ASTM D4807-05(2015)
(Test Method)Standard Test Method for Sediment in Crude Oil by Membrane Filtration
Standard Test Method for Sediment in Crude Oil by Membrane Filtration
SIGNIFICANCE AND USE
4.1 A knowledge of the sediment content of crude oil is important both in refinery operations and in crude oil commerce.
SCOPE
1.1 This test method covers the determination of sediment in crude oils by membrane filtration. This test method has been validated for crude oils with sediments up to approximately 0.15 mass %.
1.2 The accepted unit of measure for this test method is mass %, but an equation to convert to volume % is provided (see Note 6).
1.3 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.
1.4 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 6.1 and Annex A1.
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Designation: D4807 − 05 (Reapproved 2015)
Manual of Petroleum Measurement Standards (MPMS), Chapter 10.8
Standard Test Method for
Sediment in Crude Oil by Membrane Filtration
This standard is issued under the fixed designation D4807; 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 of Petroleum and Petroleum Products
2.2 API Standards:
1.1 This test method covers the determination of sediment
MPMS Chapter 8.1Manual Sampling of Petroleum and
incrudeoilsbymembranefiltration.Thistestmethodhasbeen
Petroleum Products (ASTM Practice D4057)
validated for crude oils with sediments up to approximately
MPMS Chapter 8.2Automatic Sampling of Petroleum and
0.15 mass%.
Petroleum Products (ASTM Practice D4177)
1.2 The accepted unit of measure for this test method is
MPMSChapter8.3MixingandHandlingofLiquidSamples
mass%, but an equation to convert to volume% is provided
of Petroleum and Petroleum Products (ASTM Practice
(see Note 6).
D5854)
MPMS Chapter 10.1Test Method for Sediment in Crude
1.3 The values stated in SI units are to be regarded as the
standard. The values given in parentheses are for information Oils and Fuel Oils by the Extraction Method (ASTMTest
Method D473)
only.
2.3 ISO Standard:
1.4 This standard does not purport to address all of the
ISO 5272:1979Toluene 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 A portion of a representative crude oil sample is
bility of regulatory limitations prior to use. For specific
dissolved in hot toluene and filtered under vacuum through a
warning statements, see 6.1 and Annex A1.
0.45µm porosity membrane filter. The filter with residue is
washed, dried, and weighed to give the final result.
2. Referenced Documents
2.1 ASTM Standards:
4. Significance and Use
D473TestMethodforSedimentinCrudeOilsandFuelOils
4.1 A knowledge of the sediment content of crude oil is
by the Extraction Method
important both in refinery operations and in crude oil com-
D4057Practice for Manual Sampling of Petroleum and
merce.
Petroleum Products
D4177Practice for Automatic Sampling of Petroleum and
5. Apparatus
Petroleum Products
5.1 Funnel and Filter Support Assembly—Use an assembly
D4865Guide for Generation and Dissipation of Static Elec-
designed to hold 47mm diameter filters as was used in the
tricity in Petroleum Fuel Systems
development of this test method (see Fig. 1).
D5854Practice for Mixing and Handling of Liquid Samples
5.1.1 Filter Funnel—Use a filter funnel with a 250mL
minimum capacity. The lower part of the funnel has a 40mm
This test method is under the jurisdiction of ASTM Committee D02 on inside diameter and is designed to secure the 47mm diameter
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). Published as Manual of Petroleum Measurement Standards. Available from
Current edition approved April 1, 2015. Published May 2015. Originally AmericanPetroleumInstitute(API),1220L.St.,NW,Washington,DC20005-4070,
approved in 1988. Last previous edition approved in 2010 as D4807 – 05 (2010). http://www.api.org.
DOI: 10.1520/D4807-05R15. Available fromAmerican National Standards Institute (ANSI), 25 W. 43rd St.,
For referenced ASTM standards, visit the ASTM website, www.astm.org, or 4th Floor, New York, NY 10036, http://www.ansi.org.
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM The following filtration assembly was used in generating the precision:
Standards volume information, refer to the standard’s Document Summary page on Millipore Corp., Ashly Rd., Bedford, MA 01730. Other filtration assemblies also
the ASTM website. may be acceptable.
© 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
D4807 − 05 (2015)
5.7 Mixer—Use a nonaerating, high-speed mixer meeting
the verification efficiency requirements specified in Practice
D5854 (API MPMS Chapter 8.3). Either insertion mixers or
circulating mixers are acceptable provided they meet the
criteria in Practice D5854 (API MPMS Chapter 8.3).
