ASTM D7280-06
(Test Method)Standard Test Method for Quinoline-Insoluble (QI) Content of Tar and Pitch by Stainless Steel Crucible Filtration
Standard Test Method for Quinoline-Insoluble (QI) Content of Tar and Pitch by Stainless Steel Crucible Filtration
SIGNIFICANCE AND USE
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.
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 and health practices and determine the applicability of regulatory limitations prior to use.
General Information
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Standards Content (Sample)
NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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An American National Standard
Designation:D7280–06
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 D 7280; 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 E 691 Practice for Conducting an Interlaboratory Study to
Determine the Precision of a Test Method
1.1 This test method covers the determination of the
quinoline-insoluble matter (QI) in tar and pitch using a
3. Summary of Test Method
stainless steel filtering crucible and a filtration membrane.
3.1 Thesampleisdigestedinhotquinolineandfiltered.The
1.2 This test method was evaluated in round robin testing
insoluble material is washed, dried, and weighed.
using materials in the range of zero to twenty quinoline
insoluble weight percent (wt%).
4. Significance and Use
1.3 Since this test method is empirical, strict adherence to
4.1 This test method is useful in evaluating and character-
all details of the procedure is necessary.
izing tar and pitch. It is also useful as one element in
1.4 The values stated in SI units are to be regarded as
establishingtheuniformityofshipmentsandsourcesofsupply.
standard. No other units of measurement are included in this
standard.
5. Apparatus
1.5 This standard does not purport to address all of the
5.1 Filtering Crucibles, stainless steel, with fine–screen
safety concerns, if any, associated with its use. It is the
4,5
bottom, 25 to 40-mL capacity, high-form. See Fig. 1.
responsibility of the user of this standard to establish appro-
5.2 Filter Membrane, PFTE membrane without backing,
priate safety and health practices and determine the applica-
5,6
10-µm porosity, 25-mm disk.
bility of regulatory limitations prior to use.
5.3 Filter Apparatus, 500-mL filter flask and tube with
crucible adapter.
2. Referenced Documents
2 5.4 Sieves,U.S.Standard600-µm(No.30)and250-µm(No.
2.1 ASTM Standards:
60), conforming to SpecificationE11.
D71 Test Method for Relative Density of Solid Pitch and
5.5 Electric Hot Plate or Water Bath, maintained at 75 6
Asphalt (Displacement Method)
5°C.
D95 Test Method for Water in Petroleum Products and
Bituminous Materials by Distillation
6. Reagents and Materials
D 329 Specification for Acetone
6.1 Quinoline, Refined—meeting the following require-
D 362 Specification for Industrial Grade Toluene
ments:
D 850 Test Method for Distillation of Industrial Aromatic
6.1.1 The quinoline shall distill from 5 to 95 % within a
Hydrocarbons and Related Materials
rangeof2°Cthatshallincludethetemperatureof237.4°Cafter
D 2318 Test Method for Quinoline-Insoluble (QI) Content
corrections for barometric pressure and emergent stem have
of Tar and Pitch
beenapplied.Thedistillationshallbecarriedoutinaccordance
D 4296 Practice for Sampling Pitch
with Test Method D 850 using a total immersion thermometer
E1 Specification forASTM Liquid-in-Glass Thermometers
with a range from 195 to 305°C, graduated in 0.5°C, and
E11 Specification for Wire Cloth and Sieves for Testing
conforming to the requirements for Thermometer 69C as
Purposes
described in SpecificationE1.
This test method is under the jurisdiction of ASTM Committee D02 on
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee The sole source of supply of the crucibles known to the committee at this time
D02.05 on Properties of Fuels, Petroleum Coke and Carbon Material. is Drabik Tool & Die, 15601 Commerce Park Dr., Cleveland, OH 44142.
Current edition approved Nov. 1, 2006. Published December 2006. If you are aware of alternative suppliers, please provide this information to
For referenced ASTM standards, visit the ASTM website, www.astm.org, or ASTM International Headquarters. Your comments will receive careful consider-
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM ation at a meeting of the responsible technical committee, which you may attend.
Standards volume information, refer to the standard’s Document Summary page on The sole source of supply of filter membranes known to the committee at this
the ASTM website. time is Mitex brand, Part No. LCWP 02500, available from Millipore Corporation,
Withdrawn. 290 Concord Road Billerica, MA 01821.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D7280–06
FIG. 1 Stainless Steel Filtering Crucible with Support Disk
6.1.2 The quinoline shall have a specific gravity at 15.5/ color, and contains less than 0.5 % water, filter the quinoline
15.5°C of 1.092 to 1.098, as determined by Test MethodD71, through a crucible containing5gof diatomaceous earth filter
7,6
aid.
or another method of equivalent accuracy.
