ASTM D2764-99(2004)e1

Standard Test Method for Dimethylformamide-Insoluble (DMF-I) Content of Tar and Pitch

SIGNIFICANCE AND USE
This test method is useful in evaluating and characterizing tars and pitches and as one element in establishing the uniformity of shipments or sources of supply. It is a rapid and reasonably accurate measure of the toluene insoluble (TI) content of tar and pitch Test Method D 4072.
SCOPE
1.1 This test method covers the determination of the dimethylformamide-insoluble matter (DMF-I) 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 inch-pound units are to be regarded as the 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 precautionary information, see Section 7.

General Information

• Status: Historical
• Publication Date: 31-Oct-2004
• 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 D2764-99 - Standard Test Method for Dimethylformamide-Insoluble (DMF-I) Content of Tar and Pitch
• Effective Date: 01-Nov-2004
• Replaced By: ASTM D2764-99(2009) - Standard Test Method for Dimethylformamide-Insoluble (DMF-I) Content of Tar and Pitch
• Effective Date: 01-Oct-2009
• Referred By: ASTM D2042-22 - Standard Test Method for Solubility of Asphalt Materials in Trichloroethylene or Toluene
• Effective Date: 01-Nov-2004
• Referred By: ASTM D7553-15(2021) - Standard Test Method for Solubility of Asphalt Materials in N-Propyl Bromide
• Effective Date: 01-Nov-2004

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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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
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Designation:D2764–99 (Reapproved 2004)
Standard Test Method for
Dimethylformamide-Insoluble (DMF-I) Content of Tar and
Pitch
This standard is issued under the fixed designation D2764; 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.
´ NOTE—Warning notes moved into the text editorially in November 2004.
1. Scope reasonably accurate measure of the toluene insoluble (TI)
content of tar and pitch Test Method D4072.
1.1 This test method covers the determination of the
dimethylformamide-insoluble matter (DMF-I) in tar and pitch.
5. Apparatus
1.2 Since this test method is empirical, strict adherence to
5.1 Filtering Crucible, porcelain, with fine-porosity bottom,
all details of the procedure is necessary.
30 to 40-mL capacity, high form, maximum pore diameter
1.3 The values stated in inch-pound units are to be regarded
7µm.
as the standard.
5.2 Filter Apparatus—Filter flask and tube with crucible
1.4 This standard does not purport to address all of the
adapter.
safety concerns, if any, associated with its use. It is the
5.3 Sieves,U.S.Standard 600-µm(No.30)and250-µm(No.
responsibility of the user of this standard to establish appro-
60), conforming to Specification E11.
priate safety and health practices and determine the applica-
5.4 Water Bath, maintained at 203 to 212°F (95 to 100°C).
bility of regulatory limitations prior to use. For specific
precautionary information, see Section 7.
6. Reagents and Materials
2. Referenced Documents 6.1 Dimethylformamide, reagent grade, boiling range 4°F
2 (2°C)including307°F(153°C).Storeoverasuitabledesiccant.
2.1 ASTM Standards:
Decant immediately before use. If necessary, filter through a
D329 Specification for Acetone
plug of glass wool or absorbent cotton until optically clear.
D370 Practice for Dehydration of Oil-Type Preservatives
6.2 Acetone, meeting Specification D329.(Warning—
D4072 Test Method for Toluene-Insoluble (TI) Content of
Flammable. Health hazard.)
Tar and Pitch
6.3 Concentrated Hydrochloric Acid.
D4296 Practice for Sampling Pitch
6.4 Celite Analytical Filter Aid (CAFA)—Dry to constant
E11 SpecificationforWovenWireTestSieveClothandTest
weightat22°F(105°C)andstoreintightlystopperedcontainer.
Sieves
NOTE 1—Do not use any other grade of filtering medium because
3. Summary of Test Method
porosities differ.
3.1 A sample is digested in hot DMF and filtered. Any
7. Hazards
insoluble matter is washed, dried, and weighed.
7.1 Fumes of the solvents should be removed by means of
4. Significance and Use
proper hoods from all working areas. The working area should
4.1 This test method is useful in evaluating and character- be kept free of sparks and flames. DMF fumes should not be
izing tars and pitches and as one element in establishing the inhaled,andprolongedcontactofDMFwiththeskinshouldbe
uniformity of shipments or sources of supply. It is a rapid and avoided.
7.2 Observe proper laboratory procedures for handling and
diluting hydrochloric acid.
This test method is under the jurisdiction of ASTM Committee D02 on
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee
8. Bulk Sampling
D02.05 on Properties of Fuels, Petroleum Coke and Carbon Material.
Current edition approved Nov. 16, 2004. Published November 2004. Originally 8.1 Samples from shipments shall be taken in accordance
approved in 1968. Last previous edition approved in 1999 as D2764 – 99. DOI:
with Practice D4296 and shall be free of foreign substances.
10.1520/D2764-99R04E01.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
Standards volume information, refer to the standard’s Document Summary page on Selas Grade 01, Size No. FC30 or FC40, or equivalent, has been found
the ASTM website. satisfactory for this purpose.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
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D2764–99 (2004)
The sample shall be thoroughly mixed immediately before boiling in 1 + 1 hydrochloric acid. Add equal volume of
removing a representative portion for the determination or for concentrated hydrochloric acid to distilled water. Then boil the
dehydration. crucible in distilled water, thoroughly back wash with distilled
water, dry, and ignite as in 11.1.
9. Dehydration of Sample
12. Procedure
9.1 Hard Pitch—If the solid bulk sample contains free
12.1 Make and record all weighings to the nearest 0.5 mg.
water, air-dry a representative portion in a forced draft oven at
12.2 Transfer 0.45 to 0.55 g of Celite to a clean, filtering
50°C.
crucible. Distribute the Celite evenly over the bottom. Dry in
9.2 Soft Pitch—If the presence of water is indicated by
an oven at 22 to 230°F (105 to 110°C) for 30 min. Cool in a
surface foam on heating, maintain a representative portion of
desiccator and weigh. Record the weight of crucible plus
the bulk sample at a temperature between 257 and 302°F (125
Celite.
and 150°C) in an open container until the surface is free of
12.3 Transfer 0.45 to 0.55 g of previously dried Celite to a
foam. Take care not to overheat, and remove heat source
clean, dry, and tared 100-mL beaker and weigh. Record the
immediately when foam subsides.
weight of Celite. Place 0.5 g of working sample in the same
9.3 Tar—Dehydrate a representative portion of the bulk
beaker and reweigh. Calculate and record the weight of the
sample in accordance with Test Method D370, but stop the
sample.
distillation when the temperature reaches 338°F (170°C).
12.4 Add 25 mL of dry dimethylformamide (DMF) to the
Separate any oil from the water that has distilled over (if
beaker while stirring the mixture with a stirring rod or
crystals are present, warm sufficiently to ensure their solution),
thermometer to break up lumps, then cover the beaker with a
and thoroughly mix the oil with the residual tar in the still after
small watch glass. Place the beaker and a wash bottle contain-
the latter has cooled to a moderate temperature.
ing DMF in a water bath maintained at 203 to 212°F (95 to
10. Preparation of Working Sample
100°C).(Asuitableweightcanbeusedtokeepthebeakerfrom
10.1 Hard Pitch—If the pitch can be crushed at room being upset in the water bath.) Digest for at least 30 min.
Occasionally stir the contents of the beaker to promote
temperature, prepare a 20-g working sample by suitable
crushing, mixing, and quartering of a representative portion of digestion. Che
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