ASTM D2764-99

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

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: 09-Apr-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

• Replaced By: ASTM D2764-99(2004)e1 - Standard Test Method for Dimethylformamide-Insoluble (DMF-I) Content of Tar and Pitch
• Effective Date: 01-Nov-2004
• Referred By: ASTM D2042-22 - Standard Test Method for Solubility of Asphalt Materials in Trichloroethylene or Toluene
• Effective Date: 10-Apr-1999
• Referred By: ASTM D7553-15(2021) - Standard Test Method for Solubility of Asphalt Materials in N-Propyl Bromide
• Effective Date: 10-Apr-1999

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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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
Designation: D 2764 – 99
Standard Test Method for
Dimethylformamide-Insoluble (DMF-I) Content of Tar and
Pitch
This standard is issued under the fixed designation D 2764; 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.
1. Scope 4. Significance and Use
1.1 This test method covers the determination of the 4.1 This test method is useful in evaluating and character-
dimethylformamide-insoluble matter (DMF-I) in tar and pitch. izing tars and pitches and as one element in establishing the
1.2 Since this test method is empirical, strict adherence to uniformity of shipments or sources of supply. It is a rapid and
all details of the procedure is necessary. reasonably accurate measure of the toluene insoluble (TI)
1.3 The values stated in inch-pound units are to be regarded content of tar and pitch Test Method D 4072.
as the standard.
5. Apparatus
1.4 This standard does not purport to address all of the
5.1 Filtering Crucible, porcelain, with fine-porosity bottom,
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro- 30 to 40-mL capacity, high form, maximum pore diameter 7µ
m.
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use. For specific 5.2 Filter Apparatus—Filter flask and tube with crucible
adapter.
precautionary information, see Section 7.
5.3 Sieves,U.S.Standard 600-µm(No.30)and250-µm(No.
2. Referenced Documents
60), conforming to Specification E 11.
2.1 ASTM Standards: 5.4 Water Bath, maintained at 203 to 212°F (95 to 100°C).
D 329 Specification for Acetone
6. Reagents and Materials
D 370 Test Method for Dehydration of Oil-Type Preserva-
tives 6.1 Dimethylformamide, reagent grade, boiling range 4°F
D 4072 Test Method for Toluene-Insoluble (TI) Content of (2°C)including307°F(153°C).Storeoverasuitabledesiccant.
Decant immediately before use. If necessary, filter through a
Tar and Pitch
D 4296 Practice for Sampling Pitch plug of glass wool or absorbent cotton until optically clear.
6.2 Acetone, meeting Specification D 329.
E 11 Specification for Wire-Cloth Sieves for Testing Pur-
poses
NOTE 1—Warning: Flammable. Health hazard.
3. Summary of Test Method 6.3 Concentrated Hydrochloric Acid.
6.4 Celite Analytical Filter Aid (CAFA)—Dry to constant
3.1 A sample is digested in hot DMF and filtered. Any
weightat22°F(105°C)andstoreintightlystopperedcontainer.
insoluble matter is washed, dried, and weighed.
NOTE 2—Do not use any other grade of filtering medium because
porosities differ.
This test method is under the jurisdiction of ASTM Committee D-2 on
Petroleum Products and Lubricantsand is the direct responsibility of Subcommittee
D02.05.OF on Industrial Pitches.
Current edition approved Apr. 10, 1999. Published June 1999. Originally
published as D 2764 – 68 T. Last previous edition D 2764 – 97.
Annual Book of ASTM Standards, Vol 06.04.
Annual Book of ASTM Standards, Vol 04.10.
4 6
Annual Book of ASTM Standards, Vol 05.02. Selas Grade 01, Size No. FC30 or FC40, or equivalent, has been found
Annual Book of ASTM Standards, Vol 14.02. satisfactory for this purpose.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D 2764
7. Safety Precautions working samples 24 h after crushing and sieving since changes
in composition sometimes occur in pulverized pitch.
7.1 Fumes of the solvents should be removed by means of
proper hoods from all working areas. The working area should
11. Crucible Preparation
be kept free of sparks and flames. DMF fumes should not be
inhaled,andprolongedcontactofDMFwiththeskinshouldbe
11.1 If the crucible, after thorough cleaning (11.2), has been
avoided. used for less than six determinations, clean it as follows.
7.2 Observe proper laboratory procedures for handling and
Remove the mat, wash the crucible with distilled water, dry,
diluting hydrochloric acid. and ignite in a muffle furnace for1hat about 1472°F (800°C).
Cool the crucible slowly by placing it in a drying oven for 1 h
8. Bulk Sampling
after removal from the furnace to prevent cracking and place it
in a desiccator while still warm.
8.1 Samples from shipments shall be taken in accordance
11.2 After the crucible has been used for six determinations,
with Practice D 4296 and shall be free of foreign substances.
remove any residual ash from pores in the filtering area by
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
9. Dehydration of Sample water, dry, and ignite as in 11.1.
9.1 Hard Pitch—If the solid bulk sample contains free
12. Procedure
water, air-dry a representative portion in a forced draft oven at
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 D 370, 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
...