ASTM D4072-98(2018)
(Test Method)Standard Test Method for Toluene-Insoluble (TI) Content of Tar and Pitch
Standard Test Method for Toluene-Insoluble (TI) Content of Tar and Pitch
SIGNIFICANCE AND USE
4.1 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 7.
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
Relations
Buy Standard
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 − 98 (Reapproved 2018)
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 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. No other units of measurement are included in this
izing tars and pitches and as one element in establishing the
standard.
uniformity of shipments or sources of supply.
1.4 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the
5. Apparatus
responsibility of the user of this standard to establish appro-
5.1 Extraction Apparatus, Flask with metal cap condenser
priate safety, health, and environmental practices and deter-
as shown in Fig. 1.
mine the applicability of regulatory limitations prior to use.
5.2 Extraction Thimble, AlundumAN 485 coarse (formerly
For specific hazard information, see Section 7.
RA 98), 30 mm in diameter by 80 mm in height with flat
1.5 This international standard was developed in accor-
bottom.
dance with internationally recognized principles on standard-
ization established in the Decision on Principles for the
5.3 Thimble Cover, Paper cone, made by wetting with water
Development of International Standards, Guides and Recom-
a 70 mm filter paper normally folded in a small glass funnel,
mendations issued by the World Trade Organization Technical
and drying the funnel in an oven with the paper cone in place.
Barriers to Trade (TBT) Committee.
5.4 Sieves, U.S. Standard 600 µm (No. 30) and 250 µm (No.
60), conforming to Specification E11.
2. Referenced Documents
5.5 Heater, having a minimum capacity of 300 W per unit.
2.1 ASTM Standards:
D95 Test Method for Water in Petroleum Products and
6. Reagents
Bituminous Materials by Distillation
6.1 Toluene, Industrial Pure, meeting Specification D362.
D362 SpecificationforIndustrialGradeToluene(Withdrawn
(Warning—Flammable.)
1989)
D850 Test Method for Distillation of Industrial Aromatic
6.2 Concentrated Hydrochloric Acid. (Warning—
Hydrocarbons and Related Materials
Corrosive.)
D4296 Practice for Sampling Pitch
E11 Specification for Woven Wire Test Sieve Cloth and Test
7. Hazards
Sieves
7.1 Since toluene is a toxic and flammable substance, all
working areas should be efficiently hooded and kept free of
This test method is under the jurisdiction of ASTM Committee D02 on
sparks and flames.
Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of
7.2 Observe proper laboratory procedures for handling and
SubcommitteeD02.05onPropertiesofFuels,PetroleumCokeandCarbonMaterial.
Current edition approved Dec. 1, 2018. Published December 2018. Originally
diluting hydrochloric acid.
approved in 1981. Last previous edition approved in 2003 as D4072 – 98 (2013).
DOI: 10.1520/D4072-98R18.
8. Bulk Sampling
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
8.1 Samples from shipments shall be taken in accordance
Standards volume information, refer to the standard’s Document Summary page on
with Practice D4296, and shall be free of foreign substances.
the ASTM website.
Thoroughly mix the sample immediately before removing a
The last approved version of this historical standard is referenced on
www.astm.org. representative portion for the determination or for dehydration.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D4072 − 98 (2018)
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.
10.3 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.
10.4 Discard working samples 24 h after crushing and
sieving as changes in composition sometimes occur in pulver-
ized pitch.
11. Preparation of Extraction 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.
FIG. 1 Extraction Apparatus
11.1.1 Aftereachuse,ignitethethimbleat700 °Cto800 °C
for a few hours. Cool the thimble slowly by placing in a drying
9. Dehydration of Sample
oven for 1 h after removal from the furnace to prevent
cracking. Before reuse, condition the thimble as described in
9.1 Hard Pitch—If the solid bulk sample contains free
11.1.
water, air-dry a representative portion in a forced draft oven at
11.1.2 After repeated use, boil the thimble in 1 + 1 hydro-
50 °C.
chloric acid. (Add equal volume of concentrated hydrochloric
9.2 Soft Pitch—If the presence of water is indicated by
acid to distilled water.) to remove residual ash from the pores.
surface foam on heating, maintain a representative portion of
Then boil the thimble in distilled water and wash with water.
the bulk sample of a temperature between 125 °C and 150 °C
After drying at 105 °C, ignite and condition the thimble as
in an open container until the surface is free of foam.Take care
described in 11.1 and 11.1.1.
not to overheat, and remove heat source immediately when
foam subsides.