5.8 Cooling Vessel—Useadesiccatororothertypeoftightly
covered vessel for cooling the membrane filter before weigh-
ing. The use of a desiccant/drying agent is not recommended.
FIG. 1 Membrane Filtration Assembly
5.9 Ground/Bond Wire—Use a 0.912mm to 2.59mm (No.
10 through No. 19) bare stranded flexible, stainless steel or
copper wire installed in the flask through the vacuum connec-
tion and connected to ground.
filter against the filter support. The funnel can be jacketed to
facilitateheatingthesolventfunnelandsampleduringfiltering.
6. Reagents
NOTE 1—Use of a glass funnel should minimize the effect of static
6.1 Toluene—Reagent grade chemicals shall be used in all
electricity when filtering.
tests.Unlessotherwiseindicated,itisintendedthatallreagents
5.1.2 Filter Support—Use a support base for the filter that
shall conform to the specifications of the Committee on
has a porous scintered glass center section about 40mm to
Analytical Reagents of theAmerican Chemical Society, where
43mmindiameter.Thesupportbaseisdesignedtofitsecurely
such specifications are available, or to Grade 2 of ISO 5272.
against the funnel holding the filter in place over the porous
Other grades may be used, provided it is first ascertained that
section. The filter support’s stem should be long enough to
thereagent’slotorbatchisofsufficientlyhighpuritytopermit
extend down into the filter flask such that the end is below the
its use without lessening the accuracy of the determination.
vacuum connection.
(Warning—Flammable. Keep away from heat, sparks and
5.1.3 Clamp Assembly—Useaspringorscrewtypeclampto
open flame. Vapor harmful. Toluene is toxic. Particular care
secure the funnel to the filter support. The clamp should be
shall be taken to avoid breathing the vapors and to protect the
tightenoughtopreventthesolventfromleakingthroughatthe
eyes.Keepthecontainerclosed.Usewithadequateventilation.
junction between the glass and filter membrane. The exterior
Avoid prolonged or repeated contact with the skin.)
dimensions of the funnel and support are designed to facilitate
clamping the two pieces together. 7. Sampling, Test Specimens
5.1.4 Rubber Stopper—Use a single-hole, capable of hold-
7.1 Sampling, shall include all the steps required to obtain a
ing the lower stem of the filter support securely onto the
representativeportionofthecontentsofanypipe,tank,orother
filtering flask.
system, and to transfer the sample into the laboratory test
5.1.5 Vacuum Filtering Flask—Use a 500mL or larger
container. The laboratory test container and sample volume
vacuum filtering flask.
shallbeofsufficientdimensionsandvolumetoallowmixingas
described in 7.3.1. Mixing is required to properly disperse
5.2 Membrane Filter—Use a nylon membrane filter, 47mm
sediment as well as any water present in the sample.
in diameter with 0.45µm pore size.
7.2 Laboratory Sample—Use only representative samples
5.3 Oven—Use an oven capable of maintaining a tempera-
obtained as specified in Practice D4057 (API MPMS Chapter
ture of 105°C 6 2°C(220°F 6 4°F).
8.1) or Practice D4177 (API MPMS Chapter 8.2) for this test
5.4 Vacuum Pump—Use a vacuum pump capable of reduc-
method. Analyze samples within two weeks after taking the
ing and maintaining the pressure at −80kPa (−24in. Hg)
sample. Retaining samples longer may affect the results.
during the filtering.
7.3 Sample Preparation—Thefollowingsamplepreparation
5.5 Analytical Balance—Use an analytical balance capable
and handling procedure shall apply.
of measuring to the nearest 0.0001g. Verify the balance, at
7.3.1 Mix the test sample of crude oil at room temperature
least annually, against weights traceable to a national metrol-
in the original container immediately (within 15min) before
ogy institute such as the National Institute of Standards and
analysis to ensure complete homogeneity.Atest sample drawn
Technology (NIST).
directly from a large volume dynamic mixing system shall be
5.6 Heating Coil for Filter Assembly—Use copper tubing
analyzed within 15min or else remix as follows:
(3.175mm or ⁄8in. diameter) wound around the funnel on the
NOTE 2—Analysis should follow mixing as soon as possible. The
filter apparatus and connected to a circulating bath to maintain
15min interval mentioned above is a general guideline which may not
the oil in the funnel at 90°C 6 2°C (see Fig. 1). Alternative
apply to all crudes, especially some light crudes which do not hold water
methods of heating the funnel such as heating tape or glass
thermal jacket could also be used.
