ASTM D4807-05(2010)
(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
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.
General Information
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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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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: D4807 − 05(Reapproved 2010)
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 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.
0.45-µm 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 47-mm 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 250 mL
minimum capacity. The lower part of the funnel has a 40-mm
This test method is under the jurisdiction of ASTM Committee D02 on inside diameter and is designed to secure the 47-mm diameter
Petroleum Products 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 May 1, 2010. Published May 2010. Originally AmericanPetroleumInstitute(API),1220L.St.,NW,Washington,DC20005-4070,
ε1
approved in 1988. Last previous edition approved in 2005 as D4807 – 05 . DOI: http://www.api.org.
10.1520/D4807-05R10. 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.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D4807 − 05 (2010)
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 0.912–2.59 mm (No. 10
throughNo.19)barestrandedflexible,stainlesssteelorcopper
wire installed in the flask through the vacuum connection 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 40 to 43 mm
Analytical Reagents of theAmerican Chemical Society, where
indiameter.Thesupportbaseisdesignedtofitsecurelyagainst
such specifications are available, or to Grade 2 of ISO 5272.
the funnel holding the filter in place over the porous section.
Other grades may be used, provided it is first ascertained that
Thefiltersupport’sstemshouldbelongenoughtoextenddown
thereagent’slotorbatchisofsufficientlyhighpuritytopermit
into the filter flask such that the end is below the vacuum
its use without lessening the accuracy of the determination.
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 500 mL or larger
container. The laboratory test container and sample volume
vacuum filtering flask.
shallbeofsufficientdimensionsandvolumetoallowmixingas
5.2 Membrane Filter—Use a nylon membrane filter, 47 mm
described in 7.3.1. Mixing is required to properly disperse
in diameter with 0.45-µm pore size.
sediment as well as any water present in the sample.
5.3 Oven—Use an oven capable of maintaining a tempera-
7.2 Laboratory Sample—Use only representative samples
ture of 105 6 2°C (220 6 4°F).
obtained as specified in Practice D4057 (API MPMS Chapter
5.4 Vacuum Pump—Use a vacuum pump capable of reduc- 8.1) or Practice D4177 (API MPMS Chapter 8.2) for this test
ing and maintaining the pressure at −80 kPa (−24 in. Hg)
method. Analyze samples within two weeks after taking the
during the filtering. sample. Retaining samples longer may affect the results.
5.5 Analytical Balance—Use an analytical balance capable
7.3 Sample Preparation—Thefollowingsamplepreparation
of measuring to the nearest 0.0001 g. Verify the balance, at and handling procedure shall apply.
least annually, against weights traceable to a national metrol- 7.3.1 Mix the test sample of crude oil at room temperature
ogy institute such as the National Institute of Standards and in the original container immediately (within 15 min) before
Technology (NIST). analysis to ensure complete homogeneity.Atest sample drawn
directly from a large volume dynamic mixing system shall be
5.6 Heating Coil for Filter Assembly—Use copper tubing
analyzed within 15 min or else remix as follows:
(3.175 mm or ⁄8-in. diameter) wound around the funnel on the
filter apparatus and connected to a circulating bath to maintain
NOTE 2—Analysis should follow mixing as soon as possible. The
15-min interval mentioned above is a general guideline which may not
the oil in the funnel at 90 6 2°C (see Fig. 1). Alternative
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 0.45-µm porosity also may be acceptable. MD.
D4807 − 05 (2010)
apply to all crudes, especially some light crudes which do not hold water
8.8 Apparatus Disassembly—Disassemble the filter appara-
and sediment in suspension for even this short a time.
tusbyremovingtheclampandfunnel.Inspecttheconditionof
the filter. If the filter has been properly mounted, it may not be
7.3.2 Mixingofthesampleshouldnotincreasethetempera-
necessary to wash the edges after
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