ASTM D473-02(2006)
(Test Method)Standard Test Method for Sediment in Crude Oils and Fuel Oils by the Extraction Method
Standard Test Method for Sediment in Crude Oils and Fuel Oils by the Extraction Method
SCOPE
1.1 This test method covers the determination of sediment in crude oils and fuel oils by extraction with toluene. The precision applies to a range of sediment levels from 0.01 to 0.40 % mass, although higher levels may be determined. Note 1Precision on recycled oils and crank case oils is unknown and additional testing is required to determine that precision.
1.2 &si-value;
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. For specific precautionary statements, see 6.1.
General Information
Relations
Standards Content (Sample)
NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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
An American National Standard
Designation:D473–02 (Reapproved 2006)
Designation: Manual of Petroleum Measurement Standards (MPMS), Chapter 10.1
Designation: 53/82
Standard Test Method for
Sediment in Crude Oils and Fuel Oils by the Extraction
Method
This standard is issued under the fixed designation D 473; 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.
This standard has been approved for use by agencies of the Department of Defense.
1. Scope 2.2 API Standards:
Chapter 8.1 Manual Sampling of Petroleum and Petroleum
1.1 This test method covers the determination of sediment
Products (ASTM Practice D 4057)
in crude oils and fuel oils by extraction with toluene. The
Chapter 8.2 Automatic Sampling of Petroleum and Petro-
precision applies to a range of sediment levels from 0.01 to
leum Products (ASTM Practice D 4177)
0.40 % mass, although higher levels may be determined.
Chapter 8.3 Mixing and Handling of Liquid Samples of
NOTE 1—Precision on recycled oils and crank case oils is unknown and
Petroleum and Petroleum Products (ASTM Practice
additional testing is required to determine that precision.
D 5854)
1.2 The values stated in SI units are to be regarded as the
2.3 ISO Standard:
standard. The values given in parentheses are for information
5272 Toluene for industrial use—Specifications
only.
3. Summary of Test Method
1.3 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the
3.1 Extract test portion of a representative oil sample,
responsibility of the user of this standard to establish appro-
contained in a refractory thimble, with hot toluene until the
priate safety and health practices and determine the applica-
residue reaches constant mass. The mass of residue, calculated
bility of regulatory limitations prior to use. For specific
as a percentage, is reported as sediment by extraction.
precautionary statements, see 6.1.
4. Significance and Use
2. Referenced Documents
4.1 A knowledge of the sediment content of crude oils and
2.1 ASTM Standards:
fuel oils is important both to the operation of refining and the
D 4057 Practice for Manual Sampling of Petroleum and
buying or selling of these commodities.
Petroleum Products
5. Apparatus
D 4177 Practice for Automatic Sampling of Petroleum and
Petroleum Products 5.1 Usual laboratory apparatus and glassware, together with
D 5854 Practice for Mixing and Handling of Liquid
the following are required for this test method.
Samples of Petroleum and Petroleum Products 5.1.1 Extraction Apparatus—Use the apparatus illustrated
in Figs. 1 and 2 and consisting of the elements described in
5.1.1.1-5.1.1.3.
This test method is under the jurisdiction of ASTM Committee D02 on
5.1.1.1 Extraction Flask—Use a wide-neck (Erlenmeyer)
Petroleum Products and Lubricants and theAPI Committee on Petroleum Measure-
flask of 1-L capacity, with a minimum external neck diameter
ment, and is the direct responsibility of Subcommittee D02.02.0B /COMQ, the joint
ASTM-API Committee on Sampling, Sediment, Water. of 50 mm, for the procedure.
Current edition approved Nov. 1, 2006. Published December 2006. Originally
approved in 1938. Last previous edition approved in 2002 as D 473 – 02.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Available from American Petroleum Institute (API), 1220 L. St., NW, Wash-
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
ington, DC 20005-4070, http://api-ec.api.org.
Standards volume information, refer to the standard’s Document Summary page on
Available fromAmerican National Standards Institute (ANSI), 25 W. 43rd St.,
the ASTM website.
4th Floor, New York, NY 10036, http://www.ansi.org.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D473–02 (2006)
NOTE—Apparatus B shows the water cup in position.