Reagent Chemicals, American Chemical Society Specifications, American
Chemical Society, Washington, DC. For suggestions on the testing of reagents not
listed by the American Chemical Society, see Analar Standards for Laboratory
The following filter was used in generating the precision: MSI Nylon 60 Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
Membrane Filter from Fisher Scientific, Catalog Number NO-4-SP047-00. Other and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
nylon filters of 0.45µm porosity also may be acceptable. MD.
D4807 − 05 (2015)
and sediment in suspension for even this short a time.
the filter. If the filter has been properly mounted, it may not be
necessary to wash the edges after disassembly. However, if
7.3.2 Mixingofthesampleshouldnotincreasethetempera-
upon removing the funnel dark spots are observed around the
tu
...
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.
Designation: D4807 − 05 (Reapproved 2010) D4807 − 05 (Reapproved 2015)
Manual of Petroleum Measurement Standards (MPMS), Chapter 10.8
Standard Test Method for
Sediment in Crude Oil by Membrane Filtration
This standard is issued under the fixed designation D4807; 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.
1. Scope
1.1 This test method covers the determination of sediment in crude oils by membrane filtration. This test method has been
validated for crude oils with sediments up to approximately 0.15 mass %.
1.2 The accepted unit of measure for this test method is mass %, but an equation to convert to volume % is provided (see Note
6).
1.3 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.
1.4 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 6.1 and Annex A1.
2. Referenced Documents
2.1 ASTM Standards:
D473 Test Method for Sediment in Crude Oils and Fuel Oils by the Extraction Method
D4057 Practice for Manual Sampling of Petroleum and Petroleum Products
D4177 Practice for Automatic Sampling of Petroleum and Petroleum Products
D4865 Guide for Generation and Dissipation of Static Electricity in Petroleum Fuel Systems
D5854 Practice for Mixing and Handling of Liquid Samples of Petroleum and Petroleum Products
2.2 API Standards:
MPMS Chapter 8.1 Manual Sampling of Petroleum and Petroleum Products (ASTM Practice D4057)
MPMS Chapter 8.2 Automatic Sampling of Petroleum and Petroleum Products (ASTM Practice D4177)
MPMS Chapter 8.3 Mixing and Handling of Liquid Samples of Petroleum and Petroleum Products (ASTM Practice D5854)
MPMS Chapter 10.1 Test Method for Sediment in Crude Oils and Fuel Oils by the Extraction Method (ASTM Test Method
D473)
2.3 ISO Standard:
ISO 5272:1979 Toluene for Industrial Use—Specifications
3. Summary of Test Method
3.1 A portion of a representative crude oil sample is dissolved in hot toluene and filtered under vacuum through a
0.45-μm0.45 μm porosity membrane filter. The filter with residue is washed, dried, and weighed to give the final result.
4. Significance and Use
4.1 A knowledge of the sediment content of crude oil is important both in refinery operations and in crude oil commerce.
This test method is under the jurisdiction of ASTM Committee D02 on Petroleum Products 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 May 1, 2010April 1, 2015. Published May 2010May 2015. Originally approved in 1988. Last previous edition approved in 20052010 as D4807
ε1
– 05 . (2010). DOI: 10.1520/D4807-05R10.10.1520/D4807-05R15.
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.
Published as Manual of Petroleum Measurement Standards. Available from American Petroleum Institute (API), 1220 L. St., NW, Washington, DC 20005-4070,
http://www.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
D4807 − 05 (2015)
FIG. 1 Membrane Filtration Assembly
5. Apparatus
5.1 Funnel and Filter Support Assembly—Use an assembly designed to hold 47-mm47 mm diameter filters as was used in the
development of this test method (see Fig. 1).
5.1.1 Filter Funnel—Use a filter funnel with a 250 mL 250 mL minimum capacity. The lower part of the funnel has a
40-mm40 mm inside diameter and is designed to secure the 47-mm47 mm diameter filter against the filter support. The funnel can
be jacketed to facilitate heating the solvent funnel and sample during filtering.
NOTE 1—Use of a glass funnel should minimize the effect of static electricity when filtering.
5.1.2 Filter Support—Use a support base for the filter that has a porous scintered glass center section about 4040 mm to 43 mm
43 mm in diameter. The support base is designed to fit securely against the funnel holding the filter in place over the porous section.
The filter support’s stem should be long enough to extend down into the filter flask such that the end is below the vacuum
connection.
5.1.3 Clamp Assembly—Use a spring or screw type clamp to secure the funnel to the filter support. The clamp should be tight
enough to prevent the solvent from leaking through at the junction between the glass and filter membrane. The exterior dimensions
of the funnel and support are designed to facilitate clamping the two pieces together.
5.1.4 Rubber Stopper—Use a single-hole, capable of holding the lower stem of the filter support securely onto the filtering flask.
