Standard Test Method for Determination of Sediment in Moellon

SIGNIFICANCE AND USE
This test method is intended for use in determining the toluene insoluble sediment contained 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 standard. No other units of measurement are included in this 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.

General Information

Status
Historical
Publication Date
31-Mar-2012
Technical Committee
Drafting Committee
Current Stage
Ref Project

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ASTM D5439-95(2012) - Standard Test Method for Determination of Sediment in Moellon
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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
Designation: D5439 − 95 (Reapproved 2012)
Standard Test Method for
Determination of Sediment in Moellon
This standard is issued under the fixed designation D5439; 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 4.1.1 ExtractionFlask,awide-neckErlenmeyerflaskof1-L
capacity.
1.1 This test method covers the determination of the toluene
4.1.2 Condenser, a condenser in the form of a metal coil
insolublesedimentcontainedinMoellon.Thistestmethodwas
approximately 25 mm in diameter and 50 mm in length
derived from Test Method D473.
attached to, and with the ends projecting through a lid of
1.2 The values stated in SI units are to be regarded as
sufficient diameter to cover the neck of the flask as shown in
standard. No other units of measurement are included in this
Fig. 1. The coil should be made from stainless steel, tin,
standard.
tin-plated copper, or tin-plated brass tubing having an outside
1.3 This standard does not purport to address all of the
diameter of 5 to 8 mm and a wall thickness of 1.5 mm. If
safety concerns, if any, associated with its use. It is the
constructed of tin-plated copper or brass, the tin coating shall
responsibility of the user of this standard to establish appro-
have a minimum thickness of 0.075 mm. The exposed surface
priate safety and health practices and determine the applica-
of the coil for cooling purposes is about 115 cm .
bility of regulatory limitations prior to use.
4.1.3 ExtractionThimble—Theextractionthimbleshouldbe
2. Referenced Documents of a refractory porous material, pore size index P15, 25 mm in
2 diameter by 70 mm in height, weighing not less than 15 g and
2.1 ASTM Standards:
not more than 17 g. The thimble shall be suspended from the
D473 Test Method for Sediment in Crude Oils and Fuel Oils
condenser coil by means of a basket so that it hangs approxi-
by the Extraction Method
mately midway between the surface of the extracting solvent
D4057 Practice for Manual Sampling of Petroleum and
and the bottom of the condenser coil.
Petroleum Products
D4177 Practice for Automatic Sampling of Petroleum and 4.1.4 Thimble Basket—The thimble basket shall be
corrosion-resistant, shall be made of platinum, stainless steel,
Petroleum Products
nickel-chromium alloy, or similar material, and shall meet the
2.2 ISO Standard:
requirements of Fig. 2.
ISO 5272 Toluene for Industrial Use - Specifications
4.1.5 Water Cup—Awater cup shall be used when testing a
3. Significance and Use
samplehavingahigh-watercontent(seeFig.1b).Thecupshall
3.1 This test method is intended for use in determining the
be made of glass, shall be conical in shape, shall be approxi-
toluene insoluble sediment contained in Moellon.
mately 20 mm in diameter and 25 mm deep, and shall have a
capacity of approximately 3 mL.Aglass hook fused on the rim
4. Apparatus
at one side is so shaped that when hung on the condenser the
4.1 Extraction Apparatus (see Fig. 1 and Fig. 2), consisting
cup hangs with its rim reasonably level. In this procedure, the
of the parts described in 4.1.1 – 4.1.6.
thimble basket is suspended either as shown in Fig. 1aby
meansofthecorrosion-resistantwireloopedoverthebottomof
the condenser coil and attached to the basket supports or as in
This test method is under the jurisdiction ofASTM Committee D31 on Leather
Fig. 1b where the wire supports of the basket are attached to
and is the direct responsibility of Subcommittee D31.08 on Fats and Oils. This test
method was developed in cooperation with the American Leather Chemists Assn. hooks soldered to the underside of the condenser lid.
(Method H 23–1957).
4.1.6 SourceofHeat,asourceofheat,preferablyahotplate,
Current edition approved April 1, 2012. Published April 2012. Originally
suitable for vaporizing toluene.
approved in 1993. Last previous edition approved in 2006 as D5439 – 95(2006).
DOI: 10.1520/D5439-95R12.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
5. Solvent
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Standards volume information, refer to the standard’s Document Summary page on
5.1 Toluene, conforming to ISO 5272, Grade 2.
the ASTM website.
(Warning—Flammable.)
Available from American National Standards Institute, 11 West 42nd St., 13th
Floor, New York, NY 10036. 5.1.1 The typical characteristics for the reagent are:
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D5439 − 95 (2012)
7.4 When testing samples having a high water content, use
the assembly shown in Fig. 1b. In this procedure, any water in
the test portion is removed as its toluene azeotrope and is
collected in the water cup, where it separates as a bottom layer.
The toluene layer overflows into the thimble. If the cup
becomes full of water, allow the apparatus to cool and empty
the cup.
7.5 After the extraction is completed, dry the thimble for 1
h at 115 to 120°C; cool in a desiccator, without desiccant, for
1 h and weigh to the nearest 0.2 mg.
7.6 Repeat the extraction, allowing the solvent to drip from
NOTE 1—Apparatus B shows the water cup in position.
thethimbleforatleast1hbutnotlongerthan1.25h;dry,cool,
FIG. 1 Extraction Apparatus for Determination of Sediment
and weigh the thimble as described in 7.5. Repeat this
extraction for further 1-h periods, if necessary, until the masses
of the dried thimble plus sediment, after two successive
extractions, do not differ by more than 0.2 mg.
Color (APHA) 10
A
Boiling range (initial to dry point) 2.0°C
Residue after evaporation 0.001 %
8. Calculation
Substances darkened by H SO passes ACS test
2 4
Sulfur compounds (as S) 0.003 % 8.1 Calculate the mass
...

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