FIG. 1 Extraction Apparatus for Determination of Sediment
5.1.1.2 Condenser—Acondenser in the form of a metal coil 5.1.1.5 Water Cup—Use a water cup when testing a sample
approximately 25 mm in diameter and 50 mm in length determined to have a water content greater than 10 % volume
attached to, and with the ends projecting through, a lid of (see Fig. 1, Apparatus B). The cup shall be made of glass,
sufficient diameter to cover the neck of the flask as shown in
conicalinshape,approximately20mmindiameterand25mm
Fig. 1. The coil shall be made from stainless steel, tin, deep,andhaveacapacityofapproximately3mL.Aglasshook
tin-plated copper, or tin-plated brass tubing having an outside
fused on the rim at one side is so shaped that when hung on the
diameter of 5 to 8 mm and a wall thickness of 1.5 mm. If condenser the cup hangs with its rim reasonably level. In this
constructed of tin-plated copper or brass, the tin coating shall
procedure, suspend the thimble basket as shown in Fig. 1,
have a minimum thickness of 0.075 mm. The exposed surface Apparatus A by means of the corrosion-resistant wire looped
of the coil for cooling purposes is about 115 cm .
overthebottomofthecondensercoilandattachedtothebasket
5.1.1.3 Extraction Thimble —The extraction thimble shall
supports, or as in Fig. 1,Apparatus B, where the wire supports
beofarefractoryporousmaterial,poresize20.0to30.0µm(as
of the basket are attached to hooks soldered to the underside of
certifiedbythemanufacturer),25mmindiameterby70mmin
the condenser lid.
height, weighing not less than 15 g and not more than 17 g.
5.1.1.6 Source of Heat—Use a source of heat, preferably a
Suspend the thimble from the condenser coil by means of a
hot plate operated under a ventilated hood, suitable for vapor-
basket so that it hangs approximately midway between the
izing toluene (Warning—Flammable.)
surface of the extracting solvent and the bottom of the
5.2 Analytical Balance—Use an analytical balance, with an
condenser coil.
accuracy of 0.1 mg. Verify the balance, at least annually,
5.1.1.4 Thimble Basket—The thimble basket shall be
against weights traceable to a national standards body such as
corrosion-resistant, shall be made of platinum, stainless steel,
the National Institute of Standards and Technology (NIST).
nickel-chromium alloy, or similar material, and shall meet the
5.3 Non-aerating Mixer—Use a non-aerating mixer, meet-
design and dimension requirements in Fig. 2.
ing the verification of mixing efficiency requirements specified
in Practice D 5854 (API Chapter 8.3). Either insertion mixers
5 or circulating mixers or circulating external mixers are accept-
The sole source of supply of the extraction thimble, AN 485, 25 3 70-mm,
coarse porosity, drawing number QA 005163, known to the committee at this time able provided they meet the criteria in Practice D 5854 (API
is Saint-Gobain/Norton Industrial Ceramics Corporation of Worcester, MA. If you
Chapter 8.3).
are aware of alternative suppliers, please provide this information to ASTM
5.4 Oven—Use an oven capable of maintaining a tempera-
International Headquarters. Your comments will receive careful consideration at a
meeting of the responsible technical committee, which you may attend. ture of 115 to 120°C (240 to 250°F).
D473–02 (2006)
FIG. 2 Basket Thimble Support
5.5 Cooling Vessel—Use a desiccator without desiccant as a eyes.Keepthecontainerclosed.Usewithadequateventilation.
cooling vessel. Avoid prolonged or repeated contact with the skin.)
5.6 Thermometer—Use a thermometer capable of measur- 6.1.1 The typical characteristics for the ACS reagent are
ing the temperature of the sample to the nearest 1°C (2°F). shown in Table 1.
6. Solvent
7. Sampling
6.1 Toluene—Reagent grade conforming to the specifica-
7.1 Sampling shall include all steps required to obtain an
tionsoftheCommitteeonAnalyticalReagentsoftheAmerican
aliquot of the contents of any pipe, tank, or other system and to
Chemical Society (ACS) or to Grade 2 of ISO 5272.
place the sample into the laboratory test container.
(Warning—Flammable. Keep away from heat, sparks and
open flame. Vapor harmful. Toluene is toxic. Particular care
TABLE 1 Typical Characteristics for ACS Reagent Grade Toluene
shall be taken to avoid breathing the vapors and to protect the
Assay 99.5+ %
Color (APHA) 10
A
Boiling range (initial to dry point) 2.0°C
Reagent Chemicals, American Chemical Society Specifications , American
Residue after evaporation 0.001 %
Chemical Society, Washington, DC. For suggestions on the testing of reagents not
Substances darkened by H SO passes test
2 4
listed by the American Chemical Society, see Analar Standards for Laboratory
Sulfur compounds (as S) 0.003 %
Chemicals,BDHLtd.,Poole,Dorset,U.K.,andtheUnitedStatesPharmacopeiaand
Water (H O) (by Karl Fischer titration) 0.03 %
National Formulary, U.S. Pharmacopeial Convention, Inc., (USPC), Rockville, MD
A
20852. Recorded boiling point 110.6°C.
D473–02 (2006)
7.2 Only use representative samples obtained as
...
Questions, Comments and Discussion
Ask us and Technical Secretary will try to provide an answer. You can facilitate discussion about the standard in here.