ASTM D4746-14
(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
4.1 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 D2318.
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.
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Designation: D4746 − 14
StandardTest Method for
Determination of Quinoline Insolubles (QI) in Tar and Pitch
1
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-
3
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.
2
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.
1
This test method is under the jurisdiction of ASTM Committee D02 on
5.3 Buchner Flask, 500.
Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of
SubcommitteeD02.05onPropertiesofFuels,PetroleumCokeandCarbonMaterial.
Current edition approved May 1, 2014. Published May 2014. Originally
approved in 1987. Last previous edition approved in 2013 as D4746 – 98 (2013).
3
DOI: 10.1520/D4746-14. The sole source of supply of the pressure filtration vessel known to the
2
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
1
the ASTM website. meeting of the responsible technical committee, which you may attend.
*A Summary of Changes section appears at the end of this standard
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1
---------------------- Page: 1 ----------------------
D4746 − 14
6.1.2 The quinoline shall have a specific gravity at 15.5/
15.5°C o
...
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.
Designation: D4746 − 98 (Reapproved 2013) D4746 − 14
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 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 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 D2318.
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.
2. Referenced Documents
2
2.1 ASTM Standards:
D70 Test Method for Density of Semi-Solid Bituminous Materials (Pycnometer Method)
D95 Test Method for Water in Petroleum Products and Bituminous Materials by Distillation
D329 Specification for Acetone
D850 Test Method for Distillation of Industrial Aromatic Hydrocarbons and Related Materials
D2318 Test Method for Quinoline-Insoluble (QI) Content of Tar and Pitch
D4296 Practice for Sampling Pitch
E1 Specification for ASTM Liquid-in-Glass Thermometers
3. Summary of Test Method
3.1 The sample is digested in hot quinoline and filtered through a heated pressure filter. The insoluble material is washed with
hot, fresh quinoline and with cold acetone, dried, and weighed.
4. Significance and Use
4.1 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.
5. Apparatus
3
5.1 Pressure Filtration Vessel—The pressure filtration vessel (see Fig. 1) is a stainless steel (304) jacketed block heated by
steam or cooled with water, sealed by a lid, flat gasket, and clamp. The interior of the block is designed to accept a 3A2 Berlin
porcelain filtration crucible (see 5.4). The crucible is sealed within the block by the use of three O-rings, a crucible sealing collar,
and an adjustable plunger.
1
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 July 15, 2013May 1, 2014. Published August 2013May 2014. Originally approved in 1987. Last previous edition approved in 20082013 as
D4746 – 98 (2008).(2013). DOI: 10.1520/D4746-98R13.10.1520/D4746-14.
2
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.
3
The sole source of supply of the pressure filtration vessel known to the committee at this time is Koppers Inc., 436 Seventh Ave., Pittsburgh, PA 15219-1800. If you
are aware of alternative suppliers, please provide this information to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible
1
technical committee, which you may attend.
*A Summary of Changes section appears at the end of this standard
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1
---------------------- Page: 1 ----------------------
D4746 − 14
FIG. 1 Pressure Filter
5.1.1 The seal is accomplished when the sealing lid is placed on top of the block and clamped. The adjustable plunger applies
a force to the crucible sealing collar, which in turn pushes downward on the crucible and simultaneously compresses O-ring
gaskets, forming a seal between surfaces of the crucible and the wall of the block. The filtration of material is accomplished by
nitrogen (10 to 30 psig) introduced through the lid of the pressure filter
...
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