ASTM D473-07(2012)e1
(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.
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´1
Designation: D473 − 07 (Reapproved 2012)
Manual of Petroleum Measurement Standards (MPMS), Chapter 10.1
Standard Test Method for
Sediment in Crude Oils and Fuel Oils by the Extraction
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.
ε NOTE—IP information was removed editorially in March 2016.
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
2.2 API Standards:
in crude oils and fuel oils by extraction with toluene. The
Chapter 8.1Manual Sampling of Petroleum and Petroleum
precision applies to a range of sediment levels from 0.01 to
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.
2.3 ISO Standard:
5272 Toluene for industrial use—Specifications
1.3 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the
3. Summary of Test Method
responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica- 3.1 Extract test portion of a representative oil sample,
contained in a refractory thimble, with hot toluene until the
bility of regulatory limitations prior to use. For specific
warning statements, see 5.1.1.6 and 6.1. residue reaches constant mass.The mass of residue, calculated
as a percentage, is reported as sediment by extraction.
2. Referenced Documents
4. Significance and Use
2.1 ASTM Standards:
4.1 A knowledge of the sediment content of crude oils and
D4057Practice for Manual Sampling of Petroleum and
fuel oils is important both to the operation of refining and the
Petroleum Products (API MPMS Chapter 8.1)
buying or selling of these commodities.
D4177Practice for Automatic Sampling of Petroleum and
Petroleum Products (API MPMS Chapter 8.2)
5. Apparatus
D5854Practice for Mixing and Handling of Liquid Samples
5.1 Usuallaboratoryapparatusandglassware,togetherwith
of Petroleum and Petroleum Products (API MPMS Chap-
the following are required for this test method.
ter 8.3)
5.1.1 Extraction Apparatus—Usetheapparatusillustratedin
Figs. 1 and 2 and consisting of the elements described in
This test method is under the jurisdiction of ASTM Committee D02 on
5.1.1.1 – 5.1.1.3.
Petroleum Products, Liquid Fuels, and Lubricants and the API Committee on
5.1.1.1 Extraction Flask—Use a wide-neck (Erlenmeyer)
Petroleum Measurement, and is the direct responsibility of Subcommittee D02.02
flask of 1-L capacity, with a minimum external neck diameter
/COMQ on Hydrocarbon Measurement for Custody Transfer (Joint ASTM-API).
Current edition approved Nov. 1, 2012. Published December 2012. Originally of 50 mm, for the procedure.
approved in 1938. Last previous edition approved in 2007 as D473–07. DOI:
10.1520/D0473-07R12E01.
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.
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.
© Jointly copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, USA and the American Petroleum Institute (API), 1220 L Street NW, Washington DC 20005, USA
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D473 − 07 (2012)
NOTE 1—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 5.1.1.4 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, nickel-chromium alloy, or similar material. Fig. 2 shows
sufficient diameter to cover the neck of the flask as shown in the design and dimensions of two typical baskets that have
Fig. 1. The coil shall be made from stainless steel, tin, been used successfully in the industry.
tin-plated copper, or tin-plated brass tubing having an outside
5.1.1.5 Water Cup—Use a water cup when testing a sample
diameter of 5 to 8 mm and a wall thickness of 1.5 mm. If
determined to have a water content greater than 10% volume
constructed of tin-plated copper or brass, the tin coating shall
(see Fig. 1, Apparatus B). The cup shall be made of glass,
have a minimum thickness of 0.075 mm. The exposed surface
conicalinshape,approximately20mmindiameterand25mm
of the coil for cooling purposes is about 115 cm .
deep,andhaveacapacityofapproximately3mL.Aglasshook
fusedontherimatonesideissoshapedthatwhenhungonthe
NOTE 2—The use of a water flowmeter/controller unit that monitors
condenser the cup hangs with its rim reasonably level. In this
water flow to the condenser that shuts off the heat source when the flow
rate drops below a pre-set limit has been found suitable to prevent
procedure, suspend the thimble basket as shown in Fig. 1,
vaporized toluene from igniting. The use of such a device is recom-
Apparatus A by means of the corrosion-resistant wire looped
mended.
