ASTM D5439-95(2001)
(Test Method)Standard Test Method for Determination of Sediment in Moellon
Standard Test Method for Determination of Sediment in Moellon
SCOPE
1.1 This test method covers the determination of the toluene insoluble sediment contained in Moellon. This test method was derived from Test Method D473.
1.2 The values stated in SI units are to be regarded as the standard.
1.3 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.
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Designation:D5439–95 (Reapproved 2001)
Standard Test Method for
Determination of Sediment in Moellon
This standard is issued under the fixed designation D 5439; 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
1.1 This test method covers the determination of the toluene
insoluble sediment contained in Moellon.This test method was
derived from Test Method D 473.
1.2 The values stated in SI units are to be regarded as the
standard.
1.3 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 appro-
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use.
NOTE 1—Apparatus B shows the water cup in position.
2. Referenced Documents
FIG. 1 Extraction Apparatus for Determination of Sediment
2.1 ASTM Standards:
D 473 Test Method for Sediment in Crude Oils and Fuel
2 sufficient diameter to cover the neck of the flask as shown in
Oils by the Extraction Method
Fig. 1. The coil should be made from stainless steel, tin,
D 4057 Practice for Manual Sampling of Petroleum and
3 tin-plated copper, or tin-plated brass tubing having an outside
Petroleum Products
diameter of 5 to 8 mm and a wall thickness of 1.5 mm. If
D 4177 Practice for Automatic Sampling of Petroleum and
3 constructed of tin-plated copper or brass, the tin coating shall
Petroleum Products
have a minimum thickness of 0.075 mm. The exposed surface
2.2 ISO Standard:
4 of the coil for cooling purposes is about 115 cm .
5272 Toluene-Specifications
4.1.3 Extraction Thimble—The extraction thimble should
3. Significance and Use be of a refractory porous material, pore size index P15, 25 mm
in diameter by 70 mm in height, weighing not less than 15 g
3.1 This test method is intended for use in determining the
and not more than 17 g. The thimble shall be suspended from
toluene insoluble sediment contained in Moellon.
the condenser coil by means of a basket so that it hangs
4. Apparatus
approximately midway between the surface of the extracting
solvent and the bottom of the condenser coil.
4.1 ExtractionApparatus (see Fig. 1 and Fig. 2), consisting
4.1.4 Thimble Basket—The thimble basket shall be
of the parts described in 4.1.1-4.1.6.
corrosion-resistant, shall be made of platinum, stainless steel,
4.1.1 ExtractionFlask,awide-neckErlenmeyerflaskof1-L
nickel-chromium alloy, or similar material, and shall meet the
capacity.
requirements of Fig. 2.
4.1.2 Condenser, a condenser in the form of a metal coil
4.1.5 Water Cup—Awater cup shall be used when testing a
approximately 25 mm in diameter and 50 mm in length
samplehavingahigh-watercontent(seeFig.1b).Thecupshall
attached to, and with the ends projecting through a lid of
be made of glass, shall be conical in shape, shall be approxi-
mately 20 mm in diameter and 25 mm deep, and shall have a
This test method is under the jurisdiction ofASTM Committee D31 on Leather
capacity of approximately 3 mL.Aglass hook fused on the rim
and is the direct responsibility of Subcommittee D31.08 on Fats and Oils. This test
at one side is so shaped that when hung on the condenser the
method was developed in cooperation with the American Leather Chemists Assn.
cup hangs with its rim reasonably level. In this procedure, the
(Method H 23–1957).
thimble basket is suspended either as shown in Fig. 1a by
Current edition approved May 15, 1995. Published July 1995. Originally
published as D 5439 – 93. Last previous edition D 5439 – 93.
meansofthecorrosion-resistantwireloopedoverthebottomof
Annual Book of ASTM Standards, Vol 05.01.
the condenser coil and attached to the basket supports or as in
Annual Book of ASTM Standards, Vol 05.02.
Fig. 1b where the wire supports of the basket are attached to
Available from American National Standards Institute, 11 West 42nd St., 13th
Floor, New York, NY 10036. hooks soldered to the underside of the condenser lid.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D5439
NOTE 1—Silver solder should be used on all joints.
FIG. 2 Basket Thimble Support
A
Recorded boiling point 110.6°C.
4.1.6 SourceofHeat,asourceofheat,preferablyahotplate,
suitable for vaporizing toluene.
6. Sampling
5. Solvent
6.1 Sampling is defined as all steps required to obtain an
aliquot of the contents of any pipe, tank, or other system and to
5.1 Toluene, conforming to ISO 5257, Grade 2.
place the sample into the laboratory test container.
(Warning—Flammable.)
6.2 Only representative samples obtained as specified in
5.1.1 The typical characteristics for the reagent are:
PracticesD 4057andD 4177shallbeusedforthistestmethod.
Color (APHA) 10
A
Boiling range (initial to dry point) 2.0°C
Residue after evaporation 0.001 % 7. Procedure
Substances darkened by H SO passes ACS test
2 4
7.1 For referee tests, use a new extraction thimble. For
Sulfur compounds (as S) 0.003 %
Water (H O) (by Karl Fischer titration) 0.03 % routine tests, thimbles may be reused. Before reusing a
_______________
thimble, it must be heated to a dull red heat (preferably in an
D5439
electric furnace) to remove the combustible portion of the 9. Report
accumulated sediment. Subject the thimble to a preliminary
9.1 Report the results to the nearest 0.01 % as the mass
extraction as described in 7.2 befor
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