ASTM D4746-20

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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.
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Designation: D4746 − 14 D4746 − 20
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.
ε NOTE—Editorial changes were made throughout the test method in September 2014.
1. 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 safety, health, and healthenvironmental practices and determine the
applicability of regulatory limitations prior to use. Specific hazards are given in Section 7, 6.2, and 6.3.
1.5 This international standard was developed in accordance with internationally recognized principles on standardization
established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued
by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
2. Referenced Documents
2.1 ASTM Standards:
D70 Test Method for Density of Semi-Solid Asphalt Binder (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
E11 Specification for Woven Wire Test Sieve Cloth and Test Sieves
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.
This test method is under the jurisdiction of ASTM Committee D02 on Petroleum 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 May 1, 2014June 1, 2020. Published May 2014June 2020. Originally approved in 1987. Last previous edition approved in 20132014 as
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D4746 – 98 (2013).D4746 – 14 . DOI: 10.1520/D4746-14E01.10.1520/D4746-20.
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.
*A Summary of Changes section appears at the end of this standard
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D4746 − 20
5. Apparatus
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.
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 psig to 30 psig) introduced through the lid of the pressure filter. The filtrate exits from the drain tube at the bottom
of the block. The filtrate is disposed into a Buchner flask, attached to drain tube by a No. 7 rubber stopper. A vacuum hose is
attached to the Buchner flask and placed in a 100 mL beaker containing water to indicate the exit of nitrogen when the filtration
is completed.
5.2 Beaker, 50 mL.
5.3 Buchner Flask, 500.500 mL.
5.4 Filtering Crucible, porcelain, with a medium-porosity bottom, top outer diameter 11.75 in. ⁄4 in. (45 mm), bottom outer
diameter 1.2 in. (30 mm), height 2 in. (50 mm).
5.5 Analytical Balance.
5.6 Desiccator.
5.7 Thermometer, 0 °F to 300 °F (150 °C).
5.8 Drying Oven, maintained at 221 °F (105 °C).
5.9 Mortar and Pestle.
5.10 Two Wash Bottles, 500 mL.
FIG. 1 Pressure Filter
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
technical committee, which you may attend.
D4746 − 20
5.11 Steam Bath.
5.12 Sieves—U.S. Standard 600 μm (No. 30) and 250 μm (No. 60).
6. Reagents
6.1 Quinoline—Refined, meeting the following requirements:
6.1.1 The quinoline shall be distilled from 5 % to 95 % within a range of 2 °F (1 °C) that shall include the temperature of
459.3 °F (237.4 °C) after corrections for barometric pressure and emergent steam have been applied. The distillation shall be
carried out in accordance with Method D850 using a total-immersion thermometer with a range from 383 °F to 581°F (195 °C to
305°C),305 °C), graduated in 1 °F (0.5 °C) and conforming to the requirements for thermometer 69C as described in Specification
E1. Temperature measuring devices such as precision thermocouples, resistance temperature detectors (RTDs), and liquid-in-glass
thermometers with equal or better accuracies in the appropriate temperature range may be used.
6.1.2 The quinoline shall have a specific gravity at 15.5/15.5 °C of 1.092 to 1.098, as determined by Test Method D70, or other
method of equivalent accuracy.
6.1.3 The quinoline shall be clear and light in color and shall contain less than 0.5 volume percent of water as determined by
Test Method D95. If not, redistill the quinoline in an all-glass apparatus, discarding the first 5 % and collecting the next 90 %. 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 containing 5 g of 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.
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 °F and 302 °F (125 °C 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 foam subsides.
9.3 Tar—A wet tar sample can either be dehydrated or used as received as long as conditions stated in 9.3.1 and 9.3.2 are met.
9.3.1 Dehydrate a representative portion of the bulk sample.
9.3.2 As an alternative to dehydration, the water content of the tar is determined by Test Method D95 and, if the water content
is less than 10 weight percent,10 % by mass, the QI content is corrected to a dry-tar basis (see 13.2). This alternative method
applies only to stable emulsions of water in tar, that is, no water separates when the tar sample is left undisturbed for 24 h at room
temperature.
10. Preparation of Working Sample
10.1 Pitch that is suff
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