12. Procedure
9.3 Tar—Dehydrate a representative portion of the bulk
12.1 The mass of sample taken for analysis shall yield
sample at atmospheric pressure using a simple sidearm distil-
between 150 mg and 250 mg of matter insoluble in toluene
lation apparatus similar to the one in Test Method D850 and
(TI), unless this would require less than the minimum accept-
stop the distillation when the temperature reaches 170 °C.
able sample mass of 1 g, in which case 1 g shall be used.
Separate any oil from the water that has distilled over (if
crystals are present, warm sufficiently to ensure their solution)
12.2 Place the required amount of sample in a tared 150 mL
and thoroughly mix the oil with the residual tar in the still after
beaker and weigh to the nearest 0.5 mg. Pour 60 mLof toluene
the latter has cooled to a moderate temperature.
into the beaker, stirring continuously while introducing the
9.3.1 As an alternative to dehydration, the water content of
toluene, to ensure complete mixture of the s
...
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: D4072 − 98 (Reapproved 2018)
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 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. No other units of measurement are included in this
izing tars and pitches and as one element in establishing the
standard.
uniformity of shipments or sources of supply.
1.4 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the 5. Apparatus
responsibility of the user of this standard to establish appro-
5.1 Extraction Apparatus, Flask with metal cap condenser
priate safety, health, and environmental practices and deter-
as shown in Fig. 1.
mine the applicability of regulatory limitations prior to use.
5.2 Extraction Thimble, Alundum AN 485 coarse (formerly
For specific hazard information, see Section 7.
RA 98), 30 mm in diameter by 80 mm in height with flat
1.5 This international standard was developed in accor-
bottom.
dance with internationally recognized principles on standard-
ization established in the Decision on Principles for the
5.3 Thimble Cover, Paper cone, made by wetting with water
Development of International Standards, Guides and Recom-
a 70 mm filter paper normally folded in a small glass funnel,
mendations issued by the World Trade Organization Technical
and drying the funnel in an oven with the paper cone in place.
Barriers to Trade (TBT) Committee.
5.4 Sieves, U.S. Standard 600 µm (No. 30) and 250 µm (No.
60), conforming to Specification E11.
2. Referenced Documents
5.5 Heater, having a minimum capacity of 300 W per unit.
2.1 ASTM Standards:
D95 Test Method for Water in Petroleum Products and
6. Reagents
Bituminous Materials by Distillation
6.1 Toluene, Industrial Pure, meeting Specification D362.
D362 Specification for Industrial Grade Toluene (Withdrawn
(Warning—Flammable.)
1989)
D850 Test Method for Distillation of Industrial Aromatic
6.2 Concentrated Hydrochloric Acid. (Warning—
Hydrocarbons and Related Materials
Corrosive.)
D4296 Practice for Sampling Pitch
E11 Specification for Woven Wire Test Sieve Cloth and Test
7. Hazards
Sieves
7.1 Since toluene is a toxic and flammable substance, all
working areas should be efficiently hooded and kept free of
This test method is under the jurisdiction of ASTM Committee D02 on
sparks and flames.
Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of
7.2 Observe proper laboratory procedures for handling and
Subcommittee D02.05 on Properties of Fuels, Petroleum Coke and Carbon Material.
Current edition approved Dec. 1, 2018. Published December 2018. Originally
diluting hydrochloric acid.
approved in 1981. Last previous edition approved in 2003 as D4072 – 98 (2013).
DOI: 10.1520/D4072-98R18.
8. Bulk Sampling
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
8.1 Samples from shipments shall be taken in accordance
Standards volume information, refer to the standard’s Document Summary page on
with Practice D4296, and shall be free of foreign substances.
the ASTM website.
3 Thoroughly mix the sample immediately before removing a
The last approved version of this historical standard is referenced on
www.astm.org. representative portion for the determination or for dehydration.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D4072 − 98 (2018)
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.
10.3 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.
10.4 Discard working samples 24 h after crushing and
sieving as changes in composition sometimes occur in pulver-
ized pitch.
