ASTM D4072-98(2003)e1
(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
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 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.
General Information
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Standards Content (Sample)
NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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An American National Standard
e1
Designation:D4072–98 (Reapproved 2003)
Standard Test Method for
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.
e NOTE—Warning notes were editorially moved into the standard text in November 2003.
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)and250-µm(No.
bility of regulatory limitations prior to use. For specific hazard 60), conforming to SpecificationE11.
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.
D95 Test Method for Water in Petroleum Products and (Warning—Flammable.)
Bituminous Materials by Distillation 6.2 Concentrated Hydrochloric Acid. (Warning—
D 362 Specification for Industrial Grade Toluene Corrosive.)
D 850 Test Method for Distillation of Industrial Aromatic
7. Hazards
Hydrocarbons and Related Materials
7.1 Since toluene is a toxic and flammable substance, all
D 4296 Practice for Sampling Pitch
E11 Specification for Wire Cloth and Sieves for Testing working areas should be efficiently hooded and kept free of
sparks and flames.
Purposes
7.2 Observe proper laboratory procedures for handling and
3. Summary of Test Method
diluting hydrochloric acid.
3.1 The sample is digested, then extracted with hot toluene
8. Bulk Sampling
in an alundum thimble. The insoluble matter is dried and
8.1 Samples from shipments shall be taken in accordance
weighed.
with Practice D 4296, and shall be free of foreign substances.
4. Significance and Use
Thoroughly mix the sample immediately before removing a
4.1 This test method is useful for evaluating and character- representative portion for the determination or for dehydration.
izing tars and pitches and as one element in establishing the
9. Dehydration of Sample
uniformity of shipments or sources of supply.
9.1 Hard Pitch—If the solid bulk sample contains free
water, air-dry a representative portion in a forced draft oven at
This test method is under the jurisdiction of ASTM Committee D02 on
50°C.
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee
9.2 Soft Pitch—If the presence of water is indicated by
D02.05 on Properties of Fuels, Petroleum Coke and Carbon Material.
surface foam on heating, maintain a representative portion of
Current edition approved Nov. 18, 2003. Published November 2003. Originally
approved in 1981. Last previous edition approved in 1998 as D 4072–98.
the bulk sample of a temperature between 125 and 150°C in an
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
open container until the surface is free of foam. Take care not
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
to overheat, and remove heat source immediately when foam
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. subsides.
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D4072–98 (2003)
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 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 11.1 and 11.1.1.
FIG. 1 Extraction Apparatus
12. Procedure
12.1 The mass of sample taken for analysis shall yield
9.3 Tar—Dehydrate a representative portion of the bulk
between 150 and 250 mg of matter insoluble in toluene (TI),
sample at atmospheric pressure using a simple side-arm
unless this would require less than the minimum acceptable
distillation apparatus similar to the one in Test Method D 850
sample mass of 1 g, in which case 1 g shall be used.
and stop the distillation when the temperature reaches 170°C.
12.2 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 mLof 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 7.1). Place
9.3.1 As an alternative to dehydration, the water content of
the beaker on an electric hot plate or on a steam or water bath
the tar is determined by Test Method D95 and, if the water
and heat the contents to a temperature of 95 6 5°C. Maintain
content is less than 10 mass percent, theTI content is corrected
this temperature for 25 min. Stir occasionally with a stirring
to a dry-tar basis (see 13.2). This alternative method applies
rod during this period to ensure that the sample is completely
only to stable emulsions of water in tar, that is, no water
dispersed in the toluene. Check for completeness of dispersion
separates when the ta
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