ASTM D7280-20

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: D7280 − 15 D7280 − 20
Standard Test Method for
Quinoline-Insoluble (QI) Content of Tar and Pitch by
Stainless Steel Crucible Filtration
This standard is issued under the fixed designation D7280; 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*
1.1 This test method covers the determination of the quinoline-insoluble matter (QI) in tar and pitch using a stainless steel
filtering crucible and a filtration membrane.
1.2 This test method was evaluated in round robin testing using materials in the range of zero to twenty quinoline insoluble
weight percent (wt%).
1.3 Since this test method is empirical, strict adherence to all details of the procedure is necessary.
1.4 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.5 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.
1.6 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:
D71 Test Method for Relative Density of Solid Pitch and Asphalt (Displacement Method)
D95 Test Method for Water in Petroleum Products and Bituminous Materials by Distillation
D329 Specification for Acetone
D362 Specification for Industrial Grade Toluene (Withdrawn 1989)
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
E691 Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method
3. Summary of Test Method
3.1 The sample is digested in hot quinoline and filtered. The insoluble material is washed, dried, and weighed.
4. Significance and Use
4.1 This test method is useful in evaluating and characterizing tar and pitch. It is also useful 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 Dec. 1, 2015June 1, 2020. Published December 2015July 2020. Originally approved in 2006. Last previous edition approved in 20112015 as
D7280 – 06 (2011).D7280 – 15. DOI: 10.1520/D7280-15.10.1520/D7280-20.
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.
The last approved version of this historical standard is referenced on www.astm.org.
*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
D7280 − 20
5. Apparatus
5.1 Filtering Crucibles, stainless steel, with fine-screen bottom, 25 mL to 40 mL capacity, high-form. See Fig. 1.
5.2 Filter Membrane, PFTE membrane without backing, 10 μm porosity, 25 mm disk.
5.3 Filter Apparatus, 500 mL filter flask and tube with crucible adapter.
5.4 Sieves, U.S. Standard 600 μm (No. 30) and 250 μm (No. 60), conforming to Specification E11.
5.5 Electric Hot Plate or Water Bath, maintained at 75 °C 6 5 °C.
FIG. 1 Stainless Steel Filtering Crucible with Support Disk
The sole source of supply of the crucibles known to the committee at this time is Drabik Tool & Die, 15601 Commerce Park Dr., Cleveland, OH 44142. If you are aware
of alternative suppliers, please provide this information to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of the responsible
technical committee, which you may attend.
The sole source of supply of the filter membranes known to the committee at this time is Mitex brand, Part No. LCWP 02500, available from Millipore Corporation,
290 Concord Road Billerica, MA 01821. If you are aware of alternative suppliers, please provide this information to ASTM International Headquarters. Your comments will
receive careful consideration at a meeting of the responsible technical committee, which you may attend.
D7280 − 20
6. Reagents and Materials
6.1 Quinoline, Refined—meeting the following requirements:
6.1.1 The quinoline shall distill from 5 % to 95 % within a range of 2 °C that shall include the temperature of 237.4 °C after
corrections for barometric pressure and emergent stem have been applied. The distillation shall be carried out in accordance with
Test Method D850 using a total immersion thermometer with a range from 195 °C to 305 °C, graduated in 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 ranges can 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 D71, or
another method of equivalent accuracy.
6.1.3 The quinoline shall be clear and light in color and shall contain less than 0.5 0.5 % by volume % of water, as determined
by Test Method D95. If not, redistill the quinoline in 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
6,5
a crucible containing 5 g of diatomaceous earth filter aid.
6.1.4 Store the quinoline in a tightly closed, dark bottle.
6.2 Toluene, Industrial Pure, meeting Specification D362.
6.3 Acetone, meeting Specification D329.
6.4 Filter Aid—Dry to constant weight at 105 °C, and store in tightly stoppered container.
NOTE 1—Manville Certified Analytical Filter Aid (CAFA) or Supelco/Sigma Aldrich (CAFA II) Part #11485U were used in determining precision and
bias and were found to give acceptable filtration performance. Any other grade of filter aid may differ in filtration characteristics.
7. Hazards
7.1 Fumes of the solvents should be removed by means of proper hoods from all working areas.
7.2 The working area should be kept free of sparks and flames.
7.3 Quinoline fumes should not be inhaled, and prolonged contact with the skin should be avoided.
7.4 Toluene is toxic and flammable.
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 50 °C.
9.2 Soft Pitch—If the presence of water is indicated by surface foam on heating, maintain a representative portion of the bulk
sample at a temperature between 125 °C and 150 °C in an open container until the surface is free of foam. Take care not to
overheat, and remove heat source immediately when foam subsides.
9.3 Tar—A wet tar sample may either be dehydrated or used as received as long as conditions stated in 9.3.1 and 9.3.3 are met.
9.3.1 Dehydrate a representative portion of the bulk sample at atmospheric pressure using a simple side-arm distillation
apparatus similar to the one in Test Method D850, and stop the distillation when the temperature reaches 170 °C.
9.3.2 Separate any oil from the water that has distilled over (if crystals are present, warm sufficiently to ensure their solution),
and thoroughly mix the oil with the residual tar in the still after the latter has cooled to a moderate temperature.
9.3.3 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 mass %,10 % by mass, the QI content is corrected to a dry-tar basis (see 13.2). This alternative test 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 Hard Pitch—If the pitch can be crushed at room temperature, prepare a 20 g working sample by suitable crushing, mixing,
and quartering of a representative portion of the dry sample. The crushing can be done with a small jaw crusher and a Mullite
mortar and pestle. No particle in the representative sample shall be larger than 5 mm in any dimension.
10.1.1 Crush this sample so that all of it will pass the 250 m250 μm (No. 60) sieve but will have a minimum of fine particles.
The sole source of supply of the diatomaceous earth filter aid known to the committee at this time is Celite, available from World Minerals, Santa Barbara, CA. If you
are aware of alternative suppliers, please provide this information to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of
the responsible technical committee, which you may attend.
D7280 − 20
10.1.2 Store the sieved working sample in a tightly closed container, and use within 24 h (see 10.4).
10.2 Soft Pitch—If the pitch is too soft to grind and too sticky to mix, heat a representative portion of the dry sample to the
lowest temperature that will permit passage through the 600 μm (No. 30) sieve, taking care to avoid excessive loss of volatile
matter. Do not exceed 10 min for this melting period.
10.2.1 Pass the heated sample through the 600 μm (No. 30) sieve to remove foreign matter.
10.3 Tar—Heat a representative portion of the dry tar to the lowest tem
...