ASTM D4312-95a(2000)e1

Standard Test Method for Toluene-Insoluble (TI) Content of Tar and Pitch (Short Method)

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. Specific hazard statements are given in Section 7.

General Information

• Status: Historical
• Publication Date: 31-Dec-1999
• ICS: 91.100.50 - Binders. Sealing materials
• Technical Committee: D02 - Petroleum Products, Liquid Fuels, and Lubricants
• Drafting Committee: D02.05 - Properties of Fuels, Petroleum Coke and Carbon Material

Relations

• Replaces: ASTM D4312-95a - Standard Test Method for Toluene-Insoluble (TI) Content of Tar and Pitch (Short Method)
• Effective Date: 01-Jan-2000
• Replaced By: ASTM D4312-95a(2005) - Standard Test Method for Toluene-Insoluble (TI) Content of Tar and Pitch (Short Method)
• Effective Date: 01-May-2005
• Referred By: ASTM D146/D146M-04(2020) - Standard Test Methods for Sampling and Testing Bitumen-Saturated Felts and Woven Fabrics for Roofing and Waterproofing
• Effective Date: 01-Jan-2000

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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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
An American National Standard
e1
Designation:D4312–95a (Reapproved 2000)
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.
e NOTE—Paragraph 1.3 was added editorially in November 2000.
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
1.2 Since this test method is empirical, strict adherence to weighed.
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
standard. izing tars and pitches and is one element in establishing the
uniformity of shipment 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 ExtractionApparatus, flask with metal cap condenser as
priate safety and health practices and determine the applica-
shown in Fig. 1.
bility of regulatory limitations prior to use. Specific hazard
5.2 ExtractionThimbles,AlundumAN485coarse(formerly
statements are given in Section 7.
RA 98), 30 mm in diameter by 80 mm in height with flat
2. Referenced Documents
bottom.
2.1 ASTM Standards: 5.3 Sieves,U.S.Standard 600-µm(No.30)and250-µm(No.
60), conforming to SpecificationE11.
D95 Test Method for Water in Petroleum Products and
5.4 Heater, having a minimum capacity of 300 W per unit.
Bituminous Materials by Distillation
D 329 Specification for Acetone Ahot plate or other heaters that maintain the proper reflux rate
are acceptable.
D 362 Specification for Industrial Grade Toluene
D 370 Test Method for Dehydration of Oil-Type Preserva-
5 6. Reagents
tives
6.1 Toluene, Industrial Pure, meeting Specification D 362.
D 850 Test Method for Distillation of Industrial Aromatic
6.2 Acetone, meeting the requirements of Specification
Hydrocarbons and Related Materials
D 329.
D 4072 Test Method for Toluene–Insoluble (TI) Content of
Tar and Pitch
7. Hazards
D 4296 Practice for Sampling Pitch
7.1 Since toluene is a toxic and flammable substance, all
E11 Specification for Wire–Cloth Sieves for Testing Pur-
working areas should be efficiently hooded and kept free of
poses
sparks and flames.
8. Bulk Sampling
This test method is under the jursidiction of ASTM Committee D02 on
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee
8.1 Samples from shipments shall be taken in accordance
D02.05.OF on Industrial Pitches.
with Practice D 4296, and shall be free of foreign substances.
Current edition approved Sept. 10, 1995. Published November 1995. Originally
published as D 4312 – 83. Last previous edition D 4312 – 95. Thoroughly mix the sample immediately before removing a
Annual Book of ASTM Standards, Vol 05.01.
representative portion for the determination or for dehydration.
Annual Book of ASTM Standards, Vol 06.04.
Annual Book of ASTM Standards, Vol 06.03.
Annual Book of ASTM Standards, Vol 04.10.
Annual Book of ASTM Standards, Vol 05.02.
Annual Book of ASTM Standards, Vol 14.02.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
e1
D4312–95a (2000)
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
600-µm (No. 30) sieve, taking care to avoid excessive loss of
volatile matter. 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 dry 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 sample 24 h after crushing and
sieving as changes in composition sometimes occur in pulver-
ized pitch.
11. Preparation of Alundum Thimble
FIG. 1 Extraction Apparatus
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.
9. Dehydration of Sample
Record the mass.
9.1 Hard Pitch—If the solid bulk sample contains free
11.1.1 After each use, ignite the thimble at 700 to 800°C for
water, air-dry a representative portion.
a few hours. Cool the thimble slowly by placing in a drying
9.2 Soft Pitch—If the presence of water is indicated by
oven for 1 h after removal from the furnace to prevent
surface foam on heating, maintain a representative portion of
cracking. Before reuse, condition the thimble as described in
the bulk sample of a temperature between 125 and 150°C in an
11.1.
open container until the surface is free of foam. Take care not
11.1.2 After repeated use, boil the thimble in hydrochloric
to overheat, and remove heat source immediately when foam
acid (1 + 1) to remove residual ash from the pores. Then boil
subsides.
thethimbleindistilledwaterandwashwithwater.Afterdrying
9.3 Tar—Dehydrate a representative portion of the bulk
at 105°C, ignite and condition the thimble as described in 11.1
sample in accordance with Test Method D 370, but stop the
and 11.1.1.
distillation when the temperature reaches 170°C. Separate any
12. Procedure
oil from the water that has distilled over. (If crystals are
present,warmsufficientlytoensuretheirsolution).Thoroughly 12.1 Weigh 0.50 g sam
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