ASTM D2764-99(2015)e1
(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
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.
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.
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´1
Designation: D2764 − 99 (Reapproved 2015)
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 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
uniformity of shipments or sources of supply. It is a rapid and
1.2 Since this test method is empirical, strict adherence to
reasonably accurate measure of the toluene insoluble (TI)
all details of the procedure is necessary.
content of tar and pitch Test Method D4072.
1.3 The values stated in inch-pound units are to be regarded
as standard. The values given in parentheses are mathematical
5. Apparatus
conversions to SI units that are provided for information only
5.1 Filtering Crucible, porcelain, with fine-porosity bottom,
and are not considered standard.
30 mL to 40 mL capacity, high form, maximum pore diameter
1.4 This standard does not purport to address all of the
7 µm.
safety concerns, if any, associated with its use. It is the
5.2 Filter Apparatus—Filter flask and tube with crucible
responsibility of the user of this standard to establish appro-
adapter.
priate safety and health practices and determine the applica-
5.3 Sieves, U.S. Standard 600 µm (No. 30) and 250 µm (No.
bility of regulatory limitations prior to use. For specific hazard
60), conforming to Specification E11.
information, see Sections 6 and 7.
5.4 Water Bath, maintained at 203 °F to 212 °F (95 °C to
2. Referenced Documents
100 °C).
2.1 ASTM Standards:
6. Reagents and Materials
D329 Specification for Acetone
D370 Practice for Dehydration of Oil-Type Preservatives
6.1 Dimethylformamide, reagent grade, boiling range 4 °F
D4072 Test Method for Toluene-Insoluble (TI) Content of
(2 °C) including 307 °F (153 °C). Store over a suitable desic-
Tar and Pitch
cant. Decant immediately before use. If necessary, filter
D4296 Practice for Sampling Pitch
through a plug of glass wool or absorbent cotton until optically
E11 Specification for Woven Wire Test Sieve Cloth and Test
clear.
Sieves
6.2 Acetone, meeting Specification D329.(Warning—
Flammable. Health hazard.)
3. Summary of Test Method
6.3 Concentrated Hydrochloric Acid.
3.1 A sample is digested in hot DMF and filtered. Any
6.4 Celite Analytical Filter Aid (CAFA)—Dry to constant
insoluble matter is washed, dried, and weighed.
mass at 22 °F (105 °C) and store in tightly stoppered container.
NOTE 1—Do not use any other grade of filtering medium because
This test method is under the jurisdiction of ASTM Committee D02 on porosities differ.
Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of
SubcommitteeD02.05onPropertiesofFuels,PetroleumCokeandCarbonMaterial.
7. Hazards
Current edition approved April 1, 2015. Published May 2015. Originally
7.1 Fumes of the solvents should be removed by means of
approved in 1968. Last previous edition approved in 2009 as D2764 – 99 (2009).
DOI: 10.1520/D2764-99R15E01.
proper hoods from all working areas. The working area should
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
be kept free of sparks and flames. DMF fumes should not be
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
inhaled,andprolongedcontactofDMFwiththeskinshouldbe
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. avoided.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
´1
D2764 − 99 (2015)
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 for 1 h at about 1472 °F
(800 °C). Cool the crucible slowly by placing it in a drying
8. Bulk Sampling
oven for 1 h after removal from the furnace to prevent cracking
8.1 Samples from shipments shall be taken in accordance
and place it in a desiccator while still warm.
with Practice D4296 and shall be free of foreign substances.
11.2 After the crucible has been used for six determinations,
The sample shall be thoroughly mixed immediately before
remove any residual ash from pores in the filtering area by
removing a representative portion for the determination or for
boiling in 1 + 1 hydrochloric acid. Add equal volume of
dehydration.
concentrated hydrochloric acid to distilled water. Then boil the
9. Dehydration of Sample
crucible in distilled water, thoroughly back wash with distilled
water, dry, and ignite as in 11.1.
9.1 Hard Pitch—If the solid bulk sample contains free
water, air-dry a representative portion in a forced draft oven at
12. Procedure
50 °C.
9.2 Soft Pitch—If the presence of water is indicated by 12.1 Make and record all weighings to the nearest 0.5 mg.
surface foam on heating, maintain a representative portion of
12.2 Transfer 0.45 g to 0.55 g of Celite to a clean, filtering
the bulk sample at a temperature between 257 °F and 302 °F
crucible. Distribute the Celite evenly over the bottom. Dry in
(125 °C and 150 °C) in an open container until the surface is
an oven at 221 °F to 230 °F (105 °C to 110 °C) for 30 min.
freeoffoam.Takecarenottooverheat,andremoveheatsource
Cool in a desiccator and weigh. Record the mass of crucible
immediately when foam subsides.
plus Celite.
9.3 Tar—Dehydrate a representative portion of the bulk
12.3 Transfer 0.45 g to 0.55 g of previously dried Celite to
sample in accordance with Test Method D370, but stop the
a clean, dry, and tared 100 mL beaker and weigh. Record the
distillation when the temperature reaches 338 °F (170 °C).
mass of Celite. Place 0.5 g of working sample in the same
Separate any oil from the water that has distilled over (if
beaker and reweigh. Calculate and record the mass of the
crystals are present, warm sufficiently to ensure their solution),
sample.
and thoroughly mix the oil with the residual tar in the still after
the latter has cooled to a moderate temperature.
12.4 Add 25 mL of dry dimethylformamide (DMF) to the
beaker while stirring the mixture with a stirring rod or
10. Preparation of Working Sample
thermometer to break up lumps, then cover the beaker with a
10.1 Hard Pitch—If the pitch can be crushed at room
small watch glass. Place the beaker and a wash bottle contain-
temp
...
This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
´1
Designation: D2764 − 99 (Reapproved 2009) D2764 − 99 (Reapproved 2015)
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
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.
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, 3030 mL to 40-mL40 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-μmStandard 600 μm (No. 30) and 250-μm250 μm (No. 60), conforming to Specification E11.
5.4 Water Bath, maintained at 203203 °F to 212°F (95212 °F (95 °C to 100°C).100 °C).
This test method is under the jurisdiction of ASTM Committee D02 on Petroleum Products 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 Oct. 1, 2009April 1, 2015. Published November 2009 May 2015. Originally approved in 1968. Last previous edition approved in 20042009 as
ε1
D2764–99(2004)D2764 – 99 (2009). . DOI: 10.1520/D2764-99R09.10.1520/D2764-99R15E01.
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.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
´1
D2764 − 99 (2015)
6. Reagents and Materials
6.1 Dimethylformamide, reagent grade, boiling range 4°F (2°C) including 307°F (153°C).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 weightmass at 22°F (105°C)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.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 257257 °F and 302°F (125302 °F (125 °C and 150°C)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).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-g20 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 5 mm in any dimension. Crush this
sample so that all of it will pass the 250-μm250 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 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-μm600 μm (No. 30) sieve, taking care to avoid excessive loss of
volatile matter. Do not exceed 10 min 10 min for this melting period. Pass the heated sample through the 600-μm600 μm 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-μm600 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
...
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