve to remove foreign matter.
11.3 Tar—Heat a representative portion of the tar to the lowest temperature that will permit passage through the 600 μm (No. 30)
sieve: then filter through this sieve to remove foreign matter.
11.4 Discard working samples 24 h after crushing and sieving as changes in composition sometimes occur in pulverized pitch.
12. Preparation of Extraction Thimble
12.1 Dry the clean thimble in an oven at 105 °C 6 5 °C for 45 min, cool in a desiccator, and weigh to the nearest 0.5 mg. Record
the mass.
12.1.1 After each use, ignite the thimble at 700 °C to 800 °C for a few hours. Cool the thimble slowly by placing in a drying oven
for 1 h after removal from the furnace to prevent cracking. Before reuse, condition the thimble as described in 11.112.1.
12.1.2 After repeated use, boil the thimble in 1 + 1 hydrochloric acid. (Add equal volume of concentrated hydrochloric acid to
distilled water.) to remove residual ash from the pores. Then boil the thimble in distilled water and wash with water. After drying
at 105 °C, ignite and condition the thimble as described in 11.112.1 and 11.1.112.1.1.
13. Procedure
13.1 The mass of sample taken for analysis shall yield
...