Standard Test Method for Determination of Quinoline Insolubles (QI) in Tar and Pitch by Pressure Filtration

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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Historical
Publication Date
09-Dec-1998
Current Stage
Ref Project

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ASTM D4746-98 - Standard Test Method for Determination of Quinoline Insolubles (QI) in Tar and Pitch by Pressure Filtration
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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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: D 4746 – 98 An American National Standard
AMERICAN SOCIETY FOR TESTING AND MATERIALS
100 Barr Harbor Dr., West Conshohocken, PA 19428
Reprinted from the Annual Book of ASTM Standards. Copyright ASTM
Standard Test Method for
Determination of Quinoline Insolubles (QI) in Tar and Pitch
1
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.
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.
Method D 2318.
5. Apparatus
1.2 Since this test method is empirical, strict adherence to
all details of the procedure is necessary. 5.1 Pressure Filtration Vessel—The pressure filtration ves-
7
sel (see Fig. 1) is a stainless steel (304) jacketed block heated
1.3 This standard does not purport to address all of the
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
placed on top of the block and clamped. The adjustable plunger
2.1 ASTM Standards: applies a force to the crucible sealing collar, which in turn
D 70 Test Method for Density of Semi-Solid Bituminous pushes downward on the crucible and simultaneously com-
2
Materials (Pycnometer Method) presses O-ring gaskets, forming a seal between surfaces of the
D 95 Test Method for Water in Petroleum Products and crucible and the wall of the block. The filtration of material is
3
Bituminous Materials by Distillation accomplished by nitrogen (10 to 30 psig) introduced through
4
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
4
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
3
of Tar and Pitch a 100-mL beaker containing water to indicate the exit of
5
D 4296 Practice for Sampling Pitch nitrogen when the filtration is completed.
6
E 1 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
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 consequently with cold 5.5 Analytical Balance.
acetone, dried, and weighed.
5.6 Desiccator.
5.7 Thermometer, 0 to 300°F (150°C).
5.8 Drying Oven, maintained at 221°F (105°C).
5.9 Mortar and Pestle.
1
This test method is under the jurisdiction of ASTM Committee D-2 on
5.10 Two Wash Bottles, 500 mL.
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee
5.11 Steam Bath.
D02.05.OFon Industrial Pitches.
Current edition approved Dec. 10, 1998. Published February 1999. Originally
published as D 4746 – 87. Last previous edition D 4746 – 97.
2
Annual Book of ASTM Standards, Vol 04.03.
7
3
The sole source of supply of the pressure filtration vessel known to the
Annual Book of ASTM Standards, Vol 05.01.
4
committee at this time is Koppers Co., Inc., 1005 Wm. Pitt Way, Pittsburgh, PA
Annual Book of ASTM Standards, Vol 06.04.
5
15238. If you are aware of alternative suppliers, please provide this information to
Annual Book of ASTM Standards, Vol 05.02.
6
ASTM Headquarters. Your comments will receive careful consideration at a meeting
Annual Book of ASTM Standards, Vol 14.03.
1
of the responsible technical committee, which you may attend.
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