ASTM D5439-95

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Designation: D 5439 – 95
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 Fig. 1. The coil should be made from stainless steel, tin,
Oils by the Extraction Method
tin-plated copper, or tin-plated brass tubing having an outside
D 4057 Practice for Manual Sampling of Petroleum and
3 diameter of 5 to 8 mm and a wall thickness of 1.5 mm. If
Petroleum Products
constructed of tin-plated copper or brass, the tin coating shall
D 4177 Practice for Automatic Sampling of Petroleum and
3 have a minimum thickness of 0.075 mm. The exposed surface
Petroleum Products
of the coil for cooling purposes is about 115 cm .
2.2 ISO Standard:
4 4.1.3 Extraction Thimble—The extraction thimble should
5272 Toluene-Specifications
be of a refractory porous material, pore size index P15, 25 mm
3. Significance and Use in diameter by 70 mm in height, weighing not less than 15 g
and not more than 17 g. The thimble shall be suspended from
3.1 This test method is intended for use in determining the
the condenser coil by means of a basket so that it hangs
toluene insoluble sediment contained in Moellon.
approximately midway between the surface of the extracting
4. Apparatus solvent and the bottom of the condenser coil.
4.1.4 Thimble Basket—The thimble basket shall be
4.1 Extraction Apparatus (see Fig. 1 and Fig. 2), consisting
corrosion-resistant, shall be made of platinum, stainless steel,
of the parts described in 4.1.1-4.1.6.
nickel-chromium alloy, or similar material, and shall meet the
4.1.1 Extraction Flask, a wide-neck Erlenmeyer flask of 1-L
requirements of Fig. 2.
capacity.
4.1.5 Water Cup—A water cup shall be used when testing a
4.1.2 Condenser, a condenser in the form of a metal coil
sample having a high-water content (see Fig. 1b). The cup shall
approximately 25 mm in diameter and 50 mm in length
be made of glass, shall be conical in shape, shall be approxi-
attached to, and with the ends projecting through a lid of
mately 20 mm in diameter and 25 mm deep, and shall have a
sufficient diameter to cover the neck of the flask as shown in
capacity of approximately 3 mL. A glass hook fused on the rim
at one side is so shaped that when hung on the condenser the
This test method is under the jurisdiction of ASTM Committee D-31 on Leather
cup hangs with its rim reasonably level. In this procedure, the
and is the direct responsibility of Subcommittee D31.08 on Fats and Oils. This test
thimble basket is suspended either as shown in Fig. 1a by
method was developed in cooperation with the American Leather Chemists Assn.
means of the corrosion-resistant wire looped over the bottom of
(Method H 23–1957).
the condenser coil and attached to the basket supports or as in
Current edition approved May 15, 1995. Published July 1995. Originally
published as D 5439 – 93. Last previous edition D 5439 – 93.
Fig. 1b where the wire supports of the basket are attached to
Annual Book of ASTM Standards, Vol 05.01.
hooks soldered to the underside of the condenser lid.
Annual Book of ASTM Standards, Vol 05.02.
4.1.6 Source of Heat, a source of heat, preferably a hot plate,
Available from American National Standards Institute, 11 West 42nd St., 13th
Floor, New York, NY 10036. suitable for vaporizing toluene.
Copyright © ASTM, 100 Barr Harbor Drive, West Conshohocken, PA 19428-2959, United States.
D 5439
NOTE 1—Silver solder should be used on all joints.
FIG. 2 Basket Thimble Support
5. Solvent 6.2 Only representative samples obtained as specified in
Practices D 4057 and D 4177 shall be used for this test method.
5.1 Toluene, conforming to ISO 5257, Grade 2.
7. Procedure
NOTE 1—Warning: Flammable.
7.1 For referee tests, use a new extraction thimble. For
5.1.1 The typical characteristics for the reagent are:
routine tests, thimbles may be reused. Before reusing a
Color (APHA) 10
A
thimble, it must be heated to a dull red heat (preferably in an
Boiling range (initial to dry point) 2.0°C
Residue after evaporation 0.001 %
electric furnace) to remove the combustible portion of the
Substances darkened by H SO passes ACS test
2 4
accumulated sediment. Subject the thimble to a preliminary
Sulfur compounds (as S) 0.003 %
extraction as described in 7.2 before being used for another
Water (H O) (by Karl Fischer titration) 0.03 %
_______________
determination.
A
Recorded boiling point 110.6°C.
7.2 Before using a new thimble, rub the outside surface with
fine sandpaper and remove all loosened material with a stiff
6. Sampling
brush. Give the thimble a preliminary extraction with the
6.1 Sampling is defined as all steps required to obtain an toluene, allowing the solvent to drip from the thimble for
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