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ASTM D473-07(2012)

(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

SIGNIFICANCE AND USE
4.1 A knowledge of the sediment content of crude oils and fuel oils is important both to the operation of refining and the buying or selling of these commodities.
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 1—Precision on recycled oils and crankcase oils is unknown and additional testing is required to determine that precision.  
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. For specific warning statements, see 5.1.1.6 and 6.1.

General Information

Status
Historical
Publication Date
31-Oct-2012
ICS
75.040 - Crude petroleum
75.160.20 - Liquid fuels
Technical Committee
D02 - Petroleum Products, Liquid Fuels, and Lubricants
Drafting Committee
D02.02 - Hydrocarbon Measurement for Custody Transfer (Joint ASTM-API)
Current Stage
Ref Project

Relations

Replaces
ASTM D473-07 - Standard Test Method for Sediment in Crude Oils and Fuel Oils by the Extraction Method
Effective Date
01-Nov-2012
Replaced By
ASTM D473-07(2012)e1 - Standard Test Method for Sediment in Crude Oils and Fuel Oils by the Extraction Method
Effective Date
01-Nov-2012
Referred By
ASTM D396-21 - Standard Specification for Fuel Oils
Effective Date
01-Nov-2012
Referred By
ASTM D128-98(2019) - Standard Test Methods for Analysis of Lubricating Grease
Effective Date
01-Nov-2012
Referred By
ASTM D7666-12(2019) - Standard Specification for Triglyceride Burner Fuel
Effective Date
01-Nov-2012
Referred By
ASTM D5439-95(2019) - Standard Test Method for Determination of Sediment in Moellon
Effective Date
01-Nov-2012
Referred By
ASTM D4807-05(2020) - Standard Test Method for Sediment in Crude Oil by Membrane Filtration
Effective Date
01-Nov-2012
Referred By
ASTM D6823-08(2021) - Standard Specification for Commercial Boiler Fuels With Used Lubricating Oils
Effective Date
01-Nov-2012
Referred By
ASTM D6448-16(2022) - Standard Specification for Industrial Burner Fuels from Used Lubricating Oils
Effective Date
01-Nov-2012
Referred By
ASTM G205-16 - Standard Guide for Determining Emulsion Properties, Wetting Behavior, and Corrosion-Inhibitory Properties of Crude Oils
Effective Date
01-Nov-2012

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ASTM D473-07(2012) - Standard Test Method for Sediment in Crude Oils and Fuel Oils by the Extraction MethodASTM D473-07(2012) - Standard Test Method for Sediment in Crude Oils and Fuel Oils by the Extraction Method
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ASTM D473-07(2012) - Standard Test Method for Sediment in Crude Oils and Fuel Oils by the Extraction Method
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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
Designation: D473 − 07(Reapproved 2012)
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
1
Method
This standard is issued under the fixed designation D473; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision.Anumber in parentheses indicates the year of last reapproval.A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
This standard has been approved for use by agencies of the U.S. Department of Defense.
1. Scope E29Practice for Using Significant Digits in Test Data to
Determine Conformance with Specifications
1.1 This test method covers the determination of sediment
3
2.2 API Standards:
in crude oils and fuel oils by extraction with toluene. The
precision applies to a range of sediment levels from 0.01 to Chapter 8.1Manual Sampling of Petroleum and Petroleum
Products (ASTM Practice D4057)
0.40% mass, although higher levels may be determined.
Chapter 8.2Automatic Sampling of Petroleum and Petro-
NOTE 1—Precision on recycled oils and crankcase oils is unknown and
leum Products (ASTM Practice D4177)
additional testing is required to determine that precision.
Chapter 8.3Mixing and Handling of Liquid Samples of
1.2 The values stated in SI units are to be regarded as
Petroleum and Petroleum Products (ASTM Practice
standard. No other units of measurement are included in this
D5854)
standard.
4
2.3 ISO Standard:
1.3 This standard does not purport to address all of the
5272 Toluene for industrial use—Specifications
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro-
3. Summary of Test Method
priate safety and health practices and determine the applica-
3.1 Extract test portion of a representative oil sample,
bility of regulatory limitations prior to use. For specific
contained in a refractory thimble, with hot toluene until the
warning statements, see 5.1.1.6 and 6.1.
residue reaches constant mass.The mass of residue, calculated
2. Referenced Documents
as a percentage, is reported as sediment by extraction.
2
2.1 ASTM Standards:
4. Significance and Use
D4057Practice for Manual Sampling of Petroleum and
Petroleum Products (API MPMS Chapter 8.1)
4.1 A knowledge of the sediment content of crude oils and
D4177Practice for Automatic Sampling of Petroleum and
fuel oils is important both to the operation of refining and the
Petroleum Products (API MPMS Chapter 8.2)
buying or selling of these commodities.
D5854Practice for Mixing and Handling of Liquid Samples
of Petroleum and Petroleum Products (API MPMS Chap-
5. Apparatus
ter 8.3)
5.1 Usuallaboratoryapparatusandglassware,togetherwith
the following are required for this test method.
1
This test method is under the jurisdiction of ASTM Committee D02 on
5.1.1 Extraction Apparatus—Usetheapparatusillustratedin
Petroleum Products, Liquid Fuels, and Lubricants and the API Committee on
Figs. 1 and 2 and consisting of the elements described in
Petroleum Measurement, and is the direct responsibility of Subcommittee D02.02
5.1.1.1 – 5.1.1.3.
/COMQ on Hydrocarbon Measurement for Custody Transfer (Joint ASTM-API).
Current edition approved Nov. 1, 2012. Published December 2012. Originally
approved in 1938. Last previous edition approved in 2007 as D473–07. DOI:
10.1520/D0473-07R12.
2 3
For referenced ASTM standards, visit the ASTM website, www.astm.org, or Available from American Petroleum Institute (API), 1220 L. St., NW,
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM Washington, DC 20005-4070, http://api-ec.api.org.
4
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
1

