ASTM D4312-95a

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Designation: D 4312 – 95a
Standard Test Method for
Toluene-Insoluble (TI) Content of Tar and Pitch (Short
Method)
This standard is issued under the fixed designation D 4312; 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 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 is one element in establishing the
1.2 Since this test method is empirical, strict adherence to uniformity of shipment or sources of supply.
all details of the procedure is necessary.
5. Apparatus
1.3 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the 5.1 Extraction Apparatus, flask with metal cap condenser as
shown in Fig. 1.
responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica- 5.2 Extraction Thimbles, Alundum AN 485 coarse (formerly
RA 98), 30 mm in diameter by 80 mm in height with flat
bility of regulatory limitations prior to use. Specific hazard
statements are given in Section 7. bottom.
5.3 Sieves, U.S. Standard 600-μm (No. 30) and 250-μm (No.
2. Referenced Documents
60), conforming to Specification E 11.
2.1 ASTM Standards: 5.4 Heater, having a minimum capacity of 300 W per unit.
D 95 Test Method for Water in Petroleum Products and A hot plate or other heaters that maintain the proper reflux rate
Bituminous Materials by Distillation are acceptable.
D 329 Specification for Acetone
6. Reagents
D 362 Specification for Industrial Grade Toluene
6.1 Toluene, Industrial Pure, meeting Specification D 362.
D 370 Test Method for Dehydration of Oil-Type Preserva-
tives 6.2 Acetone, meeting the requirements of Specification
D 329.
D 850 Test Method for Distillation of Industrial Aromatic
Hydrocarbons and Related Materials
7. Hazards
D 4072 Test Method for Toluene–Insoluble (TI) Content of
7.1 Since toluene is a toxic and flammable substance, all
Tar and Pitch
working areas should be efficiently hooded and kept free of
D 4296 Practice for Sampling Pitch
sparks and flames.
E 11 Specification for Wire–Cloth Sieves for Testing Pur-
poses
8. Bulk Sampling
3. Summary of Test Method
8.1 Samples from shipments shall be taken in accordance
with Practice D 4296, and shall be free of foreign substances.
3.1 The sample is digested, then extracted with hot toluene
Thoroughly mix the sample immediately before removing a
in an alundum thimble. The insoluble matter is dried and
representative portion for the determination or for dehydration.
weighed.
9. Dehydration of Sample
9.1 Hard Pitch—If the solid bulk sample contains free
This test method is under the jursidiction of ASTM Committee D-2 on
water, air-dry a representative portion.
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee
D02.05.OF on Industrial Pitches.
9.2 Soft Pitch—If the presence of water is indicated by
Current edition approved Sept. 10, 1995. Published November 1995. Originally
surface foam on heating, maintain a representative portion of
published as D 4312 – 83. Last previous edition D 4312 – 95.
2 the bulk sample of a temperature between 125 and 150°C in an
Annual Book of ASTM Standards, Vol 05.01.
Annual Book of ASTM Standards, Vol 06.04. open container until the surface is free of foam. Take care not
Annual Book of ASTM Standards, Vol 06.03.
to overheat, and remove heat source immediately when foam
Annual Book of ASTM Standards, Vol 04.10.
6 subsides.
Annual Book of ASTM Standards, Vol 04.04.
9.3 Tar—Dehydrate a representative portion of the bulk
Annual Book of ASTM Standards, Vol 14.02.
Copyright © ASTM, 100 Barr Harbor Drive, West Conshohocken, PA 19428-2959, United States.
D 4312
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 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 hydrochloric
acid (1 + 1) to remove residual ash from the pores. Then boil
the thimble in distilled water and wash with water. After drying
FIG. 1 Extraction Apparatus
at 105°C, ignite and condition the thimble as described in 11.1
and 11.1.1.
sample in accordance with Test Method D 370, but stop the
distillation when the temperature reaches 170°C. Separate any
12. Procedure
oil from the water that has distilled over. (If crystals are
12.1 Weigh 0.50 g sample to the nearest 0.5 mg in a 150 mL
present, warm sufficiently to ensure their solution). Thoroughly
tared beaker.
mix the oil with the residual tar in the still after the latter has
12.2 While stirring sample with a glass rod, add 75 mL of
cooled to a moderate temperature.
hot toluene (95 6 5°C) and continue stirring for a few minutes
9.3.1 Dehydrate a representative portion of the bulk sample
until the sample is dispersed. Digest sample containing toluene
at atmospheric pressure using a simple side-arm distillation
on an appropriate heat source (preferably a hot water or steam
apparatus similar to the one in Test Method D 850 and stop the
bath) at 95 6 5°C for 25 min with occasional stirring.
distillation when the temperature reaches 170°C. Separate any
12.3 While sample is digesting, weig
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