11. Preparation of Extraction 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.
FIG. 1 Extraction Apparatus
11.1.1 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
9. Dehydration of Sample
oven for 1 h after removal from the furnace to prevent
cracking. Before reuse, condition the thimble as described in
9.1 Hard Pitch—If the solid bulk sample contains free
11.1.
water, air-dry a representative portion in a forced draft oven at
11.1.2 After repeated use, boil the thimble in 1 + 1 hydro-
50 °C.
chloric acid. (Add equal volume of concentrated hydrochloric
9.2 Soft Pitch—If the presence of water is indicated by
acid to distilled water.) to remove residual ash from the pores.
surface foam on heating, maintain a representative portion of
Then boil the thimble in distilled water and wash with water.
the bulk sample of a temperature between 125 °C and 150 °C
After drying at 105 °C, ignite and condition the thimble as
in an open container until the surface is free of foam. Take care
described in 11.1 and 11.1.1.
not to overheat, and remove heat source immediately when
foam subsides.
12. Procedure
9.3 Tar—Dehydrate a representative portion of the bulk
12.1 The mass of sample taken for analysis shall yield
sample at atmospheric pressure using a simple sidearm distil-
between 150 mg and 250 mg of matter insoluble in toluene
lation apparatus similar to the one in Test Method D850 and
(TI), unless this would require less than the minimum accept-
stop the distillation when the temperature reaches 170 °C.
able sample mass of 1 g, in which case 1 g shall be used.
Separate any oil from the water that has distilled over (if
crystals are present, warm sufficiently to ensure their solution)
12.2 Place the required amount of sample in a tared 150 mL
and thoroughly mix the oil with the residual tar in the still after
beaker and weigh to the nearest 0.5 mg. Pour 60 mL of toluene
the latter has cooled to a moderate temperature.
into the beaker, stirring continuously while introducing the
9.3.1 As an alternative to dehydration, the water content of
toluene, to ensure complete mixture of the sample and toluene
the tar is determined by Test Method D95 and, if the water
and thorough disper
...
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 2013) D4072 − 98 (Reapproved 2018)
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
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 safety, health, and healthenvironmental practices and determine the
applicability of regulatory limitations prior to use. For specific hazard information, see Section 7.
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
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 as one element in establishing the
uniformity of shipments or sources of supply.
5. Apparatus
5.1 Extraction Apparatus, Flask with metal cap condenser as shown in Fig. 1.
5.2 Extraction Thimble, Alundum AN 485 coarse (formerly RA 98), 30 mm 30 mm in diameter by 80 mm 80 mm in height with
flat bottom.
5.3 Thimble Cover, Paper cone, made by wetting with water a 70-mm70 mm filter paper normally folded in a small glass funnel,
and drying the funnel in an oven with the paper cone in place.
5.4 Sieves, U.S. Standard 600-μmStandard 600 μm (No. 30) and 250-μm250 μm (No. 60), conforming to Specification E11.
5.5 Heater, having a minimum capacity of 300 W 300 W per unit.
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, 2013Dec. 1, 2018. Published August 2013December 2018. Originally approved in 1981. Last previous edition approved in 20082003
as D4072 – 98 (2008).(2013). DOI: 10.1520/D4072-98R13.10.1520/D4072-98R18.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at service@astm.org. 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.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D4072 − 98 (2018)
FIG. 1 Extraction Apparatus
6. Reagents
6.1 Toluene, Industrial Pure, meeting Specification D362. (Warning—Flammable.)
6.2 Concentrated Hydrochloric Acid. (Warning—Corrosive.)
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.
7.2 Observe proper laboratory procedures for handling and diluting hydrochloric acid.
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 in a forced draft oven at
50°C.50 °C.
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 remove heat source immediately when foam subsides.
9.3 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.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.
9.3.1 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 mass percent,10 % by mass, the TI content is corrected to a dry-tar basis (see 13.2). 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 24 h at room
temperature.
10. Preparation of Working Sample
10.1 Hard Pitch—If the pitch can be crushed at room temperature, prepare a 20-g20 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 5 mm in any dimension. Crush this
sample so that all of it will pass the 250-μm250 μm (No. 60) sieve. Store the sieved working sample in a tightly closed container
and use within 24 h 24 h (see 10.4).
10.2 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-μm600 μm (No. 30) sieve. Do not exceed 10 min 10 min for this
melting period. Pass the heated sample through the 600-μm600 μm sieve to remove foreign matter.
D4072 − 98 (2018)
10.3 Tar—Heat a representative portion of the tar to the lowest temperature that will permit passage through the 600-μm600 μm
(No. 30) sieve: then filter through this sieve to remove foreign matter.
10.4 Discard working samples 24 h 24 h after crushing and sieving as changes in composition sometimes occur in pulverized
pitch.
11. Preparation of Extraction Thimble
11.1 Dry the clean thi
...
Questions, Comments and Discussion
Ask us and Technical Secretary will try to provide an answer. You can facilitate discussion about the standard in here.