6.1.4 Store the quinoline in a tightly closed, dark bottle.
6.1.3 Thequinolineshallbeclearandlightincolorandshall
6.2 Toluene, Industrial Pure, meeting Specification D 362.
contain less than 0.5 volume % of water, as determined byTest
Method D95. If not, redistill the quinoline in all-glass appa-
ratus, discarding the first 5 % and collecting the next 90 %. If 7
The sole source of supply of the diatomaceous earth filter aid known to the
the quinoline contains suspended matter but is clear, light in committee at this time is Celite, available fromWorld Minerals, Santa Barbara, CA.
D7280–06
6.3 Acetone, meeting Specification D 329. crusher and a Mullite mortar and pestle. No particle in the
6.4 Filter Aid—Dry to constant weight at 105°C, and store representative sample shall be larger than 5 mm in any
dimension.
in tightly stoppered container.
10.1.1 Crush this sample so that all of it will pass the
NOTE 1—Manville Certified Analytical Filter Aid (CAFA) or Supelco/
250-µm (No. 60) sieve but will have a minimum of fine
Sigma Aldrich (CAFA II) Part #11485U were used in determining
particles.
precision and bias and were found to give acceptable filtration perfor-
mance.Any other grade of filter aid may differ in filtration characteristics. 10.1.2 Store the sieved working sample in a tightly closed
container, and use within 24 h (see 10.4).
7. Hazards
10.2 Soft Pitch—If the pitch is too soft to grind and too
stickytomix,heatarepresentativeportionofthedrysampleto
7.1 Fumes of the solvents should be removed by means of
the lowest temperature that will permit passage through the
proper hoods from all working areas.
600-µm (No. 30) sieve, taking care to avoid excessive loss of
7.2 The working area should be kept free of sparks and
volatile matter. Do not exceed 10 min for this melting period.
flames.
10.2.1 Pass the heated sample through the 600-µm sieve to
7.3 Quinoline fumes should not be inhaled, and prolonged
remove foreign matter.
contact with the skin should be avoided.
10.3 Tar—Heat a representative portion of the dry tar to the
7.4 Toluene is toxic and flammable.
lowest temperature that will permit passage through the
600-µm (No. 30) sieve, then filter through this sieve to remove
8. Bulk Sampling
foreign matter.
8.1 Samples from shipments shall be taken in accordance
10.4 Preservation of Samples—Store samples as large
with Practice D 4296 and shall be free of foreign substances.
lumps or as solidified melts in closed containers. Discard
Thoroughly mix the sample immediately before removing a
working samples 24 h after crushing and sieving as changes in
representative portion for the determination or for dehydration.
composition sometimes occur in pulverized pitch.
9. Dehydration of Sample
11. Filter Crucible Preparation
9.1 Hard Pitch—If the solid bulk sample contains free
11.1 Unscrew the bottom ring of the filtering crucible and
water, air-dry a representative portion in a forced draft oven at
inspect the support disk and the ring surfaces to be certain that
50°C.
they are free of any foreign particles.
9.2 Soft Pitch—If the presence of water is indicated by
11.2 Placethesupportingdiskbackintotheringandseatthe
surface foam on heating, maintain a representative portion of
disk on the inside supporting shoulder of the ring.
the bulk sample at a temperature between 125 and 150°C in an
11.3 Using forceps, carefully place a single membrane over
open container until the surface is free of foam. Take care not
the threaded part of the ring onto the support disk. The
to overheat, and remove heat source immediately when foam
membrane must be centered exactly within the threaded hole.
subsides.
11.4 Screw the barrel into the ring assembly until it is finger
9.3 Tar—Awettarsamplemayeitherbedehydratedorused
tight. Do not overtighten the barrel and ring.
as received as long as conditions stated in 9.3.1 and 9.3.3 are
met.
12. Procedure
9.3.1 Dehydrate a representative portion of the bulk sample
at atmospheric pressure using a simple side-arm distillation 12.1 Make and record all weighings to the nearest 1 mg.
apparatussimilartotheoneinTestMethodD 850,andstopthe
12.2 Select a sample mass that will yield between 75 and
distillation when the temper
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