ASTM D473-07(2017)
(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.
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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Designation: D473 − 07 (Reapproved 2017)
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.
1. Scope D4177Practice for Automatic Sampling of Petroleum and
Petroleum Products (API MPMS Chapter 8.2)
1.1 This test method covers the determination of sediment
D5854Practice for Mixing and Handling of Liquid Samples
in crude oils and fuel oils by extraction with toluene. The
of Petroleum and Petroleum Products (API MPMS Chap-
precision applies to a range of sediment levels from 0.01% to
ter 8.3)
0.40% mass, although higher levels may be determined.
E29Practice for Using Significant Digits in Test Data to
NOTE 1—Precision on recycled oils and crankcase oils is unknown and
Determine Conformance with Specifications
additional testing is required to determine that precision. 3
2.2 API Standards:
1.2 The values stated in SI units are to be regarded as
Chapter 8.1Manual Sampling of Petroleum and Petroleum
standard. No other units of measurement are included in this
Products (ASTM Practice D4057)
standard.
Chapter 8.2Automatic Sampling of Petroleum and Petro-
leum Products (ASTM Practice D4177)
1.3 This standard does not purport to address all of the
Chapter 8.3Mixing and Handling of Liquid Samples of
safety concerns, if any, associated with its use. It is the
Petroleum and Petroleum Products (ASTM Practice
responsibility of the user of this standard to establish appro-
D5854)
priate safety and health practices and determine the applica-
2.3 ISO Standard:
bility of regulatory limitations prior to use. For specific
5272 Toluene for industrial use—Specifications
warning statements, see 5.1.1.6 and 6.1.
1.4 This international standard was developed in accor-
3. Summary of Test Method
dance with internationally recognized principles on standard-
3.1 Extract test portion of a representative oil sample,
ization established in the Decision on Principles for the
contained in a refractory thimble, with hot toluene until the
Development of International Standards, Guides and Recom-
residue reaches constant mass.The mass of residue, calculated
mendations issued by the World Trade Organization Technical
as a percentage, is reported as sediment by extraction.
Barriers to Trade (TBT) Committee.
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
D4057Practice for Manual Sampling of Petroleum and
buying or selling of these commodities.
Petroleum Products (API MPMS Chapter 8.1)
5. Apparatus
5.1 Usuallaboratoryapparatusandglassware,togetherwith
This test method is under the jurisdiction of ASTM Committee D02 on
the following are required for this test method.
Petroleum Products, Liquid Fuels, and Lubricants and the API Committee on
5.1.1 Extraction Apparatus—Usetheapparatusillustratedin
Petroleum Measurement, and is the direct responsibility of Subcommittee D02.02
Figs. 1 and 2 and consisting of the elements described in
/COMQ on Hydrocarbon Measurement for Custody Transfer (Joint ASTM-API).
CurrenteditionapprovedJune1,2017.PublishedJuly2017.Originallyapproved
5.1.1.1 – 5.1.1.3.
ɛ1
in 1938. Last previous edition approved in 2012 as D473–07 (2012) . DOI:
10.1520/D0473-07R17.
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
D473 − 07 (2017)
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) means of a basket so that it hangs approximately midway
flask of 1L capacity, with a minimum external neck diameter betweenthesurfaceoftheextractingsolventandthebottomof
of 50mm, for the procedure.
the 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 25mm in diameter and 50mm in length at-
corrosion-resistant and shall be made of platinum, stainless
tached 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 5mm to 8mm and a wall thickness of 1.5mm. 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 0.075mm. The exposed surface
conicalinshape,approximately20mmindiameterand25mm
of the coil for cooling purposes is about 115cm .
deep,andhaveacapacityofapproximately3mL.Aglasshook
NOTE 2—The use of a water flowmeter/controller unit that monitors
fusedontherimatonesideissoshapedthatwhenhungonthe
water flow to the condenser that shuts off the heat source when the flow
condenser the cup hangs with its rim reasonably level. In this
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
be of a refractory porous material, pore size 20.0µm to
ofthebasketareattachedtohookssolderedtotheundersideof
30.0µm (as certified by the manufacturer), 25mm in diameter
the condenser lid.
by 70mm in height, weighing not less than 15g and not more
5.1.1.6 Source of Heat—Use a source of heat, preferably a
than 17g. Suspend the thimble from the condenser coil by
hot plate operated under a ventilated hood, suitable for vapor-
izing toluene (Warning—Flammable.)
