ASTM D2764-20

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Designation: D2764 − 99 (Reapproved 2015) D2764 − 20
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.
ε NOTE—SI units formatting was corrected editorially in May 2015.
1. Scope 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 standard. The values given in parentheses are mathematical
conversions to SI units that are provided for information only and are not considered 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 safety, health, and healthenvironmental practices and determine the
applicability of regulatory limitations prior to use. For specific hazard information, see Sections 6 and 7.
1.5 This international standard was developed in accordance with internationally recognized principles on standardization
established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued
by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
2. Referenced Documents
2.1 ASTM Standards:
D329 Specification for Acetone
D370 Practice for Dehydration of Oil-Type Preservatives
D4072 Test Method for Toluene-Insoluble (TI) Content of Tar and Pitch
D4296 Practice for Sampling Pitch
E11 Specification for Woven Wire Test Sieve Cloth and Test Sieves
3. Summary of Test Method
3.1 A sample is digested in hot DMF and filtered. Any insoluble matter is washed, dried, and weighed.
4. Significance and Use
4.1 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 D4072.
5. Apparatus
5.1 Filtering Crucible, porcelain, with fine-porosity bottom, 30 mL to 40 mL capacity, high form, maximum pore diameter
7 μm.
5.2 Filter Apparatus—Filter flask and tube with crucible adapter.
5.3 Sieves, U.S. Standard 600 μm (No. 30) and 250 μm (No. 60), conforming to Specification E11.
This test method is under the jurisdiction of ASTM Committee D02 on Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of Subcommittee
D02.05 on Properties of Fuels, Petroleum Coke and Carbon Material.
Current edition approved April 1, 2015June 1, 2020. Published May 2015June 2020. Originally approved in 1968. Last previous edition approved in 20092015 as
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D2764 – 99 (2009).(2015) . DOI: 10.1520/D2764-99R15E01. 10.1520/D2764-20.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or 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 the ASTM website.
*A Summary of Changes section appears at the end of this standard
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D2764 − 20
5.4 Water Bath, maintained at 203 °F to 212 °F (95 °C to 100 °C).
6. Reagents and Materials
6.1 Dimethylformamide, reagent grade, boiling range 4 °F (2 °C) including 307 °F (153 °C). Store over a suitable desiccant.
Decant immediately before use. If necessary, filter through a plug of glass wool or absorbent cotton until optically clear.
6.2 Acetone, meeting Specification D329. (Warning—Flammable. Health hazard.)
6.3 Concentrated Hydrochloric Acid.
6.4 Celite Analytical Filter Aid (CAFA)—Dry to constant mass at 22 °F (105 °C) and store in tightly stoppered container.
NOTE 1—Do not use any other grade of filtering medium because porosities differ.
7. Hazards
7.1 Fumes of the solvents should be removed by means of proper hoods from all working areas. The working area should be
kept free of sparks and flames. DMF fumes should not be inhaled, and prolonged contact of DMF with the skin should be avoided.
7.2 Observe proper laboratory procedures for handling and diluting hydrochloric acid.
8. Bulk Sampling
8.1 Samples from shipments shall be taken in accordance with Practice D4296 and shall be free of foreign substances. The
sample shall be thoroughly mixed immediately before removing a representative portion for the determination or for dehydration.
9. Dehydration of Sample
9.1 Hard Pitch—If the solid bulk sample contains free water, air-dry a representative portion in a forced draft oven at 50 °C.
9.2 Soft Pitch—If the presence of water is indicated by surface foam on heating, maintain a representative portion of the bulk
sample at a temperature between 257 °F and 302 °F (125 °C and 150 °C) in an open container until the surface is free of foam.
Take care not to overheat, and remove heat source immediately when foam subsides.
9.3 Tar—Dehydrate a representative portion of the bulk sample in accordance with Test Method D370, but stop the distillation
when the temperature reaches 338 °F (170 °C). Separate any oil from the water that has distilled over (if crystals are present, warm
sufficiently to ensure their solution), and thoroughly mix the oil with the residual tar in the still after the latter has cooled to a
moderate temperature.
10. Preparation of Working Sample
10.1 Hard Pitch—If the pitch can be crushed at room temperature, prepare a 20 g working sample by suitable crushing, mixing,
and quartering of a representative portion of the dry sample. The crushing can be done with a small jaw crusher and a mullite
mortar and pestle. No particle in the representative sample shall be larger than 5 mm in any dimension. Crush this sample so that
all of it will pass the 250 μm (No. 60) sieve but have a minimum of fine particles. Store the sieved working sample in a tightly
closed container and use within 24 h (see 10.4).
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 the 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 (No. 30) 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 Preservation of Working Samples—Store samples as large lumps or as solidified melts in closed containers. Discard
working samples 24 h after crushing and sieving since changes in composition sometimes occur in pulverized pitch.
11. Crucible Preparation
11.1 If the crucible, after thorough cleaning (11.2), has been used for less than six determinations, clean it as follows. Remove
the mat, wash the crucible with distilled water, dry, and ignite in a muffle furnace for 1 h at about 1472 °F (800 °C
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