ASTM D4072-98(2013)
(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 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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
Designation: D4072 − 98 (Reapproved 2013)
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 4. Significance and Use
1.1 This test method covers the determination of toluene- 4.1 This test method is useful for evaluating and character-
insoluble matter (TI) in tar and pitch. izing tars and pitches and as one element in establishing the
uniformity of shipments or sources of supply.
1.2 Since this test method is empirical, strict adherence to
all details of the procedure is necessary.
5. Apparatus
1.3 The values stated in SI units are to be regarded as
5.1 Extraction Apparatus, Flask with metal cap condenser
standard. No other units of measurement are included in this
as shown in Fig. 1.
standard.
5.2 Extraction Thimble, AlundumAN 485 coarse (formerly
1.4 This standard does not purport to address all of the
RA 98), 30 mm in diameter by 80 mm in height with flat
safety concerns, if any, associated with its use. It is the
bottom.
responsibility of the user of this standard to establish appro-
5.3 Thimble Cover, Paper cone, made by wetting with water
priate safety and health practices and determine the applica-
a 70-mm filter paper normally folded in a small glass funnel,
bility of regulatory limitations prior to use. For specific hazard
and drying the funnel in an oven with the paper cone in place.
information, see Section 7.
5.4 Sieves,U.S.Standard 600-µm(No.30)and250-µm(No.
2. Referenced Documents
60), conforming to Specification E11.
2.1 ASTM Standards:
5.5 Heater, having a minimum capacity of 300 W per unit.
D95 Test Method for Water in Petroleum Products and
Bituminous Materials by Distillation
6. Reagents
D362 SpecificationforIndustrialGradeToluene(Withdrawn
6.1 Toluene, Industrial Pure, meeting Specification D362.
1989)
(Warning—Flammable.)
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
3. Summary of Test Method
working areas should be efficiently hooded and kept free of
sparks and flames.
3.1 The sample is digested, then extracted with hot toluene
in an alundum thimble. The insoluble matter is dried and
7.2 Observe proper laboratory procedures for handling and
weighed.
diluting hydrochloric acid.
8. Bulk Sampling
This test method is under the jurisdiction of ASTM Committee D02 on
8.1 Samples from shipments shall be taken in accordance
Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of
with Practice D4296, and shall be free of foreign substances.
SubcommitteeD02.05onPropertiesofFuels,PetroleumCokeandCarbonMaterial.
Current edition approved May 1, 2013. Published August 2013. Originally
Thoroughly mix the sample immediately before removing a
approved in 1981. Last previous edition approved in 2008 as D4072 – 98 (2008).
representative portion for the determination or for dehydration.
DOI: 10.1520/D4072-98R13.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
9. Dehydration of Sample
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
9.1 Hard Pitch—If the solid bulk sample contains free
the ASTM website.
water, air-dry a representative portion in a forced draft oven at
The last approved version of this historical standard is referenced on
www.astm.org. 50°C.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D4072 − 98 (2013)
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 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
FIG. 1 Extraction Apparatus
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.
9.2 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 and 150°C in an
described in 11.1 and 11.1.1.
open container until the surface is free of foam. Take care not
to overheat, and remove heat source immediately when foam
12. Procedure
subsides.
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 sidearm distil-
unless this would require less than the minimum acceptable
lation apparatus similar to the one in Test Method D850 and
sample mass of 1 g, in which case 1 g shall be used.
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-
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