ASTM D4746-98(2008)
(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 Test Method D 2318.
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. Specific hazards are given in Section 7, 6.2, and 6.3.
General Information
Relations
Standards Content (Sample)
NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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Designation: D4746 − 98(Reapproved 2008)
Standard Test Method for
Determination of Quinoline Insolubles (QI) in Tar and Pitch
by Pressure Filtration
This standard is issued under the fixed designation D4746; 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 3. Summary of Test Method
1.1 This test method covers the determination of the
3.1 The sample is digested in hot quinoline and filtered
quinoline-insoluble matter (QI) in tar and pitch by pressure
through a heated pressure filter. The insoluble material is
filtration and gives results comparable to those obtained by
washed with hot, fresh quinoline and with cold acetone, dried,
Test Method D2318.
and weighed.
1.2 Since this test method is empirical, strict adherence to
4. Significance and Use
all details of the procedure is necessary.
4.1 This test method is useful in evaluating and character-
1.3 The values stated in inch-pound units are to be regarded
izing tar and pitch and as one element in establishing the
as standard. The values given in parentheses are mathematical
uniformity of shipments and sources of supply.
conversions to SI units that are provided for information only
and are not considered standard.
5. Apparatus
1.4 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the
5.1 Pressure Filtration Vessel—The pressure filtration ves-
responsibility of the user of this standard to establish appro-
sel (see Fig. 1) is a stainless steel (304) jacketed block heated
priate safety and health practices and determine the applica-
by steam or cooled with water, sealed by a lid, flat gasket, and
bilityofregulatorylimitationspriortouse.Specifichazardsare
clamp. The interior of the block is designed to accept a 3A2
given in Section 7, 6.2, and 6.3.
Berlin porcelain filtration crucible (see 5.4). The crucible is
sealed within the block by the use of three O-rings, a crucible
2. Referenced Documents
sealing collar, and an adjustable plunger.
5.1.1 The seal is accomplished when the sealing lid is
2.1 ASTM Standards:
placedontopoftheblockandclamped.Theadjustableplunger
D70 Test Method for Density of Semi-Solid Bituminous
applies a force to the crucible sealing collar, which in turn
Materials (Pycnometer Method)
pushes downward on the crucible and simultaneously com-
D95 Test Method for Water in Petroleum Products and
presses O-ring gaskets, forming a seal between surfaces of the
Bituminous Materials by Distillation
crucible and the wall of the block. The filtration of material is
D329 Specification for Acetone
accomplished by nitrogen (10 to 30 psig) introduced through
D850 Test Method for Distillation of Industrial Aromatic
the lid of the pressure filter. The filtrate exits from the drain
Hydrocarbons and Related Materials
tube at the bottom of the block. The filtrate is disposed into a
D2318 Test Method for Quinoline-Insoluble (QI) Content of
Buchnerflask,attachedtodraintubebyaNo.7rubberstopper.
Tar and Pitch
A vacuum hose is attached to the Buchner flask and placed in
D4296 Practice for Sampling Pitch
a 100-mL beaker containing water to indicate the exit of
E1 Specification for ASTM Liquid-in-Glass Thermometers
nitrogen when the filtration is completed.
5.2 Beaker, 50 mL.
This test method is under the jurisdiction of ASTM Committee D02 on
5.3 Buchner Flask, 500.
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 Oct. 15, 2008. Published December 2008. Originally
´1
approved in 1987. Last previous edition approved in 2003 as D4746–98(2003) .
DOI: 10.1520/D4746-98R08. 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 Inc., 436 Seventh Ave., Pittsburgh, PA
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM 15219-1800. If you are aware of alternative suppliers, please provide this informa-
Standards volume information, refer to the standard’s Document Summary page on tion toASTM Headquarters. Your comments will receive careful consideration at a
the ASTM website. meeting of the responsible technical committee, which you may attend.
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D4746 − 98 (2008)
6.1.3 Thequinolineshallbeclearandlightincolorandshall
contain less than 0.5 volume % of water as determined by Test
Method D95. If not, redistill the quinoline in an all-glass
apparatus,discardingthefirst5%andcollectingthenext90%.
If the quinoline contains suspended matter but is clear, light in
color, and contains less than 0.5 % water, filter the quinoline
through a crucible containing5gof celite filter aid.
6.1.4 Store the quinoline in a tightly closed, dark bottle.
6.2 1+1 Hydrochloric Acid Solution—Add equal volume
concentrated hydrochloric acid to distilled water. (Warning—
Corrosive.)
6.3 Acetone, meeting Specification D329.(Warning—
Flammable (Health Hazard).)
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. 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 D4296 and shall be free of foreign substances.
FIG. 1 Pressure Filter
Thoroughly mix the sample immediately before removing a
representative portion for the determination or for dehydration.
9. Dehydration of Sample
5.4 Filtering Crucible, porcelain, with a medium-porosity
3 9.1 Hard Pitch—If the solid bulk sample contains free
bottom, top outer diameter 1 ⁄4 in. (45 mm), bottom outer
water, air dry a representative portion in a forced draft oven at
diameter 1.2 in. (30 mm), height 2 in. (50 mm).
122°F (50°C).
5.5 Analytical Balance.
9.2 Soft Pitch (Softening Point <140°F (60°C))—If the
5.6 Desiccator.
presence of water is indicated by surface foam on heating,
5.7 Thermometer, 0 to 300°F (150°C).
maintain a representative portion of the bulk sample at a
temperature between 257 and 302°F (125 and 150°C) in an
5.8 Drying Oven, maintained at 221°F (105°C).
open container until the surface is free of foam. Take care not
5.9 Mortar and Pestle.
to overheat, and remove the heat source immediately when the
5.10 Two Wash Bottles, 500 mL. foam subsides.
5.11 Steam Bath. 9.3 Tar—Awet tar sample can either be dehydrated or used
as received as long as conditions stated in 9.3.1 and 9.3.2 are
6. Reagents
met.
9.3.1 Dehydrate a representative portion of the bulk sample.
6.1 Quinoline—Refined, meeting the following require-
9.3.2 As an alternative to dehydration, the water content of
ments:
the tar is determined by Test Method D95 and, if the water
6.1.1 The quinoline shall be distilled from 5 to 95 % within
content is less than 10 weight %, the QI content is corrected to
a range of 2°F (1°C) that shall include the temperature of
a dry-tar basis (see 13.2). This alternative method applies only
459.3°F (237.4°C) after corrections for barometric pressure
to stable emulsions of water in tar, that is, no water separates
andemergentsteamhavebeenapplied.Thedistillationshallbe
when the tar sample is left undisturbed for 24 h at room
carried out in accordance with Method D850 using a total-
temperature.
immersion thermometer with a range from 383 to 581°F (195
to 305°C), graduated in 1°F (0.5°C) and conforming to the
10. Preparation of Working Sample
requirements for thermometer 69C as described in Specifica-
tion E1. 10.1 Pitch that is sufficiently hard at room temperature shall
6.1.2 The quinoline shall have a specific gravity at 15.5/ be finely pulverized in a mortar. Crush this sample
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