ASTM D4746-98(2003)e1
(Test Method)Standard Test Method for Determination of Quinoline Insolubles (QI) in Tar and Pitch by Pressure Filtration
Standard Test Method for Determination of Quinoline Insolubles (QI) in Tar and Pitch by Pressure Filtration
SIGNIFICANCE AND USE
This test method is useful in evaluating and characterizing tar and pitch and as one element in establishing the uniformity of shipments and sources of supply.
SCOPE
1.1 This test method covers the determination of the quinoline-insoluble matter (QI) in tar and pitch by pressure filtration and gives results comparable to those obtained by Method D 2318.
1.2 Since this test method is empirical, strict adherence to all details of the procedure is necessary.
1.3 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. Specific precautionary statements are given in Section 7.
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An American National Standard
e1
Designation:D4746–98 (Reapproved 2003)
Standard Test Method for
Determination of Quinoline Insolubles (QI) in Tar and Pitch
by Pressure Filtration
This standard is issued under the fixed designation D 4746; 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.
e NOTE—Warning notes were editorially moved into the standard text in November 2003.
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-
quinoline-insoluble matter (QI) in tar and pitch by pressure izing tar and pitch and as one element in establishing the
filtration and gives results comparable to those obtained by uniformity of shipments and sources of supply.
Test Method D 2318.
5. Apparatus
1.2 Since this test method is empirical, strict adherence to
5.1 Pressure Filtration Vessel—The pressure filtration ves-
all details of the procedure is necessary.
1.3 This standard does not purport to address all of the sel (see Fig. 1) is a stainless steel (304) jacketed block heated
by steam or cooled with water, sealed by a lid, flat gasket, and
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro- clamp. The interior of the block is designed to accept a 3A2
Berlin porcelain filtration crucible (see 5.4). The crucible is
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use. Specific precau- sealed within the block by the use of three O-rings, a crucible
sealing collar, and an adjustable plunger.
tionary statements are given in Section 7.
5.1.1 The seal is accomplished when the sealing lid is
2. Referenced Documents
placedontopoftheblockandclamped.Theadjustableplunger
2.1 ASTM Standards: applies a force to the crucible sealing collar, which in turn
D70 Test Method for Density of Semi-Solid Bituminous pushes downward on the crucible and simultaneously com-
Materials (Pycnometer Method) presses O-ring gaskets, forming a seal between surfaces of the
D95 Test Method for Water in Petroleum Products and crucible and the wall of the block. The filtration of material is
Bituminous Materials by Distillation accomplished by nitrogen (10 to 30 psig) introduced through
D 329 Specification for Acetone the lid of the pressure filter. The filtrate exits from the drain
D 850 Test Method for Distillation of Industrial Aromatic tube at the bottom of the block. The filtrate is disposed into a
Hydrocarbons and Related Materials Buchner flask, attached to drain tube by a No. 7 rubber stopper.
D 2318 Test Method for Quinoline-Insoluble (QI) Content A vacuum hose is attached to the Buchner flask and placed in
of Tar and Pitch a 100-mL beaker containing water to indicate the exit of
D 4296 Practice for Sampling Pitch nitrogen when the filtration is completed.
E1 Specification for ASTM Thermometers 5.2 Beaker,50mL.
5.3 Buchner Flask, 500.
3. Summary of Test Method
5.4 Filtering Crucible, porcelain, with a medium-porosity
3.1 The sample is digested in hot quinoline and filtered bottom, top outer diameter 1 ⁄4 in. (45 mm), bottom outer
through a heated pressure filter. The insoluble material is
diameter 1.2 in. (30 mm), height 2 in. (50 mm).
washed with hot, fresh quinoline and with cold acetone, dried, 5.5 Analytical Balance.
and weighed.
5.6 Desiccator.
5.7 Thermometer, 0 to 300°F (150°C).
1 5.8 Drying Oven, maintained at 221°F (105°C).
This test method is under the jurisdiction of ASTM Committee D02 on
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee
D02.05 on Properties of Fuels, Petroleum Coke and Carbon Material.
Current edition approved Nov. 18, 2003. Published November 2003. Originally
approved in 1987. Last previous edition approved in 1998 as D 4746–98. The sole source of supply of the pressure filtration vessel known to the
For referenced ASTM standards, visit the ASTM website, www.astm.org, or committee at this time is Koppers Co., Inc., 1005 Wm. Pitt Way, Pittsburgh, PA
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM 15238. If you are aware of alternative suppliers, please provide this information to
Standards volume information, refer to the standard’s Document Summary page on ASTMHeadquarters.Yourcommentswillreceivecarefulconsiderationatameeting
the ASTM website. of the responsible technical committee, which you may attend.
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D4746–98 (2003)
6.3 Acetone, meeting Specification D 329.(Warning—
Flammable (Health Hazard).)
7. Safety Precautions
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. Quinoline fumes should not
be inhaled, and prolonged contact with 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 D 4296 and shall be free of foreign substances.
Thoroughly mix the sample 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
122°F (50°C).
9.2 Soft Pitch (Softening Point <140°F (60°C))—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 and 302°F (125 and 150°C) in an
open container until the surface is free of foam. Take care not
to overheat, and remove the heat source immediately when the
FIG. 1 Pressure Filter
foam subsides.
9.3 Tar—Awet tar sample can either be dehydrated or used
5.9 Mortar and Pestle.
as received as long as conditions stated in 9.3.1 and 9.3.2 are
5.10 Two Wash Bottles, 500 mL.
met.
5.11 Steam Bath.
9.3.1 Dehydrate a representative portion of the bulk sample.
9.3.2 As an alternative to dehydration, the water content of
6. Reagents
the tar is determined by Test Method D95 and, if the water
6.1 Quinoline—Refined, meeting the following require-
content is less than 10 weight %, the QI content is corrected to
ments:
a dry-tar basis (see 13.2). This alternative method applies only
6.1.1 The quinoline shall be distilled from 5 to 95 % within
to stable emulsions of water in tar, that is, no water separates
a range of 2°F (1°C) that shall include the temperature of
when the tar sample is left undisturbed for 24 h at room
459.3°F (237.4°C) after corrections for barometric pressure
temperature.
andemergentsteamhavebeenapplied.Thedistillationshallbe
carried out in accordance with Method D 850 using a total- 10. Preparation of Working Sample
immersion thermometer with a range from 383 to 581°F (195
10.1 Pitch that is sufficiently hard at room temperature shall
to 305°C), graduated in 1°F (0.5°C) and conforming to the
be finely pulverized in a mortar. Crush this sample so that all
requirements for thermometer 69C as described in Specifica-
of it will pass the 250-µm (No. 60) sieve. Soft pitches and tars
tionE1.
shall be warmed and well agitated before sampling.
6.1.2 The quinoline shall have a specific gravity at 15.5/
10.2 The amount of sample to be taken for the test shall be
15.5°C of 1.092 to 1.098, as determined by Test MethodD70,
such that the final quantity of quinoline insoluble (QI) shall be
or other method of equivalent accuracy.
not less than 0.1 g. As a guide, the following sample sizes are
6.1.3 Thequinolineshallbeclearandlightincolorandshall
recommended:
contain less than 0.5 volume % of water as determined by Test
Sample Size, g
Method D95. If not, redistill the quinoline
...
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