ASTM D4807-05(2020)

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.
Designation: D4807 − 05 (Reapproved 2020)
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 D473TestMethodforSedimentinCrudeOilsandFuelOils
by the Extraction Method
1.1 This test method covers the determination of sediment
D4057Practice for Manual Sampling of Petroleum and
incrudeoilsbymembranefiltration.Thistestmethodhasbeen
Petroleum Products
validated for crude oils with sediments up to approximately
D4177Practice for Automatic Sampling of Petroleum and
0.15% by mass.
Petroleum Products
1.2 The accepted unit of measure for this test method is
D4865Guide for Generation and Dissipation of Static Elec-
mass%, but an equation to convert to volume% is provided
tricity in Petroleum Fuel Systems
(see Note 6).
D5854Practice for Mixing and Handling of Liquid Samples
1.3 The values stated in SI units are to be regarded as the
of Petroleum and Petroleum Products
standard. The values given in parentheses are for information
2.2 API Standards:
only.
MPMS Chapter 8.1Manual Sampling of Petroleum and
1.4 This standard does not purport to address all of the
Petroleum Products (ASTM Practice D4057)
safety concerns, if any, associated with its use. It is the
MPMS Chapter 8.2Automatic Sampling of Petroleum and
responsibility of the user of this standard to establish appro-
Petroleum Products (ASTM Practice D4177)
priate safety, health, and environmental practices and deter-
MPMSChapter8.3MixingandHandlingofLiquidSamples
mine the applicability of regulatory limitations prior to use.
of Petroleum and Petroleum Products (ASTM Practice
For specific warning statements, see 6.1 and Annex A1.
D5854)
1.5 This international standard was developed in accor-
MPMS Chapter 10.1Test Method for Sediment in Crude
dance with internationally recognized principles on standard-
Oils and Fuel Oils by the Extraction Method (ASTMTest
ization established in the Decision on Principles for the
Method D473)
Development of International Standards, Guides and Recom-
mendations issued by the World Trade Organization Technical 2.3 ISO Standard:
Barriers to Trade (TBT) Committee. ISO 5272:1979Toluene for Industrial Use—Specifications
2. Referenced Documents
3. Summary of Test Method
2.1 ASTM Standards:
3.1 A portion of a representative crude oil sample is
dissolved in hot toluene and filtered under vacuum through a
This test method is under the jurisdiction of ASTM Committee D02 on
0.45µm porosity membrane filter. The filter with residue is
Petroleum Products, Liquid Fuels, and Lubricants and the API Committee on
washed, dried, and weighed to give the final result.
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, 2020. Published June 2020. Originally
approved in 1988. Last previous edition approved in 2015 as D4807 – 05 (2015).
DOI: 10.1520/D4807-05R20. Published as Manual of Petroleum Measurement Standards. Available from
For referenced ASTM standards, visit the ASTM website, www.astm.org, or AmericanPetroleumInstitute(API),1220L.St.,NW,Washington,DC20005-4070,
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM http://www.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
D4807 − 05 (2020)
5.4 Vacuum Pump—Use a vacuum pump capable of reduc-
ing and maintaining the pressure at −80kPa (−24in. Hg)
during the filtering.
5.5 Analytical Balance—Use an analytical balance capable
of measuring to the nearest 0.0001g. Verify the balance, at
least annually, against weights traceable to a national metrol-
ogy institute such as the National Institute of Standards and
Technology (NIST).
FIG. 1 Membrane Filtration Assembly
5.6 Heating Coil for Filter Assembly—Use copper tubing
(3.175mm or ⁄8in. diameter) wound around the funnel on the
filter apparatus and connected to a circulating bath to maintain
the oil in the funnel at 90°C 6 2°C (see Fig. 1). Alternative
4. Significance and Use
methods of heating the funnel such as heating tape or glass
4.1 A knowledge of the sediment content of crude oil is
thermal jacket could also be used.
important both in refinery operations and in crude oil com-
5.7 Mixer—Use a nonaerating, high-speed mixer meeting
merce.
the verification efficiency requirements specified in Practice
D5854 (API MPMS Chapter 8.3). Either insertion mixers or
5. Apparatus
circulating mixers are acceptable provided they meet the
5.1 Funnel and Filter Support Assembly—Use an assembly
criteria in Practice D5854 (API MPMS Chapter 8.3).
designed to hold 47mm diameter filters as was used in the
5.8 Cooling Vessel—Useadesiccatororothertypeoftightly
development of this test method (see Fig. 1).
covered vessel for cooling the membrane filter before weigh-
5.1.1 Filter Funnel—Use a filter funnel with a 250mL
ing. The use of a desiccant/drying agent is not recommended.
minimum capacity. The lower part of the funnel has a 40mm
inside diameter and is designed to secure the 47mm diameter
5.9 Ground/Bond Wire—Use a 0.912mm to 2.59mm (No.
filter against the filter support. The funnel can be jacketed to
10 through No. 19) bare stranded flexible, stainless steel or
facilitateheatingthesolventfunnelandsampleduringfiltering.
copper wire installed in the flask through the vacuum connec-
tion and connected to ground.
