ASTM D2764-99(2009)
(Test Method)Standard Test Method for Dimethylformamide-Insoluble (DMF-I) Content of Tar and Pitch
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 D4072.
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 and health practices and determine the applicability of regulatory limitations prior to use. For specific hazard information, see Sections 6 and 7.
General Information
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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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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: D2764 − 99(Reapproved 2009)
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.
1. Scope uniformity of shipments or sources of supply. It is a rapid and
reasonably accurate measure of the toluene insoluble (TI)
1.1 This test method covers the determination of the
content of tar and pitch Test Method D4072.
dimethylformamide-insoluble matter (DMF-I) in tar and pitch.
1.2 Since this test method is empirical, strict adherence to
5. Apparatus
all details of the procedure is necessary.
5.1 Filtering Crucible, porcelain, with fine-porosity bottom,
1.3 The values stated in inch-pound units are to be regarded
30 to 40-mL capacity, high form, maximum pore diameter
as standard. The values given in parentheses are mathematical
7 µm.
conversions to SI units that are provided for information only
5.2 Filter Apparatus—Filter flask and tube with crucible
and are not considered standard.
adapter.
1.4 This standard does not purport to address all of the
5.3 Sieves,U.S.Standard 600-µm(No.30)and250-µm(No.
safety concerns, if any, associated with its use. It is the
60), conforming to Specification E11.
responsibility of the user of this standard to establish appro-
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 hazard
information, see Sections 6 and 7. 6. Reagents and Materials
6.1 Dimethylformamide, reagent grade, boiling range 4°F
2. Referenced Documents
(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
D4296 Practice for Sampling Pitch
6.3 Concentrated Hydrochloric Acid.
E11 Specification for Woven Wire Test Sieve Cloth and Test
6.4 Celite Analytical Filter Aid (CAFA)—Dry to constant
Sieves
weightat22°F(105°C)andstoreintightlystopperedcontainer.
3. Summary of Test Method
NOTE 1—Do not use any other grade of filtering medium because
porosities differ.
3.1 A sample is digested in hot DMF and filtered. Any
insoluble matter is washed, dried, and weighed.
7. Hazards
4. Significance and Use
7.1 Fumes of the solvents should be removed by means of
4.1 This test method is useful in evaluating and character-
proper hoods from all working areas. The working area should
izing tars and pitches and as one element in establishing the
be kept free of sparks and flames. DMF fumes should not be
inhaled,andprolongedcontactofDMFwiththeskinshouldbe
This test method is under the jurisdiction of ASTM Committee D02 on
avoided.
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee
D02.05 on Properties of Fuels, Petroleum Coke and Carbon Material.
7.2 Observe proper laboratory procedures for handling and
Current edition approved Oct. 1, 2009. Published November 2009. Originally
diluting hydrochloric acid.
´1
approved in 1968. Last previous edition approved in 2004 as D2764–99(2004) .
DOI: 10.1520/D2764-99R09.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or 8. Bulk Sampling
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
8.1 Samples from shipments shall be taken in accordance
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. with Practice D4296 and shall be free of foreign substances.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D2764 − 99 (2009)
The sample shall be thoroughly mixed immediately before 11.2 After the crucible has been used for six determinations,
removing a representative portion for the determination or for remove any residual ash from pores in the filtering area by
dehydration. boiling in 1 + 1 hydrochloric acid. Add equal volume of
concentrated hydrochloric acid to distilled water. Then boil the
9. Dehydration of Sample
crucible in distilled water, thoroughly back wash with distilled
9.1 Hard Pitch—If the solid bulk sample contains free water, dry, and ignite as in 11.1.
water, air-dry a representative portion in a forced draft oven at
12. Procedure
50°C.
12.1 Make and record all weighings to the nearest 0.5 mg.
9.2 Soft Pitch—If the presence of water is indicated by
12.2 Transfer 0.45 to 0.55 g of Celite to a clean, filtering
surface foam on heating, maintain a representative portion of
crucible. Distribute the Celite evenly over the bottom. Dry in
the bulk sample at a temperature between 257 and 302°F (125
an oven at 22 to 230°F (105 to 110°C) for 30 min. Cool in a
and 150°C) in an open container until the surface is free of
desiccator and weigh. Record the weight of crucible plus
foam. Take care not to overheat, and remove heat source
Celite.
immediately when foam subsides.
12.3 Transfer 0.45 to 0.55 g of previously dried Celite to a
9.3 Tar—Dehydrate a representative portion of the bulk
clean, dry, and tared 100-mL beaker and weigh. Record the
sample in accordance with Test Method D370, but stop the
weight of Celite. Place 0.5 g of working sample in the same
distillation when the temperature reaches 338°F (170°C).
beaker and reweigh. Calculate and record the weight of the
Separate any oil from the water that has distilled over (if
sample.
crystals are present, warm sufficiently to ensure their solution),
12.4 Add 25 mL of dry dimethylformamide (DMF) to the
and thoroughly mix the oil with the residual tar in the still after
the latter has cooled to a moderate temperature. beaker while stirring the mixture with a stirring rod or
thermometer to break up lumps, then cover the beaker with a
10. Preparation of Working Sample
small watch glass. Place the beaker and a wash bottle contain-
ing DMF in a water bath maintained at 203 to 212°F (95 to
10.1 Hard Pitch—If the pitch can be crushed at room
100°C).(Asuitableweightcanbeusedtokeepthebeakerfrom
temperature, prepare a 20-g working sample by suitable
being upset in the water bath.) Digest for at least 30 min.
crushing, mixing, and quartering of a representative portion of
Occasionally stir
...
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