ASTM D4312-95a(2005)

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

SIGNIFICANCE AND USE
This test method is useful for evaluating and characterizing tars and pitches and is one element in establishing the uniformity of shipment 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.
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: 30-Apr-2005
• 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(2000)e1 - Standard Test Method for Toluene-Insoluble (TI) Content of Tar and Pitch (Short Method)
• Effective Date: 01-May-2005
• Replaced By: ASTM D4312-95a(2010) - Standard Test Method for Toluene-Insoluble (TI) Content of Tar and Pitch (Short Method)
• Effective Date: 01-May-2010
• 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-May-2005

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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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:D4312–95a (Reapproved 2005)
Standard Test Method for
Toluene-Insoluble (TI) Content of Tar and Pitch (Short
Method)
This standard is issued under the fixed designation D4312; 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 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 The values stated in SI units are to be regarded as
standard. 5.1 ExtractionApparatus, flask with metal cap condenser as
shown in Fig. 1.
1.4 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the 5.2 ExtractionThimbles,AlundumAN485coarse(formerly
responsibility of the user of this standard to establish appro- RA 98), 30 mm in diameter by 80 mm in height with flat
bottom.
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use. Specific hazard 5.3 Sieves,U.S.Standard 600-µm(No.30)and250-µm(No.
60), conforming to Specification E11.
statements are given in Section 7.
5.4 Heater, having a minimum capacity of 300 W per unit.
2. Referenced Documents
Ahot plate or other heaters that maintain the proper reflux rate
2.1 ASTM Standards: are acceptable.
D95 Test Method for Water in Petroleum Products and
6. Reagents
Bituminous Materials by Distillation
D329 Specification for Acetone 6.1 Toluene, Industrial Pure, meeting Specification D362.
6.2 Acetone, meeting the requirements of Specification
D362 Specification for Industrial Grade Toluene
D370 Practice for Dehydration of Oil-Type Preservatives D329.
D850 Test Method for Distillation of Industrial Aromatic
7. Hazards
Hydrocarbons and Related Materials
7.1 Since toluene is a toxic and flammable substance, all
D4072 Test Method for Toluene-Insoluble (TI) Content of
working areas should be efficiently hooded and kept free of
Tar and Pitch
sparks and flames.
D4296 Practice for Sampling Pitch
E11 SpecificationforWovenWireTestSieveClothandTest
8. Bulk Sampling
Sieves
8.1 Samples from shipments shall be taken in accordance
3. Summary of Test Method
with Practice D4296, and shall be free of foreign substances.
Thoroughly mix the sample immediately before removing a
3.1 The sample is digested, then extracted with hot toluene
representative portion for the determination or for dehydration.
in an alundum thimble. The insoluble matter is dried and
weighed.
9. Dehydration of Sample
9.1 Hard Pitch—If the solid bulk sample contains free
This test method is under the jurisdiction of ASTM Committee D02 on
water, air-dry a representative portion.
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.
Current edition approved May 1, 2005. Published May 2005. Originally surface foam on heating, maintain a representative portion of
´1
approved in 1983. Last previous edition approved in 2000 as D4312–95a (2000) .
the bulk sample of a temperature between 125 and 150°C in an
DOI: 10.1520/D4312-95AR05.
open container until the surface is free of foam. Take care not
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
to overheat, and remove heat source immediately when foam
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
Standards volume information, refer to the standard’s Document Summary page on
subsides.
the ASTM website.
Withdrawn.
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D4312–95a (2005)
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
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
FIG. 1 Extraction Apparatus
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
9.3 Tar—Dehydrate a representative portion of the bulk
thethimbleindistilledwaterandwashwithwater.Afterdrying
sample in accordance with Test Method D370, but stop the
at 105°C, ignite and condition the thimble as described in 11.1
distillation when the temperature reaches 170°C. Separate any
and 11.1.1.
oil from the water that has distilled over. (If crystals are
present,warmsufficientlytoensuretheirsolution).Thoroughly
12. Procedure
mix the oil with the residual tar in the still after the latter has
12.1 Weigh 0.50 g sample to the nearest 0.5 mg in a 150 mL
cooled to a moderate temperature.
tared beaker.
9.3.1 Dehydrate a representative portion of the bulk sample
12.2 While stirring sample with a glass rod, add 75 mL of
at atmospheric pressure using a simple side-arm distillation
hot toluene (95 6 5°C) and continue stirring for a few minutes
apparatus similar to the one in Test M
...