NOTE 1—Use of a glass funnel should minimize the effect of static
electricity when filtering.
6. Reagents
5.1.2 Filter Support—Use a support base for the filter that
6.1 Toluene—Reagent grade chemicals shall be used in all
has a porous scintered glass center section about 40mm to
tests.Unlessotherwiseindicated,itisintendedthatallreagents
43mmindiameter.Thesupportbaseisdesignedtofitsecurely
shall conform to the specifications of the Committee on
against the funnel holding the filter in place over the porous
Analytical Reagents of theAmerican Chemical Society, where
section. The filter support’s stem should be long enough to
such specifications are available, or to Grade 2 of ISO 5272.
extend down into the filter flask such that the end is below the
Other grades may be used, provided it is first ascertained that
vacuum connection.
thereagent’slotorbatchisofsufficientlyhighpuritytopermit
5.1.3 Clamp Assembly—Useaspringorscrewtypeclampto
its use without lessening the accuracy of the determination.
secure the funnel to the filter support. The clamp should be
(Warning—Flammable. Keep away from heat, sparks and
tightenoughtopreventthesolventfromleakingthroughatthe
open flame. Vapor harmful. Toluene is toxic. Particular care
junction between the glass and filter membrane. The exterior
shall be taken to avoid breathing the vapors and to protect the
dimensions of the funnel and support are designed to facilitate
eyes.Keepthecontainerclosed.Usewithadequateventilation.
clamping the two pieces together.
Avoid prolonged or repeated contact with the skin.)
5.1.4 Rubber Stopper—Use a single-hole, capable of hold-
ing the lower stem of the filter support securely onto the
7. Sampling, Test Specimens
filtering flask.
7.1 Sampling, shall include all the steps required to obtain a
5.1.5 Vacuum Filtering Flask—Use a 500mL or larger
vacuum filtering flask. representativeportionofthecontentsofanypipe,tank,orother
system, and to transfer the sample into the laboratory test
5.2 Membrane Filter—Use a nylon membrane filter, 47mm
6 container. The laboratory test container and sample volume
in diameter with 0.45µm pore size.
shallbeofsufficientdimensionsandvolumetoallowmixingas
5.3 Oven—Use an oven capable of maintaining a tempera-
described in 7.3.1. Mixing is required to properly disperse
ture of 105°C 6 2°C(220°F 6 4°F).
sediment as well as any water present in the sample.
5 7
The following filtration assembly was used in generating the precision: ACS Reagent Chemicals, Specifications and Procedures for Reagents and
Millipore Corp., Ashly Rd., Bedford, MA 01730. Other filtration assemblies also Standard-Grade Reference Materials, American Chemical Society, Washington,
may be acceptable. DC. For suggestions on the testing of reagents not listed by theAmerican Chemical
The following filter was used in generating the precision: MSI Nylon 60 Society, see Analar Standards for Laboratory Chemicals, BDH Ltd., Poole, Dorset,
Membrane Filter from Fisher Scientific, Catalog Number NO-4-SP047-00. Other U.K., and the United States Pharmacopeia and National Formulary, U.S. Pharma-
nylon filters of 0.45µm porosity also may be acceptable. copeial Convention, Inc. (USPC), Rockville, MD.
D4807 − 05 (2020)
7.2 Laboratory Sample—Use only representative samples filter in 10min to 15min. If the nature of the crude (for
obtained as specified in Practice D4057 (API MPMS Chapter example, heavy versus light gravity or high versus low
8.1) or Practice D4177 (API MPMS Chapter 8.2) for this test viscosity) or the amount of sediment causes the filtration to
method. Analyze samples within two weeks after taking the proceed extremely slowly (for example, filtering times greater
sample. Retaining samples longer may affect the results. than 30min), reduce the sample size to 5g or less and repeat
the test. Keep the volume of toluene at 100mL.
7.3 Sample Preparation—Thefollowingsamplepreparation
NOTE 4—If the filtration of a given crude typically takes less than
and handling procedure shall apply.
10min and the sample stays at 90°C 6 2°C (195°F 6 4°F) during this
7.3.1 Mix the test sample of crude oil at room temperature
time, then external heating o
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