ASTM D2318-98(2003)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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An American National Standard
Designation:D2318–98 (Reapproved 2003)
Standard Test Method for
Quinoline-Insoluble (QI) Content of Tar and Pitch
This standard is issued under the fixed designation D 2318; 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. izing tar and pitch, and as one element in establishing the
1.2 Since this test method is empirical, strict adherence to uniformity of shipments and sources of supply.
all details of the procedure is necessary.
5. Apparatus
1.3 The values stated in SI units are to be regarded as the
5.1 Filtering Crucibles, porcelain, with fine-porosity bot-
standard.
1.4 This standard does not purport to address all of the tom, 25 to 40-mL capacity, high-form, maximum pore diam-
eter, 7 µm.
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro- 5.2 Filter Apparatus—Filter flask and tube with crucible
adapter.
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use. See Section 7. 5.3 Sieves—U. S. Standard 600-µm (No. 30) and 250-µm
(No. 60), conforming to SpecificationE11.
2. Referenced Documents
5.4 Electric Hot Plate or Water Bath, maintained at 75 6
2.1 ASTM Standards: 5°C.
D71 Test Method for Relative Density of Solid Pitch and
6. Reagents and Materials
Asphalt (Displacement Method)
6.1 Quinoline, Refined,meetingthefollowingrequirements:
D95 Test Method for Water in Petroleum Products and
Bituminous Materials by Distillation 6.1.1 The quinoline shall distill from 5 to 95 % within a
rangeof2°Cthatshallincludethetemperatureof237.4°Cafter
D 329 Specification for Acetone
D 362 Specification for Industrial Grade Toluene corrections for barometric pressure and emergent stem have
D 850 Test Method for Distillation of Industrial Aromatic been applied.The distillation shall be carried out in accordance
with Test Method D 850 using a total immersion thermometer
Hydrocarbons and Related Materials
D 4296 Practice for Sampling Pitch with a range from 195 to 305°C, graduated in 0.5°C, and
conforming to the requirements for Thermometer 69C as
E1 Specification for ASTM Thermometers
E11 Specification for Wire Cloth and Sieves for Testing described in SpecificationE1.
6.1.2 The quinoline shall have a specific gravity at 15.5/
Purposes
15.5°C of 1.092 to 1.098, as determined by Test MethodD71,
3. Summary of Test Method
or other method of equivalent accuracy.
3.1 The sample is digested in hot quinoline and filtered.The 6.1.3 Thequinolineshallbeclearandlightincolorandshall
insoluble material is washed, dried, and weighed. contain less than 0.5 volume % of water as determined by Test
Method D95. If not, redistill the quinoline in all-glass appa-
1 ratus, discarding the first 5 % and collecting the next 90 %. If
This test method is under the jurisdiction of ASTM Committee D02 on
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee the quinoline contains suspended matter but is clear, light in
D02.05 on Properties of Fuels, Petroleum Coke and Carbon Material.
color, and contains less than 0.5 % water, filter the quinoline
Current edition approved Nov. 1, 2003. Published November 2003. Originally
through a crucible containing5gof Celite Filter Aid.
approved in 1964. Last previous edition approved in 1998 as D 2318–98.
6.1.4 Store the quinoline in a tightly closed, dark bottle.
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
6.2 Toluene, Industrial Pure, meeting Specification D 362.
Standards volume information, refer to the standard’s Document Summary page on
6.3 Acetone, meeting Specification D 329.
the ASTM website.
3 6.4 Concentrated Hydrochloric Acid.
Withdrawn.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D2318–98 (2003)
6.5 Celite Analytical Filter Aid (CAFA)—Dry to constant 250-µm (No. 60) sieve but will have a minimum of fine
weight at 105°C, and store in tightly stoppered container. particles. Store the sieved working sample in a tightly closed
6.5.1 Do not use any other grade of filter aid because container and use within 24 h (see 10.4).
filtration characteristics may differ. CAFA is manufactured 10.2 Soft Pitch—If the pitch is too soft to grind and too
only by Manville Co. and distributed through scientific supply sticky to mix, heat a representative portion of the dry sample to
houses. the lowest temperature that will permit passage through the
600-µm (No. 30) sieve, taking care to avoid excessive loss of
7. Hazards
volatile matter. Do not exceed 10 min for this melting period.
7.1 Fumes of the solvents should be removed by means of Pass the heated sample through the 600-µm sieve to remove
proper hoods from all working areas. The working area should
foreign matter.
be kept free of sparks and flames. Quinoline fumes should not 10.3 Tar—Heat a representative portion of the dry tar to the
be inhaled, and prolonged contact with the skin should be
lowest temperature that will permit passage through the
avoided. Toluene is toxic and flammable. 600-µm (No. 30) sieve, then filter through this sieve to remove
7.2 Observe proper laboratory procedures for handling hy-
foreign matter.
drochloric and diluting acid.
10.4 Preservation of Samples—Store samples as large
lumps or as solidified melts in closed containers. Discard
8. Bulk Sampling
working samples 24 h after crushing and sieving as changes in
8.1 Samples from shipments shall be taken in accordance
composition sometimes occur in pulverized pitch.
with Practice D 4296 and shall be free of foreign substances.
Thoroughly mix the sample immediately before removing a
11. Crucible Preparations
representative portion for the determination or for dehydration.
11.1 If the crucible, after thorough cleaning (see 11.2), has
been used for less than six determinations, clean it as follows:
9. Dehydration of Sample
Remove the mat, wash the crucible with distilled water, dry,
9.1 Hard Pitch—If the solid bulk sample contains free
and ignite in a muffle furnace for1hat about 800°C. Cool the
water, air-dry a representative portion in a forced draft oven at
crucible slowly by placing it in a drying oven for 1 h after
50°C.
removal from the furnace to prevent cracking and place it in a
9.2 Soft Pitch—If the presence of water is indicated by
desiccator while still warm.
surface foam on heating, maintain a representative portion of
11.2 After the crucible has been used for six determinations,
the bulk sample at a temperature between 125 and 150°C in an
remove any residual ash from pores in the filtering area by
open container until the surface is free of foam. Take care not
boiling in 1 + 1 hydrochloric acid. Add equal volume of
to overheat, and remove heat source immediately when foam
concentrated hydrochloric acid to distilled water. Then boil the
subsides.
crucible in distilled water, thoroughly back wash with distilled
9.3 Tar—Awettarsamplemayeitherbedehydratedorused
water, dry, and ignite as in 11.1.
as received as long as conditions stated in 9.3.1 and 9.3.2 are
met.
12. Procedure
9.3.1 Dehydrate a representative portion of the
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