5.1.5 Vacuum Filtering Flask—Use a 500 mL 500 mL or larger vacuum filtering flask.
5.2 Membrane Filter—Use a nylon membrane filter, 47 mm 47 mm in diameter with 0.45-μm0.45 μm pore size.
5.3 Oven—Use an oven capable of maintaining a temperature of 105105 °C 6 2°C (220 2 °C (220 °F 6 4°F).4 °F).
5.4 Vacuum Pump—Use a vacuum pump capable of reducing and maintaining the pressure at −80 kPa (−24 in. −80 kPa (−24 in.
Hg) during the filtering.
5.5 Analytical Balance—Use an analytical balance capable of measuring to the nearest 0.0001 g. 0.0001 g. Verify the balance,
at least annually, against weights traceable to a national metrology institute such as the National Institute of Standards and
Technology (NIST).
5.6 Heating Coil for Filter Assembly—Use copper tubing (3.175 mm (3.175 mm or ⁄8-in. in. diameter) wound around the funnel
on the filter apparatus and connected to a circulating bath to maintain the oil in the funnel at 9090 °C 6 2°C2 °C (see Fig. 1).
Alternative methods of heating the funnel such as heating tape or glass thermal jacket could also be used.
5.7 Mixer—Use a nonaerating, high-speed mixer meeting the verification efficiency requirements specified in Practice D5854
(API MPMS Chapter 8.3). Either insertion mixers or circulating mixers are acceptable provided they meet the criteria in Practice
D5854 (API MPMS Chapter 8.3).
5.8 Cooling Vessel—Use a desiccator or other type of tightly covered vessel for cooling the membrane filter before weighing.
The use of a desiccant/drying agent is not recommended.
5.9 Ground/Bond Wire—Use a 0.912–2.59 mm 0.912 mm to 2.59 mm (No. 10 through No. 19) bare stranded flexible, stainless
steel or copper wire installed in the flask through the vacuum connection and connected to ground.
6. Reagents
6.1 Toluene—Reagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended that all reagents shall
conform to the specifications of the Committee on Analytical Reagents of the American Chemical Society, where such
The following filtration assembly was used in generating the precision: Millipore Corp., Ashly Rd., Bedford, MA 01730. Other filtration assemblies also may be
acceptable.
The following filter was used in generating the precision: MSI Nylon 60 Membrane Filter from Fisher Scientific, Catalog Number NO-4-SP047-00. Other nylon filters
of 0.45-μm0.45 μm porosity also may be acceptable.
D4807 − 05 (2015)
specifications are available, or to Grade 2 of ISO 5272. Other grades may be used, provided it is first ascertained that the reagent’s
lot or batch is of sufficiently high purity to permit its use without lessening the accuracy of the determination. (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.)
7. Sampling, Test Specimens
7.1 Sampling, shall include all the steps required to obtain a representative portion of the contents of any pipe, tank, or other
system, and to transfer the sample into the laboratory test container. The laboratory test container and sample volume shall be of
sufficient dimensions and volume to allow mixing as described in 7.3.1. Mixing is required to properly disperse sediment as well
as any water present in the sample.
7.2 Laboratory Sample—Use only representative samples obtained as specified in Practice D4057 (API MPMS Chapter 8.1) or
Practice D4177 (API MPMS Chapter 8.2) for this test method. Analyze samples within two weeks after taking the sample.
Retaining samples longer may affect the results.
7.3 Sample Preparation—The following sample preparation and handling procedure shall apply.
7.3.1 Mix the test sample of crude oil at room temperature in the original container immediately (within 15 min) 15 min) before
analysis to ensure complete homogeneity. A test sample drawn directly from a large volume dynamic mixing system shall be
analyzed within 15 min 15 min or else remix as follows:
NOTE 2—Analysis should follow mixing as soon as possible. The 15-min15 min interval mentioned above is a general guideline which may not apply
to all crudes, especially some light crudes which do not hold water and sediment in suspension for even this short a time.
7.3.2 Mixing of the sample should not increase the temperature of the sample more than 10°C (20°F),10 °C (20 °F), or a loss
of water may occur affecting the sample’s composition. The type of mixer depends on the quantity of crude. Before any unknown
mixer is used, the specifications for the homogenization test, Practice D5854 (API MPMS Chapter 8.3), must be met. The mixer
must be re-evaluated following any changes in the type of crude, quantity of crude, or shape of the sample container.
7.3.3 For small test sample volumes, 5050 mL to 300 mL, 300 mL, a nonaerating, high-speed, shear mixer is required.
...
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