The sole source of supply of the extraction thimble,AN 485, 25mm × 70mm,
coarse porosity, drawing number QA005163, known to the committee at this time
5.2 Analytical Balance—Use an analytical balance, with an
is Saint-Gobain/Norton Industrial Ceramics Corporation of Worcester, MA. If you
accuracy of 0.1mg. Verify the balance, at least annually,
are aware of alternative suppliers, please provide this information to ASTM
against weights traceable to a national standards body such as
International Headquarters. Your comments will receive careful consideration at a
meeting of the responsible technical committee, which you may attend. the National Institute of Standards and Technology (NIST).
D473 − 07 (2017)
FIG. 2 Basket Thimble Support
5.3 Non-aerating Mixer—Use a non-aerating mixer, meet- 6. Solvent
ingtheverificationofmixingefficiencyrequirementsspecified
6.1 Toluene—Reagent grade conforming to the specifica-
inPracticeD5854(APIChapter8.3).Eitherinsertionmixersor
tionsoftheCommitteeonAnalyticalReagentsoftheAmerican
circulatingmixersorcirculatingexternalmixersareacceptable 6
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
5.4 Oven—Use an oven capable of maintaining a tempera- shall be taken to avoid breathing the vapors and to protect the
ture of 115°C to 120°C (240°F to 250°F).
5.5 Cooling Vessel—Useadesiccatorwithoutdesiccantasa
Reagent Chemicals, American Chemical Society Specifications , American
cooling vessel.
Chemical Society, Washington, DC. For suggestions on the testing of reagents not
listed by the American Chemical Society, see Analar Standards for Laboratory
5.6 Temperature Measuring Device—Such as a
Chemicals,BDHLtd.,Poole,Dorset,U.K.,andtheUnitedStatesPharmacopeiaand
thermometer, capable of measuring the temperature of the
National Formulary, U.S. Pharmacopeial Convention, Inc., (USPC), Rockville, MD
sample to the nearest 1°C (2°F). 20852.
D473 − 07 (2017)
TABLE 1 Typical Characteristics for ACS Reagent Grade Toluene
After several determinations (the accumulated sediment may
Assay 99.5+ % be sufficient to interfere with further determinations), follow
Color (APHA) 10
the procedure described in 8.3 to remove the combustible
A
Boiling range (initial to dry point) 2.0 °C
portion of the accumulated sediment.Avoid excessive reuse of
Residue after evaporation 0.001 %
Substances darkened by H SO passes test thimbles, as over time the pores become clogged with inor-
2 4
Sulfur compounds (as S) 0.003 %
ganic material re
...
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 2017)
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. 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 0.010.01 % 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.
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.
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, 2012June 1, 2017. Published December 2012July 2017. Originally approved in 1938. Last previous edition approved in 20072012 as
ɛ1
D473D473 – 07 (2012) –07. DOI: 10.1520/D0473-07R12E01.10.1520/D0473-07R17.
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.
© 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
D473 − 07 (2017)
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-L1 L capacity, with a minimum external neck diameter of
50 mm, 50 mm, for the procedure.
5.1.1.2 Condenser—A condenser in the form of a metal coil approximately 25 mm 25 mm in diameter and 50 mm 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 55 mm
to 8 mm 8 mm and a wall thickness of 1.5 mm. 1.5 mm. If constructed of tin-plated copper or brass, the tin coating shall have a
minimum thickness of 0.075 mm. 0.075 mm. The exposed surface of the coil for cooling purposes is about 115 cm115 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 20.020.0 μm to 30.0 μm
30.0 μm (as certified by the manufacturer), 25 mm 25 mm in diameter by 70 mm 70 mm in height, weighing not less than 15 g
15 g and not more than 17 g. 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, 2525 mm × 70-mm,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.
D473 − 07 (2017)
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 20 mm in diameter and 25 mm 25 mm
deep, and have a capacity of approximately 3 mL. 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—WarningFlammable.)—Flammable.)
5.2 Analytical Balance—Use an analytical balance, with an accuracy of 0.1 mg. 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 115115 °C to 120°C (240120 °C (240 °F to 250°F).250 °F).
5.5 Cooling Vessel—Use a desiccator without desiccant as a cooling vessel.
D473 − 07 (2017)
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
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.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).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)
...
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