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 Filtration1
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 D473 Test Method for Sediment in Crude Oils and Fuel Oils
1.1 This test method covers the determination of sediment by the Extraction Method
in crude oils by membrane filtration. This test method has been D4057 Practice for Manual Sampling of Petroleum and
validated for crude oils with sediments up to approximately Petroleum Products
0.15 % by mass. D4177 Practice for Automatic Sampling of Petroleum and
Petroleum Products
1.2 The accepted unit of measure for this test method is
D4865 Guide 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).
D5854 Practice 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
only. 2.2 API Standards:3
MPMS Chapter 8.1 Manual 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 8.2 Automatic 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-
MPMS Chapter 8.3 Mixing and Handling of Liquid Samples
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 10.1 Test Method for Sediment in Crude
dance with internationally recognized principles on standard-
ization established in the Decision on Principles for the Oils and Fuel Oils by the Extraction Method (ASTM Test
Development of International Standards, Guides and Recom- Method D473)
mendations issued by the World Trade Organization Technical 2.3 ISO Standard:4
Barriers to Trade (TBT) Committee. ISO 5272:1979 Toluene for Industrial Use—Specifications
2. Referenced Documents 3. Summary of Test Method
2.1 ASTM Standards:2
3.1 A portion of a representative crude oil sample is
dissolved in hot toluene and filtered under vacuum through a
1
This test method is under the jurisdiction of ASTM Committee D02 on 0.45 µm porosity membrane filter. The filter with residue is
Petroleum Products, Liquid Fuels, and Lubricants and the API Committee on
Petroleum Measurement, and is the direct responsibility of Subcommittee D02.02 washed, dried, and weighed to give the final result.
/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).
3
DOI: 10.1520/D4807-05R20. Published as Manual of Petroleum Measurement Standards. Available from
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or American Petroleum Institute (API), 1220 L. St., NW, Washington, DC 20005-4070,
contact ASTM Customer Service at [email protected]. For Annual Book of ASTM http://www.api.org.
4
Standards volume information, refer to the standard’s Document Summary page on Available from American National Standards Institute (ANSI), 25 W. 43rd St.,
the ASTM website. 4th Floor, New York, NY 10036, http://www.ansi.org.

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 D4807 − 05 (2020)
5.4 Vacuum Pump—Use a vacuum pump capable of reduc-
ing and maintaining the pressure at −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. 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
(3.175 mm or 1⁄8 in. diameter) wound around the funnel on the
filter apparatus and connected to a circulating bath to maintain
4. Significance and Use the oil in the funnel at 90 °C 6 2 °C (see Fig. 1). Alternative
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-
merce. 5.7 Mixer—Use a nonaerating, high-speed mixer meeting
the verification efficiency requirements specified in Practice
5. Apparatus D5854 (API MPMS Chapter 8.3). Either insertion mixers or
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 47 mm diameter filters as was used in the
development of this test method (see Fig. 1).5 5.8 Cooling Vessel—Use a desiccator or other type of tightly
5.1.1 Filter Funnel—Use a filter funnel with a 250 mL covered vessel for cooling the membrane filter before weigh-
minimum capacity. The lower part of the funnel has a 40 mm ing. The use of a desiccant/drying agent is not recommended.
inside diameter and is designed to secure the 47 mm diameter 5.9 Ground/Bond Wire—Use a 0.912 mm to 2.59 mm (No.
filter against the filter support. The funnel can be jacketed to 10 through No. 19) bare stranded flexible, stainless steel or
facilitate heating the solvent funnel and sample during filtering. copper wire installed in the flask through the vacuum connec-
NOTE 1—Use of a glass funnel should minimize the effect of static tion and connected to ground.
electricity when filtering.
6. Reagents
5.1.2 Filter Support—Use a support base for the filter that
has a porous scintered glass center section about 40 mm to 6.1 Toluene—Reagent grade chemicals shall be used in all
43 mm in diameter. The support base is designed to fit securely tests. Unless otherwise indicated, it is intended that all reagents
against the funnel holding the filter in place over the porous shall conform to the specifications of the Committee on
section. The filter support’s stem should be long enough to Analytical Reagents of the American Chemical Society, where
extend down into the filter flask such that the end is below the such specifications are available,7 or to Grade 2 of ISO 5272.
vacuum connection. Other grades may be used, provided it is first ascertained that
5.1.3 Clamp Assembly—Use a spring or screw type clamp to the reagent’s lot or batch is of sufficiently high purity to permit
secure the funnel to the filter support. The clamp should be its use without lessening the accuracy of the determination.
tight enough to prevent the solvent from leaking through at the (Warning—Flammable. Keep away from heat, sparks and
junction between the glass and filter membrane. The exterior open flame. Vapor harmful. Toluene is toxic. Particular care
dimensions of the funnel and support are designed to facilitate shall be taken to avoid breathing the vapors and to protect the
clamping the two pieces together. eyes. Keep the container closed. Use with adequate ventilation.
5.1.4 Rubber Stopper—Use a single-hole, capable of hold- Avoid prolonged or repeated contact with the skin.)
ing the lower stem of the filter support securely onto the
filtering flask. 7. Sampling, Test Specimens
5.1.5 Vacuum Filtering Flask—Use a 500 mL or larger 7.1 Sampling, shall include all the steps required to obtain a
vacuum filtering flask. representative portion of the contents of any pipe, tank, or other
5.2 Membrane Filter—Use a nylon membrane filter, 47 mm system, and to transfer the sample into the laboratory test
in diameter with 0.45 µm pore size.6 container. The laboratory test container and sample volume
shall be of sufficient dimensions and volume to allow mixing as
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 the American Chemical
6
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 0.45 µm porosity also may be acceptable. copeial Convention, Inc. (USPC), Rockville, MD.
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 D4807 − 05 (2020)
7.2 Laboratory Sample—Use only representative samples filter in 10 min to 15 min. 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 30 min), reduce the sample size to 5 g or less and repeat
7.3 Sample Preparation—The following sample preparation the test. Keep the volume of toluene at 100 mL.
NOTE 4—If the filtration of a given crude typically takes less than
and handling procedure shall apply. 10 min 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 of the filter funnel may not be necessary.
in the original container immediately (within 15 min) before
8.7 Filter Washing—Before the last portion of sample has
analysis to ensure complete homogeneity. A test sample drawn
completely filtered, wash the funnel and filter with 50 mL of
directly from a large volume dynamic mixing system shall be
hot toluene (90 °C, 195 °F) until no oil is visible on the filter.
analyzed within 15 min or else remix as follows:
With the vacuum on, leave the filter on the apparatus for 2 min.
NOTE 2—Analysis should follow mixing as soon as possible. The
15 min interval mentioned above is a general guideline which may not
8.8 Apparatus Disassembly—Disassemble the filter appara-
apply to all crudes, especially some light crudes which do not hold water tus by removing the clamp and funnel. Inspect the condition of
and sediment in suspension for even this short a time. the filter. If the filter has been properly mounted, it may not be
7.3.2 Mixing of the sample should not increase the tempera- necessary to wash the edges after disassembly. However, if
ture of the sample more than 10 °C (20 °F), or a loss of water upon removing the funnel dark spots are observed around the
may occur affecting the sample’s composition. The type of edge of the filter further washing is necessary. With the vacuum
mixer depends on the quantity of crude. Before any unknown on, use a dropper to wash the filter’s edges with hot toluene
mixer is used, the specifications for the homogenization test, (90 °C, 195 °F).
Practice D5854 (API MPMS Chapter 8.3), must be met. The 8.9 If the filter is completely or partially covered with black

