ASTM D7280-06(2011)
(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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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Designation: D7280 − 06(Reapproved 2011)
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 D2318 Test Method for Quinoline-Insoluble (QI) Content of
Tar and Pitch
1.1 This test method covers the determination of the
D4296 Practice for Sampling Pitch
quinoline-insoluble matter (QI) in tar and pitch using a
E1 Specification for ASTM Liquid-in-Glass Thermometers
stainless steel filtering crucible and a filtration membrane.
E11 Specification for Woven Wire Test Sieve Cloth and Test
1.2 This test method was evaluated in round robin testing
Sieves
using materials in the range of zero to twenty quinoline
E691 Practice for Conducting an Interlaboratory Study to
insoluble weight percent (wt%).
Determine the Precision of a Test Method
1.3 Since this test method is empirical, strict adherence to
all details of the procedure is necessary. 3. Summary of Test Method
1.4 The values stated in SI units are to be regarded as 3.1 Thesampleisdigestedinhotquinolineandfiltered.The
standard. No other units of measurement are included in this insoluble material is washed, dried, and weighed.
standard.
4. Significance and Use
1.5 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the
4.1 This test method is useful in evaluating and character-
responsibility of the user of this standard to establish appro-
izing tar and pitch. It is also useful as one element in
priate safety and health practices and determine the applica-
establishingtheuniformityofshipmentsandsourcesofsupply.
bility of regulatory limitations prior to use.
5. Apparatus
2. Referenced Documents
5.1 Filtering Crucibles, stainless steel, with fine–screen
2.1 ASTM Standards:
bottom, 25 to 40-mL capacity, high-form. See Fig. 1.
D71 Test Method for Relative Density of Solid Pitch and
5.2 Filter Membrane, PFTE membrane without backing,
Asphalt (Displacement Method)
10-µm porosity, 25-mm disk.
D95 Test Method for Water in Petroleum Products and
Bituminous Materials by Distillation 5.3 Filter Apparatus, 500-mL filter flask and tube with
crucible adapter.
D329 Specification for Acetone
D362 SpecificationforIndustrialGradeToluene(Withdrawn
5.4 Sieves,U.S.Standard600-µm(No.30)and250-µm(No.
1989)
60), conforming to Specification E11.
D850 Test Method for Distillation of Industrial Aromatic
5.5 Electric Hot Plate or Water Bath, maintained at 75 6
Hydrocarbons and Related Materials
5°C.
This test method is under the jurisdiction of ASTM Committee D02 on
Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of The sole source of supply of the crucibles known to the committee at this time
SubcommitteeD02.05onPropertiesofFuels,PetroleumCokeandCarbonMaterial. is Drabik Tool & Die, 15601 Commerce Park Dr., Cleveland, OH 44142. If you are
Current edition approved May 1, 2011. Published May 2011. Originally aware of alternative suppliers, please provide this information to ASTM Interna-
ε1
approved in 2006. Last previous edition approved in 2006 as D7280 – 06 . DOI: tional Headquarters.Your comments will receive careful consideration at a meeting
10.1520/D7280-06R11. of the responsible technical committee, which you may attend.
2 5
For referenced ASTM standards, visit the ASTM website, www.astm.org, or The sole source of supply of the filter membranes known to the committee at
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM this time is Mitex brand, Part No. LCWP 02500, available from Millipore
Standards volume information, refer to the standard’s Document Summary page on Corporation,290ConcordRoadBillerica,MA01821.Ifyouareawareofalternative
the ASTM website. suppliers, please provide this information to ASTM International Headquarters.
The last approved version of this historical standard is referenced on Your comments will receive careful consideration at a meeting of the responsible
www.astm.org. technical committee, which you may attend.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D7280 − 06 (2011)
FIG. 1 Stainless Steel Filtering Crucible with Support Disk
6. Reagents and Materials 6.1.3 Thequinolineshallbeclearandlightincolorandshall
contain less than 0.5 volume % of water, as determined byTest
6.1 Quinoline, Refined—meeting the following require-
Method D95. If not, redistill the quinoline in all-glass
ments:
apparatus, discarding the first 5 % and collecting the next
6.1.1 The quinoline shall distill from 5 to 95 % within a
90 %. If the quinoline contains suspended matter but is clear,
rangeof2°Cthatshallincludethetemperatureof237.4°Cafter
light in color, and contains less than 0.5 % water, filter the
corrections for barometric pressure and emergent stem have
quinoline through a crucible containing5gof diatomaceous
beenapplied.Thedistillationshallbecarriedoutinaccordance
6,5
earth filter aid.
with Test Method D850 using a total immersion thermometer
with a range from 195 to 305°C, graduated in 0.5°C, and
conforming to the requirements for Thermometer 69C as
The sole source of supply of the diatomaceous earth filter aid known to the
described in Specification E1.
committee at this time is Celite, available fromWorld Minerals, Santa Barbara, CA.