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
ofthebasketareattachedtohookssolderedtotheundersideof
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,
against weights traceable to a national standards body such as
The sole source of supply of the extraction thimble, AN 485, 25 × 70-mm,
the National Institute of Standards and Technology (NIST).
coarse porosity, drawing number QA005163, known to the committee at this time
is Saint-Gobain/Norton Industrial Ceramics Corporation of Worcester, MA. If you
5.3 Non-aerating Mixer—Use a non-aerating mixer, meet-
are aware of alternative suppliers, please provide this information to ASTM
ingtheverificationofmixingefficiencyrequirementsspecified
International Headquarters. Your comments will receive careful consideration at a
meeting of the responsible technical committee, which you may attend. inPracticeD5854(APIChapter8.3).Eitherinsertionmixersor
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D473 − 07 (2012)
FIG. 2 Basket Thimble Support
circulatingmixersorcirculatingexternalmixersareacceptable Chemical Society (ACS) or to Grade 2 of ISO 5272.
providedtheymeetthecriteriainPracticeD5854(APIChapter (Warning—Flammable. Keep away from heat, sparks and
8.3). open flame. Vapor harmful. Toluene is toxic. Particular care
shall be taken to avoid breathing the vapors and to protect the
5.4 Oven—Use an oven capable of maintaining a tempera-
eyes.Keepthecontainerclosed.Usewithadequateventilation.
ture of 115 to 120°C (240 to 250°F).
Avoid prolonged or repeated contact with the skin.)
5.5 Cooling Vessel—Useadesiccatorwithoutdesiccantasa
6.1.1 The typical characteristics for the ACS reagent are
cooling vessel.
shown in Table 1.
5.6 Temperature Measuring Device—Such as a
thermometer, capable of measuring the temperature of the
Reagent Chemicals, American Chemical Society Specifications , American
sample to the nearest 1°C (2°F).
Chemical Society, Washington, DC. For suggestions on the testing of reagents not
listed by the American Chemical Society, see Analar Standards for Laboratory
6. Solvent
Chemicals,BDHLtd.,Poole,Dorset,U.K.,andtheUnitedStatesPharmacopeiaand
6.1 Toluene—Reagent grade conforming to the specifica-
National Formulary, U.S. Pharmacopeial Convention, Inc., (USPC), Rockville, MD
tionsoftheCommitteeonAnalyticalReagentsoftheAmerican 20852.
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D473 − 07 (2012)
TABLE 1 Typical Characteristics for ACS Reagent Grade Toluene
portion of the accumulated sediment.Avoid excessive reuse of
Assay 99.5+ % thimbles, as over time the pores become clogged with inor-
Color (APHA) 10
ganic material resulting in falsely high results. When in doubt
A
Boiling range (initial to dry point) 2.0°C
regarding a higher than normal result, discard the thimble and
Residue after evaporation 0.001 %
Substances darkened by H SO passes test r
...
This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
´1
Designation: D473 − 07 (Reapproved 2012) 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
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. A number 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.
ε NOTE—IP information was removed editorially in March 2016.
1. 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.
2. Referenced Documents
2.1 ASTM Standards:
D4057 Practice for Manual Sampling of Petroleum and Petroleum Products (API MPMS Chapter 8.1)
D4177 Practice for Automatic Sampling of Petroleum and Petroleum Products (API MPMS Chapter 8.2)
D5854 Practice for Mixing and Handling of Liquid Samples of Petroleum and Petroleum Products (API MPMS Chapter 8.3)
E29 Practice for Using Significant Digits in Test Data to Determine Conformance with Specifications
2.2 API Standards:
Chapter 8.1 Manual Sampling of Petroleum and Petroleum Products (ASTM Practice D4057)
Chapter 8.2 Automatic Sampling of Petroleum and Petroleum Products (ASTM Practice D4177)
Chapter 8.3 Mixing and Handling of Liquid Samples of Petroleum and Petroleum Products (ASTM Practice D5854)
2.3 ISO Standard:
5272 Toluene for industrial use—Specifications
3. Summary of Test Method
3.1 Extract test portion of a representative oil sample, contained in a refractory thimble, with hot toluene until the residue
reaches constant mass. The mass of residue, calculated as a percentage, is reported as sediment by extraction.
This test method is under the jurisdiction of ASTM Committee D02 on Petroleum Products, Liquid Fuels, and Lubricants and the API Committee on Petroleum
Measurement, and is the direct responsibility of Subcommittee D02.02 /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/D0473-07R12.10.1520/D0473-07R12E01.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or 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 the ASTM website.
Available from American Petroleum Institute (API), 1220 L. St., NW, Washington, DC 20005-4070, http://api-ec.api.org.
Available from American National Standards Institute (ANSI), 25 W. 43rd St., 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
D473 − 07 (2012)
NOTE 1—Apparatus B shows the water cup in position.
FIG. 1 Extraction Apparatus for Determination of Sediment
4. 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.
5. Apparatus
5.1 Usual laboratory apparatus and glassware, together with the following are required for this test method.
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.
5.1.1.1 Extraction Flask—Use a wide-neck (Erlenmeyer) flask of 1-L capacity, with a minimum external neck diameter of 50
mm, for the procedure.
