ASTM D4312-15

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

SIGNIFICANCE AND USE
4.1 This test method is useful for evaluating and characterizing tars and pitches and is one element in establishing the uniformity of shipment 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.  
1.3.1 Exception—Other non-SI units are provided 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 and health practices and determine the applicability of regulatory limitations prior to use. Specific hazard statements are given in Section 7.

General Information

• Status: Historical
• Publication Date: 30-Nov-2015
• ICS: 91.100.50 - Binders. Sealing materials
• Technical Committee: D02 - Petroleum Products, Liquid Fuels, and Lubricants
• Drafting Committee: D02.05 - Properties of Fuels, Petroleum Coke and Carbon Material

Relations

• Replaces: ASTM D4312-95a(2010) - Standard Test Method for Toluene-Insoluble (TI) Content of Tar and Pitch (Short Method)
• Effective Date: 01-Dec-2015
• Replaced By: ASTM D4312-20 - Standard Test Method for Toluene-Insoluble (TI) Content of Tar and Pitch (Short Method)
• Effective Date: 01-Jun-2020
• 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-Dec-2015

Standards Content (Sample)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
Designation: D4312 − 15
Standard Test Method for
Toluene-Insoluble (TI) Content of Tar and Pitch (Short
1
Method)
This standard is issued under the fixed designation D4312; 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* 3. Summary of Test Method
1.1 This test method covers the determination of toluene- 3.1 The sample is digested, then extracted with hot toluene
insoluble matter (TI) in tar and pitch. in an alundum thimble. The insoluble matter is dried and
weighed.
1.2 Since this test method is empirical, strict adherence to
all details of the procedure is necessary.
4. Significance and Use
1.3 The values stated in SI units are to be regarded as
4.1 This test method is useful for evaluating and character-
standard.
izing tars and pitches and is one element in establishing the
1.3.1 Exception—Other non-SI units are provided for infor-
uniformity of shipment or sources of supply.
mation only.
5. Apparatus
1.4 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the
5.1 ExtractionApparatus, flask with metal cap condenser as
responsibility of the user of this standard to establish appro-
shown in Fig. 1.
priate safety and health practices and determine the applica-
5.2 Extraction Thimbles, Alundum AN 485 coarse (for-
bility of regulatory limitations prior to use. Specific hazard
merly RA98), 30 mm in diameter by 80 mm in height with flat
statements are given in Section 7.
bottom.
5.3 Sieves, U.S. Standard 600 µm (No. 30) and 250 µm (No.
2. Referenced Documents
2 60), conforming to Specification E11.
2.1 ASTM Standards:
5.4 Heater, having a minimum capacity of 300 W per unit.
D95 Test Method for Water in Petroleum Products and
Bituminous Materials by Distillation Ahot plate or other heaters that maintain the proper reflux rate
are acceptable.
D329 Specification for Acetone
D362 SpecificationforIndustrialGradeToluene(Withdrawn
3
6. Reagents
1989)
D850 Test Method for Distillation of Industrial Aromatic 6.1 Toluene, Industrial Pure, meeting Specification D362.
Hydrocarbons and Related Materials
6.2 Acetone, meeting the requirements of Specification
D4072 Test Method for Toluene-Insoluble (TI) Content of
D329.
Tar and Pitch
D4296 Practice for Sampling Pitch 7. Hazards
E11 Specification for Woven Wire Test Sieve Cloth and Test
7.1 Since toluene is a toxic and flammable substance, all
Sieves
working areas should be efficiently hooded and kept free of
sparks and flames.
1
This test method is under the jurisdiction of ASTM Committee D02 on
8. Bulk Sampling
Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of
SubcommitteeD02.05onPropertiesofFuels,PetroleumCokeandCarbonMaterial.
8.1 Samples from shipments shall be taken in accordance
Current edition approved Dec. 1, 2015. Published December 2015. Originally
with Practice D4296, and shall be free of foreign substances.
approved in 1983. Last previous edition approved in 2010 as D4312 – 95a (2010).
Thoroughly mix the sample immediately before removing a
DOI: 10.1520/D4312-15.
2
representative portion for the determination or for dehydration.
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 9. Dehydration of Sample
the ASTM website.
3
9.1 Hard Pitch—If the solid bulk sample contains free
The last approved version of this historical standard is referenced on
www.astm.org. water, air-dry a representative portion.
*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
1

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D4312 − 15
10.3 Tar—Heat a representative portion of the dry 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.
10.4 Discard working sample 24 h after crushing and
sieving as changes in composition sometimes occur in pulver-
ized pitch.
11. Preparation of Alundum Thimble
11.1 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.
11.1.1 Aftereachuse,ignitethethimbleat700 °Cto800 °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
FIG. 1 Extraction Apparatus
cracking. Before reuse, condition the thimble as described in
11.1.
...

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: D4312 − 95a (Reapproved 2010) D4312 − 15
Standard Test Method for
Toluene-Insoluble (TI) Content of Tar and Pitch (Short
1
Method)
This standard is issued under the fixed designation D4312; 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.
1.3.1 Exception—Other non-SI units are provided 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 and health practices and determine the applicability of regulatory
limitations prior to use. Specific hazard statements are given in Section 7.
2. Referenced Documents
2
2.1 ASTM Standards:
D95 Test Method for Water in Petroleum Products and Bituminous Materials by Distillation
D329 Specification for Acetone
3
D362 Specification for Industrial Grade Toluene (Withdrawn 1989)
D370 Practice for Dehydration of Oil-Type Preservatives
D850 Test Method for Distillation of Industrial Aromatic Hydrocarbons and Related Materials
D4072 Test Method for Toluene-Insoluble (TI) Content of Tar and Pitch
D4296 Practice for Sampling Pitch
E11 Specification for Woven Wire Test Sieve Cloth and Test Sieves
3. Summary of Test Method
3.1 The sample is digested, then extracted with hot toluene in an alundum thimble. The insoluble matter is dried and weighed.
4. Significance and Use
4.1 This test method is useful for evaluating and characterizing tars and pitches and is one element in establishing the uniformity
of shipment or sources of supply.
5. Apparatus
5.1 Extraction Apparatus, flask with metal cap condenser as shown in Fig. 1.
5.2 Extraction Thimbles, Alundum AN 485 coarse (formerly RA 98), 30 mm in diameter by 80 mm in height with flat bottom.
5.3 Sieves, U.S. Standard 600-μmStandard 600 μm (No. 30) and 250-μm250 μm (No. 60), conforming to Specification E11.
5.4 Heater, having a minimum capacity of 300 W per unit. A hot plate or other heaters that maintain the proper reflux rate are
acceptable.
1
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 May 1, 2010Dec. 1, 2015. Published May 2010December 2015. Originally approved in 1983. Last previous edition approved in 20052010 as
D4312D4312 – 95a (2010).–95a (2005). DOI: 10.1520/D4312-95R10.10.1520/D4312-15.
2
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.
3
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
1

---------------------- Page: 1 ----------------------
D4312 − 15
FIG. 1 Extraction Apparatus
6. Reagents
6.1 Toluene, Industrial Pure, meeting Specification D362.
6.2 Acetone, meeting the requirements of Specification D329.
7. Hazards
7.1 Since toluene is a toxic and flammable substance, all working areas should be efficiently hooded and kept free of sparks and
flames.
8. Bulk Sampling
8.1 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.
9. Dehydration of Sample
9.1 Hard Pitch—If the solid bulk sample contains free water, air-dry a representative portion.
9.2 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 125125 °C and 150°C150 °C in an open container until the surface is free of foam. Take care
not to overheat, and rem
...