---------------------- Page: 1 ----------------------
D473 − 07 (2012)
NOTE 1—Apparatus B shows the water cup in position.
FIG. 1 Extraction Apparatus for Determination of Sediment
5.1.1.1 Extraction Flask—Use a wide-neck (Erlenmeyer) basket so that it hangs approximately midway between the
flask of 1-L capacity, with a minimum external neck diameter surface of the extracting solvent and the bottom of the
of 50 mm, for the procedure.
condenser coil.
5.1.1.2 Condenser—Acondenser in the form of a metal coil
5.1.1.4 Thimble Basket—The thimble basket shall be
approximately 25 mm in diameter and 50 mm in length
corrosion-resistant and shall be made of platinum, stainless
attached to, and with the ends projecting through, a lid of
steel, nic
...

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5.1 This test method provides a rapid and precise elemental measurement with simple sample preparation. Typical analysis times are approximately 4 min to 5 min per sample with a preparation time of approximately 1 min to 3 min per sample.  
5.2 The quality of crude oil is related to the amount of sulfur present. Knowledge of the vanadium and nickel concentration is necessary for processing purposes as well as contractual agreements.  
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5.1 A knowledge of the sediment content of crude oils and fuel oils is important both to the operation of refining and the buying or selling of these commodities.
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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.
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5.1 Accurate elemental analysis of petroleum products and lubricants is necessary for the determination of chemical properties, which are used to establish compliance with commercial and regulatory specifications.  
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5.1 Accurate elemental analysis of petroleum products and lubricants is necessary for the determination of chemical properties, which are used to establish compliance with commercial and regulatory specifications.  
5.2 Atomic Absorption Spectrometry (AAS) is one of the most widely used analytical techniques in the oil industry for elemental analysis. There are at least twelve Standard Test Methods published by ASTM D02 Committee on Petroleum Products and Lubricants for such analysis. See Table 1.  
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Standard Test Methods for Determination of Nickel, Vanadium, and Iron in Crude Oils and Residual Fuels by Inductively Coupled Plasma (ICP) Atomic Emission Spectrometry

SIGNIFICANCE AND USE
4.1 These test methods cover, in single procedures, the determination of Ni, V, and Fe in crude oils and residual oils. These test methods complement Test Method D1548, which covers only the determination of vanadium.  
4.2 When fuels are combusted, vanadium present in the fuel can form corrosive compounds. The value of crude oils can be determined, in part, by the concentrations of nickel, vanadium, and iron. Nickel and vanadium, present at trace levels in petroleum fractions, can deactivate catalysts during processing. These test methods provide a means of determining the concentrations of nickel, vanadium, and iron.
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1.1 These test methods cover the determination of nickel, vanadium, and iron in crude oils and residual fuels by inductively coupled plasma (ICP) atomic emission spectrometry. Two different test methods are presented.  
1.2 Test Method A (Sections 7 – 11 and 18 – 22)—ICP is used to analyze a sample dissolved in an organic solvent. This test method uses oil-soluble metals for calibration and does not purport to quantitatively determine or detect insoluble particulates.  
1.3 Test Method B (Sections 12 – 22)—ICP is used to analyze a sample that is decomposed with acid.  
1.4 The concentration ranges covered by these test methods are determined by the sensitivity of the instruments, the amount of sample taken for analysis, and the dilution volume. A specific statement is given in 15.2. Typically, the low concentration limits are a few tenths of a milligram per kilogram. Precision data are provided for the concentration ranges specified in Section 21.  
1.5 The values stated in SI units are to be regarded as standard.  
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1.6 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, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
1.7 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

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1.1 This specification2 covers hot- and cold-worked precipitation-hardenable nickel alloy rod, bar, forgings, and forging stock for moderate or high temperature service (Table 1).  
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1.4 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

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