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mixer must be re-evaluated following any changes in the type or dark brown crude oil residue after the washing step above,
of crude, quantity of crude, or shape of the sample container. then discard the filter and repeat the test with a smaller sample
7.3.3 For small test sample volumes, 50 mL to 300 mL, a size.
nonaerating, high-speed, shear mixer is required. Use the NOTE 5—Normally the color of the sediment on the filter is gray or light
mixing time, mixing speed, and height above the bottom of the tan. A black or deep brown colored deposit on the filter is indicative of
container found to be satisfactory in Practice D5854 (API incomplete washing.
MPMS Chapter 8.3). Clean and dry the mixer between 8.10 If the appearance of the filter is acceptable (as in 8.9)
samples. then carefully remove it and place it in an oven at 105 °C
8. Procedure (220 °F) for 15 min. Cool in the cooling vessel to room
temperature (5 min to 10 min) and reweigh to the nearest
8.1 Filter Preparation—Prepare nylon filters by heating in 0.0001 g.
an oven at 105 °C 6 2 °C (220 °F 6 4 °F) for 15 min. Cool
and store the dried filters in a cooling vessel (desiccator 9. Calculation
without desiccant) until needed. Use only new filters.
9.1 Calculate the mass percent of sediment as follows:
8.2 Weigh the filter immediately before use to the nearest
m2 2 m1
0.0001 g. S5 3 100 (1)
ms
8.3 Using tweezers, place the membrane filter on the center
of the filter support, which is mounted on the filtering flask where:
with a rubber stopper. Attach the funnel to the filter support and S = sediment content of the sample as a percentage by
clamp it securely. mass,
m1 = mass of the filter, g,
8.4 Connect the heating coil to the circulating bath and
m2 = mass of the filter with the sediment, g, and
place the coil around the lower part of the funnel. Set the ms = mass of the sample, g.
temperature of the circulating bath so as to maintain the oil in
the funnel at 90 °C 6 2 °C (195 °F 6 4 °F). 10. Report
NOTE 3—Care should be taken not to overheat the funnel so as to cause
evaporation of the toluene and glazing of the filter. 10.1 Report results to the nearest 0.001 % as the mass
8.5 Sample Addition—Into a 200 mL beaker, weigh 10 g of percent of sediment by membrane filtration. The test report
a thoroughly mixed sample (see Section 7) to the nearest shall reference this Test Method D4807 (API MPMS Chapter
0.0001 g. Add 100 mL of toluene to the beaker and heat the 10.8) as the procedure used.
NOTE 6—Since water and sediment values are commonly reported as
mixture with stirring to 90 °C 6 2 °C (195 °F 6 4 °F). volume percent, calculate the volume of the sediment as a percentage of
Maintain the temperature at 90 °C 6 2 °C (195 °F 6 4 °F) for the original sample. As a major portion of the sediment probably would be
about 15 min to dissolve any wax in the crude. sand (silicon dioxide, which has a density of 2.32) and a small amount of
other naturally occurring materials (with a relative density lower than that
8.6 Start the vacuum pump and adjust the vacuum to of sand), use an arbitrary density of 2.0 for the resulting sediment. Then,
−80 kPa (−24 in. Hg). Carefully pour the sample mixture into to obtain volume percent sediment, divide the mass percent sediment by
the filter funnel in three portions. Generally the sample should 2.0 and multiply by the relative density of the crude oil. (Note that this

