ASTM D4072-98
(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
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 the standard.
1.4 This standard does not purport to address all of the safety concerns, 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. For specific hazard information, see Section 7.
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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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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: D 4072 – 98 An American National Standard
AMERICAN SOCIETY FOR TESTING AND MATERIALS
100 Barr Harbor Dr., West Conshohocken, PA 19428
Reprinted from the Annual Book of ASTM Standards. Copyright ASTM
Standard Test Method for
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Toluene-Insoluble (TI) Content of Tar and Pitch
This standard is issued under the fixed designation D 4072; 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 (e) indicates an editorial change since the last revision or reapproval.
1. Scope 5. Apparatus
1.1 This test method covers the determination of toluene- 5.1 Extraction Apparatus—Flask with metal cap condenser
insoluble matter (TI) in tar and pitch. as shown in Fig. 1.
1.2 Since this test method is empirical, strict adherence to 5.2 Extraction Thimble, Alundum AN 485 coarse (formerly
all details of the procedure is necessary. RA 98), 30 mm in diameter by 80 mm in height with flat
1.3 The values stated in SI units are to be regarded as the bottom.
standard. 5.3 Thimble Cover—Paper cone, made by wetting with
1.4 This standard does not purport to address all of the water a 70-mm filter paper normally folded in a small glass
safety concerns, if any, associated with its use. It is the funnel, and drying the funnel in an oven with the paper cone in
responsibility of the user of this standard to establish appro- place.
priate safety and health practices and determine the applica- 5.4 Sieves, U.S. Standard 600-μm (No. 30) and 250-μm (No.
bility of regulatory limitations prior to use. For specific hazard 60), conforming to Specification E 11.
information, see Section 7. 5.5 Heater, having a minimum capacity of 300 W per unit.
2. Referenced Documents 6. Reagents
2.1 ASTM Standards: 6.1 Toluene, Industrial Pure, meeting Specification D 362.
D 95 Test Method for Water in Petroleum Products and
NOTE 1—Warning: Flammable.
2
Bituminous Materials by Distillation
3 6.2 Concentrated Hydrochloric Acid.
D 362 Specification for Industrial Grade Toluene
D 850 Test Method for Distillation of Industrial Aromatic
NOTE 2—Warning: Corrosive.
3
Hydrocarbons and Related Materials
4
7. Hazards
D 4296 Practice for Sampling Pitch
E 11 Specification for Wire-Cloth Sieves for Testing Pur-
7.1 Since toluene is a toxic and flammable substance, all
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poses
working areas should be efficiently hooded and kept free of
sparks and flames.
3. Summary of Test Method
7.2 Observe proper laboratory procedures for handling and
3.1 The sample is digested, then extracted with hot toluene
diluting hydrochloric acid.
in an alundum thimble. The insoluble matter is dried and
8. Bulk Sampling
weighed.
8.1 Samples from shipments shall be taken in accordance
4. Significance and Use
with Practice D 4296, and shall be free of foreign substances.
4.1 This test method is useful for evaluating and character-
Thoroughly mix the sample immediately before removing a
izing tars and pitches and as one element in establishing the
representative portion for the determination or for dehydration.
uniformity of shipments or sources of supply.
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
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This test method is under the jurisdiction of ASTM Committee D-2 on
50°C.
Petroleum Products and Lubricantsand is the direct responsibility of Subcommittee
D02.05.OFon Industrial Pitches. 9.2 Soft Pitch—If the presence of water is indicated by
Current edition approved Dec. 10, 1998. Published February 1999. Originally
surface foam on heating, maintain a representative portion of
published as D 4072 – 81. Last previous edition D 4072 – 97.
the bulk sample of a temperature between 125 and 150°C in an
2
Annual Book of ASTM Standards, Vol 05.01.
3
open container until the surface is free of foam. Take care not
Annual Book of ASTM Standards, Vol 06.03.
4
Annual Book of ASTM Standards, Vol 04.04.
5
Annual Book of ASTM Standards, Vol 14.02.
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NOTICE:¬This¬standard¬has¬either¬been¬superceded¬and¬replaced¬by¬a¬new¬version¬or¬discontinued.¬
Contact¬ASTM¬International¬(www.astm.org)¬for¬the¬latest¬information.¬
D 4072
11. Preparation of Extraction Thimble
11.1 Dry the clean thimble in an oven at 105 6 5°C for 45
min, cool in a desiccator, and weigh to the nearest 0.5 mg.
Record the mass.
11.1.1 After each use, ignite the thimble at 700 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
11.1.
11.1.2 After repeated use, boil the thimble in 1 + 1 hydro-
chloric acid. (Add equal volume of concentrated
...
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