5.1.1.2 Condenser—A condenser in the form of a metal coil approximately 25 mm in diameter and 50 mm in length attached
to, and with the ends projecting through, a lid of sufficient diameter to cover the neck of the flask as shown in Fig. 1. The coil shall
be made from stainless steel, tin, tin-plated copper, or tin-plated brass tubing having an outside diameter of 5 to 8 mm and a wall
thickness of 1.5 mm. If constructed of tin-plated copper or brass, the tin coating shall have a minimum thickness of 0.075 mm.
The exposed surface of the coil for cooling purposes is about 115 cm .
NOTE 2—The use of a water flowmeter/controller unit that monitors water flow to the condenser that shuts off the heat source when the flow rate drops
below a pre-set limit has been found suitable to prevent vaporized toluene from igniting. The use of such a device is recommended.
5.1.1.3 Extraction Thimble —The extraction thimble shall be of a refractory porous material, pore size 20.0 to 30.0 μm (as
certified by the manufacturer), 25 mm in diameter by 70 mm in height, weighing not less than 15 g and not more than 17 g. Suspend
the thimble from the condenser coil by means of a basket so that it hangs approximately midway between the surface of the
extracting solvent and the bottom of the condenser coil.
5.1.1.4 Thimble Basket—The thimble basket shall be corrosion-resistant and shall be made of platinum, stainless steel,
nickel-chromium alloy, or similar material. Fig. 2 shows the design and dimensions of two typical baskets that have been used
successfully in the industry.
The sole source of supply of the extraction thimble, AN 485, 25 × 70-mm, coarse porosity, drawing number QA 005163, known to the committee at this time is
Saint-Gobain/Norton Industrial Ceramics Corporation of Worcester, MA. If you are aware of alternative suppliers, please provide this information to ASTM International
Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend.
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D473 − 07 (2012)
FIG. 2 Basket Thimble Support
5.1.1.5 Water Cup—Use a water cup when testing a sample determined to have a water content greater than 10 % volume (see
Fig. 1, Apparatus B). The cup shall be made of glass, conical in shape, approximately 20 mm in diameter and 25 mm deep, and
have a 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 cup hangs with its rim reasonably level. In this procedure, suspend the thimble basket as shown in Fig. 1, Apparatus A by means
of the corrosion-resistant wire looped over the bottom of the condenser coil and attached to the basket supports, or as in Fig. 1,
Apparatus B, where the wire supports of the basket are attached to hooks soldered to the underside of the condenser lid.
5.1.1.6 Source of Heat—Use a source of heat, preferably a hot plate operated under a ventilated hood, suitable for vaporizing
toluene (Warning—Flammable.)
5.2 Analytical Balance—Use an analytical balance, with an accuracy of 0.1 mg. Verify the balance, at least annually, against
weights traceable to a national standards body such as the National Institute of Standards and Technology (NIST).
5.3 Non-aerating Mixer—Use a non-aerating mixer, meeting the verification of mixing efficiency requirements specified in
Practice D5854 (API Chapter 8.3). Either insertion mixers or circulating mixers or circulating external mixers are acceptable
provided they meet the criteria in Practice D5854 (API Chapter 8.3).
5.4 Oven—Use an oven capable of maintaining a temperature of 115 to 120°C (240 to 250°F).
5.5 Cooling Vessel—Use a desiccator without desiccant as a cooling vessel.
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D473 − 07 (2012)
TABLE 1 Typical Characteristics for ACS Reagent Grade Toluene
Assay 99.5+ %
Color (APHA) 10
A
Boiling range (initial to dry point) 2.0°C
Residue after evaporation 0.001 %
Substances darkened by H SO passes test
2 4
Sulfur compounds (as S) 0.003 %
Water (H O) (by Karl Fischer titration) 0.03 %
A
Recorded boiling point 110.6°C.
5.6 Temperature Measuring Device—Such as a thermometer, capable of measuring the temperature of the sample to the nearest
1°C (2°F).
6. Solvent
6.1 Toluene—Reagent grade conforming to the specifications of the Committee on Analytical Reagents of the American
Chemical Society (ACS) or to Grade 2 of ISO 5272. (Warning—Flammable. Keep away from heat, sparks and open flame. Vapor
harmful. Toluene is toxic. Particular care shall be taken to avoid breathing the vapors and to protect the eyes. Keep the container
closed. Use with adequate ventilation. Avoid prolonged or repeated contact with the skin.)
6.1.1 The typical characteristics for the ACS reagent are shown in Table 1.
7. Sampling
7.1 Sampling shall include all steps required to obtain an aliquot of the contents of any pipe, tank, or other system and to place
the sample into the laboratory test container.
7.2 Only use representative samples obtained as specified in Practices D4057 (API Chapter 8.1) and D4177 (API Chapter 8.2)
for this test method.
7.3 Draw test portions from the laboratory samples immediately after thorough mixing. Heat viscous samples to a temperature
which renders the
...
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