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 D4807 − 05 (2020)
TABLE 1 Precision Intervals 10.3 The test report shall also contain all details necessary
Mass Sediment Repeatability Reproducibility for complete identification of the product tested; any deviation,
0.0050 0.0031 0.0083 by agreement or otherwise, from the procedure specified; and
0.0100 0.0044 0.0118 the date of the test.
0.0150 0.0054 0.0144
0.0200 0.0062 0.0166 11. Precision and Bias
0.0250 0.0069 0.0186
0.0300 0.0076 0.0204 11.1 Repeatability—The difference between successive test
0.0350 0.0082 0.0220 results, obtained by the same operator with the same apparatus
0.0400 0.0088 0.0235
0.0450 0.0093 0.0249 under constant operating conditions on identical test material,
0.0500 0.0098 0.0263 would in the long run, in the normal and correct operation of
0.0600 0.0107 0.0288
0.0700 0.0116 0.0311
the test method, exceed the following values in only one case
0.0800 0.0124 0.0333 in twenty (see Table 1).
0.0900 0.0132 0.0353
0.1000 0.0139 0.0372
0.04388~ X 1/2 ! (3)
0.1250 0.0155 0.0416
0.1500 0.0170 0.0455
where:
X = sample mean in mass percent.
11.2 Reproducibility—The difference between two single
and independent test results obtained by different operators
calculation is provided for convenience only, and the precision and bias working in different laboratories on identical test material
for this standard are based on mass percent sediment and not on volume would, in the long run, in the normal and correct operation of
percent of sediment.) the test method, exceed the following values only in one case
S in twenty (see Table 1).
SV 5 3 relative density of the oil (2)
2.0 0.1176~ X 1/2 ! (4)
where: where:
SV = the sediment content of the sample as a percentage by X = sample mean in mass percent.
volume, and
11.3 Bias—The data generated during the development of
S = the sediment content of the sample as a percentage by
this test method showed that more sediment is reported for
mass.
crude oil using this test method compared to the results of Test
10.2 Report that the sample mixing procedure was per- Method D473 (API MPMS Chapter 10.1).
formed in accordance with the procedures specified in Practice
D5854 (API MPMS Chapter 8.3). Report the temperature of the 12. Keywords
sample before and after mixing. 12.1 crude oil; membrane filtration; sediment

ANNEX

(Mandatory Information)

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A1. SAFETY PRECAUTIONS TO AVOID STATIC DISCHARGE

A1.1 In Guide D4865 it is noted that micro-filters are filtration, very little time is available for charge recombination
prolific generators of electrostatic charge. This is particularly due to high velocities through the membrane. As a conse-
true in the case of membrane filters used in this procedure. quence even high conductivity oils may cause charges to
A1.1.1 The flow of crude oil through the membrane in accumulate in the membrane holder and receiver and develop
performing this type of test causes charges to separate due to significant voltage differences between the oil and apparatus.
the presence of ionic impurities or additives in the crude oil. Using a glass receiving flask and placing a grounding wire in
Charges of one polarity are carried with the moving oil while the receiver will minimize the development of voltage in the
the opposite charges accumulate within the membrane and its fuel.
holder. The surface charges seek a path to ground.
A1.3 Although grounding the apparatus will not prevent
A1.2 The rate at which these charges recombine depends on charge separation or accumulation of charges in the oil, it is
the conductivity of the oil. Relaxation time could be of the necessary to bond all parts of the filtration apparatus together
order of 10 s to 100 s with low conductivity oil. In membrane and provide a grounding wire. It is essential that no unbonded

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 D4807 − 05 (2020)
metal components are present during filtration since they
concentrate charge and develop voltage sufficient to cause
static discharge within the apparatus.
A1.4 To verify that bonding of all parts of the filtration
apparatus is complete the method requires that an electrical
conductivity test be conducted using a multimeter. There must
be 10 Ω or less resistance between any two points.

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