6.1.2 The quinoline shall have a specific gravity at 15.5/
If you are aware of alternative suppliers, please provide this information to ASTM
15.5°C of 1.092 to 1.098, as determined by Test Method D71,
International Headquarters. Your comments will receive careful consideration at a
or another method of equivalent accuracy. meeting of the responsible technical committee, which you may attend.
D7280 − 06 (2011)
6.1.4 Store the quinoline in a tightly closed, dark bottle. 10. Preparation of Working Sample
10.1 Hard Pitch—If the pitch can be crushed at room
6.2 Toluene, Industrial Pure, meeting Specification D362.
temperature, prepare a 20-g working sample by suitable
6.3 Acetone, meeting Specification D329.
crushing, mixing, and quartering of a representative portion of
6.4 Filter Aid—Dry to constant weight at 105°C, and store the dry sample. The crushing can be done with a small jaw
crusher and a Mullite mortar and pestle. No particle in the
in tightly stoppered container.
representative sample shall be larger than 5 mm in any
NOTE 1—Manville Certified Analytical Filter Aid (CAFA) or Supelco/
dimension.
Sigma Aldrich (CAFA II) Part #11485U were used in determining
10.1.1 Crush this sample so that all of it will pass the
precision and bias and were found to give acceptable filtration perfor-
250-µm (No. 60) sieve but will have a minimum of fine
mance.Any other grade of filter aid may differ in filtration characteristics.
particles.
7. Hazards 10.1.2 Store the sieved working sample in a tightly closed
container, and use within 24 h (see 10.4).
7.1 Fumes of the solvents should be removed by means of
10.2 Soft Pitch—If the pitch is too soft to grind and too
proper hoods from all working areas.
stickytomix,heatarepresentativeportionofthedrysampleto
7.2 The working area should be kept free of sparks and
the lowest temperature that will permit passage through the
flames.
600-µm (No. 30) sieve, taking care to avoid excessive loss of
volatile matter. Do not exceed 10 min for this melting period.
7.3 Quinoline fumes should not be inhaled, and prolonged
contact with the skin should be avoided. 10.2.1 Pass the heated sample through the 600-µm sieve to
remove foreign matter.
7.4 Toluene is toxic and flammable.
10.3 Tar—Heat a representative portion of the dry tar to the
lowest temperature that will permit passage through the
8. Bulk Sampling
600-µm (No. 30) sieve, then filter through this sieve to remove
8.1 Samples from shipments shall be taken in accordance
foreign matter.
with Practice D4296 and shall be free of foreign substances.
10.4 Preservation of Samples—Store samples as large
Thoroughly mix the sample immediately before removing a
lumps or as solidified melts in closed containers. Discard
representative portion for the determination or for dehydration.
working samples 24 h after crushing and sieving as changes in
composition sometimes occur in pulverized pitch.
9. Dehydration of Sample
9.1 Hard Pitch—If the solid bulk sample contains free
11. Filter Crucible Preparation
water, air-dry a representative portion in a forced draft oven at
11.1 Unscrew the bottom ring of the filtering crucible and
50°C.
inspect the support disk and the ring surfaces to be certain that
9.2 Soft Pitch—If the presence of water is indicated by
they are free of any foreign particles.
surface foam on heating, maintain a representative portion of
11.2 Placethesupportingdiskbackintotheringandseatthe
the bulk sample at a temperature between 125 and 150°C in an
disk on the inside supporting shoulder of the ring.
open container until the surface is free of foam. Take care not
11.3 Using forceps, carefully place a single membrane over
to overheat, and remove heat source immediately when foam
the threaded part of the ring onto the support disk. The
subsides.
membrane must be centered exactly within the threaded hole.
9.3 Tar—Awet tar sample may either be dehydrated or used
11.4 Screw the barrel into the ring assemb
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