ASTM D2318-98(2008)
(Test Method)Standard Test Method for Quinoline-Insoluble (QI) Content of Tar and Pitch
Standard Test Method for Quinoline-Insoluble (QI) Content of Tar and Pitch
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.
1.2 Since this test method is empirical, strict adherence to all details of the procedure is necessary.
1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this 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. For hazards information, see Section 7.
General Information
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Standards Content (Sample)
NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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: D2318 − 98(Reapproved 2008)
Standard Test Method for
Quinoline-Insoluble (QI) Content of Tar and Pitch
This standard is issued under the fixed designation D2318; 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
3.1 The sample is digested in hot quinoline and filtered.The
1.1 This test method covers the determination of the
insoluble material is washed, dried, and weighed.
quinoline-insoluble matter (QI) in tar and pitch.
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 SI units are to be regarded as
izing tar and pitch, and as one element in establishing the
standard. No other units of measurement are included in this
uniformity of shipments and sources of supply.
standard.
5. Apparatus
1.4 This standard does not purport to address all of the
5.1 Filtering Crucibles, porcelain, with fine-porosity
safety concerns, if any, associated with its use. It is the
bottom, 25 to 40-mL capacity, high-form, maximum pore
responsibility of the user of this standard to establish appro-
diameter, 7 µm.
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use. For hazards
5.2 Filter Apparatus—Filter flask and tube with crucible
information, see Section 7.
adapter.
5.3 Sieves—U. S. Standard 600-µm (No. 30) and 250-µm
2. Referenced Documents
(No. 60), conforming to Specification E11.
2.1 ASTM Standards:
5.4 Electric Hot Plate or Water Bath, maintained at 75 6
D71 Test Method for Relative Density of Solid Pitch and
5°C.
Asphalt (Displacement Method)
D95 Test Method for Water in Petroleum Products and
6. Reagents and Materials
Bituminous Materials by Distillation
6.1 Quinoline, Refined,meetingthefollowingrequirements:
D329 Specification for Acetone
6.1.1 The quinoline shall distill from 5 to 95 % within a
D362 SpecificationforIndustrialGradeToluene(Withdrawn
rangeof2°Cthatshallincludethetemperatureof237.4°Cafter
1989)
corrections for barometric pressure and emergent stem have
D850 Test Method for Distillation of Industrial Aromatic
been applied.The distillation shall be carried out in accordance
Hydrocarbons and Related Materials
with Test Method D850 using a total immersion thermometer
D4296 Practice for Sampling Pitch
with a range from 195 to 305°C, graduated in 0.5°C, and
E1 Specification for ASTM Liquid-in-Glass Thermometers
conforming to the requirements for Thermometer 69C as
E11 Specification for Woven Wire Test Sieve Cloth and Test
described in Specification E1.
Sieves
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 other method of equivalent accuracy.
This test method is under the jurisdiction of ASTM Committee D02 on
6.1.3 Thequinolineshallbeclearandlightincolorandshall
Petroleum Products and Lubricantsand is the direct responsibility of Subcommittee
contain less than 0.5 volume % of water as determined by Test
D02.05 on Properties of Fuels, Petroleum Coke and Carbon Material.
Method D95. If not, redistill the quinoline in all-glass
Current edition approved Oct. 15, 2008. Published November 2008. Originally
approved in 1964. Last previous edition approved in 2003 as D2318–98(2003).
apparatus, discarding the first 5 % and collecting the next
DOI: 10.1520/D2318-98R08.
90 %. If the quinoline contains suspended matter but is clear,
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
light in color, and contains less than 0.5 % water, filter the
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 quinolinethroughacruciblecontaining5gofCeliteFilterAid.
the ASTM website.
6.1.4 Store the quinoline in a tightly closed, dark bottle.
The last approved version of this historical standard is referenced on
www.astm.org. 6.2 Toluene, Industrial Pure, meeting Specification D362.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D2318 − 98 (2008)
6.3 Acetone, meeting Specification D329. crushing, mixing, and quartering of a representative portion of
the dry sample. The crushing can be done with a small jaw
6.4 Concentrated Hydrochloric Acid.
crusher and a mullite mortar and pestle. No particle in the
6.5 Celite Analytical Filter Aid (CAFA)—Dry to constant
representative sample shall be larger than 5 mm in any
weight at 105°C, and store in tightly stoppered container.
dimension. Crush this sample so that all of it will pass the
6.5.1 Do not use any other grade of filter aid because
250-µm (No. 60) sieve but will have a minimum of fine
filtration characteristics may differ. CAFA is manufactured
particles. Store the sieved working sample in a tightly closed
only by Manville Co. and distributed through scientific supply
container and use within 24 h (see 10.4).
houses.
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
7. Hazards
the lowest temperature that will permit passage through the
7.1 Fumes of the solvents should be removed by means of
600-µm (No. 30) sieve, taking care to avoid excessive loss of
proper hoods from all working areas. The working area should
volatile matter. Do not exceed 10 min for this melting period.
be kept free of sparks and flames. Quinoline fumes should not
Pass the heated sample through the 600-µm sieve to remove
be inhaled, and prolonged contact with the skin should be
foreign matter.
avoided. Toluene is toxic and flammable.
10.3 Tar—Heat a representative portion of the dry tar to the
7.2 Observe proper laboratory procedures for handling hy-
lowest temperature that will permit passage through the
drochloric and diluting acid.
600-µm (No. 30) sieve, then filter through this sieve to remove
foreign matter.
8. Bulk Sampling
10.4 Preservation of Samples—Store samples as large
8.1 Samples from shipments shall be taken in accordance
lumps or as solidified melts in closed containers. Discard
with Practice D4296 and shall be free of foreign substances.
working samples 24 h after crushing and sieving as changes in
Thoroughly mix the sample immediately before removing a
composition sometimes occur in pulverized pitch.
representative portion for the determination or for dehydration.
11. Crucible Preparations
9. Dehydration of Sample
11.1 If the crucible, after thorough cleaning (see 11.2), has
9.1 Hard Pitch—If the solid bulk sample contains free
been used for less than six determinations, clean it as follows:
water, air-dry a representative portion in a forced draft oven at
Remove the mat, wash the crucible with distilled water, dry,
50°C.
and ignite in a muffle furnace for1hat about 800°C. Cool the
crucible slowly by placing it in a drying oven for 1 h after
9.2 Soft Pitch—If the presence of water is indicated by
removal from the furnace to prevent cracking and place it in a
surface foam on heating, maintain a representative portion of
desiccator while still warm.
the bulk sample at a temperature between 125 and 150°C in an
open container until the surface is free of foam. Take care not
11.2 After the crucible has been used for six determinations,
to overheat, and remove heat source immediately when foam
remove any residual ash from pores in the filtering area by
subsides.
boiling in 1 + 1 hydrochloric acid. Add equal volume of
concentrated hydrochloric acid to distilled water. Then boil t
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