An American National Standard

Designation: D 4807 – 88 (Reapproved 1999)

Designation: MPMS Chapter 10.8

Standard Test Method for

Sediment in Crude Oil by Membrane Filtration1
This standard is issued under the fixed designation D 4807; 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 (e) indicates an editorial change since the last revision or reapproval.

This test method has been approved by the sponsoring committee and accepted by the Cooperating Societies in accordance with
established procedures.

This standard has been approved for use by agencies of the Department of Defense.

1. Scope 4. Significance and Use

1.1 This test method covers the determination of sediment 4.1 A knowledge of the sediment content of crude oil is
in crude oils by membrane filtration. This test method has been important both in the operation of the refinery and in the
validated for crude oils with sediments up to about 0.15 mass buying and selling of crude oils.
%.
1.2 This standard does not purport to address all of the 5. Apparatus
safety concerns, if any, associated with its use. It is the 5.1 Reservoir and Filter Support Assembly—an assembly
responsibility of the user of this standard to establish appro- designed to hold 47-mm diameter filters was used in the
priate safety and health practices and determine the applica- development of this test method (see Fig. 1).4
bility of regulatory limitations prior to use. 5.1.1 Filter Reservoir—capable of holding from about 250
1.3 The accepted unit of measure for this test method is mL of solvent. The lower part of the reservoir has a 40-mm
mass %. inside diameter and is designed to secure the 47-mm diameter
filter against the filter support. The reservoir can be jacketed to
2. Referenced Documents facilitate heating the reservoir and sample during filtering.
2.1 ASTM Standards: NOTE 1—Use of a glass reservoir should minimize the effect of static
D 473 Test Method for Sediment in Crude Oils and Fuel electricity when filtering.
Oils by the Extraction Method2
D 2892 Test Method for Distillation of Crude Petroleum 5.1.2 Filter Support/Funnel—support base for the filter has
(15-Theoretical Plate Column)3 a porous scintered glass center section about 40 to 43 mm in
D 4057 Practice for Manual Sampling of Petroleum and diameter. The support base is designed to fit securely against
Petroleum Products3 the reservoir holding the filter in place over the porous section.
D 4177 Practice for Automatic Sampling of Petroleum and The stem of the funnel portion should be long enough to extend
Petroleum Products3 down into the filter flask such that the end is below the outlet
D 4377 Test Method for Water in Crude Oils by Pontentio- for the vacuum.
metric Karl Fischer Titration3 5.1.3 Clamp Assembly—spring or screw type clamp to
secure the reservoir to the filter support. The clamp should be
3. Summary of Test Method tight enough to prevent the solvent from leaking through at the
3.1 A portion of a representative crude oil sample is junction between the glass and filter membrane. The exterior
dissolved in hot toluene and filtered under vacuum through a dimensions of the reservoir and support/funnel are designed to
0.45-µm porosity membrane filter. The filter with residue is facilitate clamping the two pieces together.
washed, dried, and weighed to give the final result. 5.1.4 Rubber Stopper—a single-hole, capable of holding the
lower stem of the filter support/funnel securely onto the
filtering flask.
5.1.5 Vacuum Filtering Flask, 500 mL or larger.
1
This test method is under the jurisdiction of ASTM Committee D-2 on 5.2 Membrane Filter, nylon membrane filter, 47 mm in
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee
D02.02 on Static Petroleum Measurement.
Current edition approved March 25, 1988. Published May 1988. 4
A filtration assembly as supplied by Millipore Corp., Ashly Rd., Bedford, MA
2
Annual Book of ASTM Standards, Vol 05.01. 01730, was found acceptable.
3
Annual Book of ASTM Standards, Vol 05.02.

Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.

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 D 4807
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 D 4057 or D 4177 for this test
method. Analyze samples within two weeks after taking the
sample. Retaining samples longer may affect the results.
FIG. 1 Membrane Filtration Assembly 7.3 Test Samples—The following sample handling proce-
dure shall apply.
7.3.1 Mix the test sample of crude oil at room temperature
diameter with 0.45-µm pore size.5
in the original container immediately (within 15 min) before
5.3 Oven, capable of maintaining a temperature of 105 6
analysis to ensure complete homogeneity. A test sample drawn
2°C.
directly from a large volume dynamic mixing system analyze
5.4 Vacuum Pump, capable of reducing and maintaining the
within 15 min or else remix as follows:
pressure at 200 mm Hg (−80 KPA) during the filtering.
5.5 Analytical Balance, capable of measuring to the nearest NOTE 3—Analysis should follow mixing as soon as possible. The
0.0001 g. 15-min interval mentioned above is a general guideline which may not
5.6 Heating Coil for Filter Assembly— copper tubing (1⁄8- apply to all crudes, especially some light crudes which do not hold water
in suspension for even this short a time.
in. diameter) wound around the reservoir on the filter apparatus
and connected to a circulating bath to maintain the oil in the 7.3.2 Mixing of the sample should not increase the tempera-
reservoir at 90 6 2°C (see Fig. 1). Alternative methods of ture of the sample more than 10°C, or a loss of water may
heating the reservoir such as heating tape or glass thermal occur and this affects sample composition. The type of mixer
jacket could also be used. depends on the quantity of crude. Before any unknown mixer
5.7 Mixer6—a nonaerating, high-speed mixer capable of is used, the specifications for the homogenization test, Annex
meeting the homogenization efficiency test in Annex A1. Large A, must be met. The mixer must be re-evaluated following any
volume dynamic mixing systems such as those used with changes in the type of crude, quantity of crude, or shape of the
automatic crude oil sampling receptacles are also acceptable sample container.
providing they comply with Annex A1. 7.3.3 For small test sample volumes, 50 to 300 mL, a
nonaerating, high-speed, shear mixer is required. Use the
6. Reagents mixing time, mixing speed, and height above the bottom of the
6.1 Purity of Reagents—Reagent grade chemicals shall be container found to be satisfactory in Annex A1. Clean and dry
used in all tests. Unless otherwise indicated, it is intended that the mixer between samples.
all reagents shall conform to the specifications of the Commit-
8. Procedure
tee on Analytical Reagents of the American Chemical Society,
where such specifications are available.7 Other grades may be 8.1 Prepare nylon filters by heating in an oven at 105°C for
used, provided it is first ascertained that the reagent is of 15 min. Cool and store the dried filters in a desiccator (without
sufficiently high purity to permit its use without lessening the desiccant) until needed. Use only new filters.
accuracy of the determination. 8.2 Weigh the filter immediately before use to the nearest
6.2 Toluene (Warning, Flammable). 0.0001 g.
8.3 Using tweezers, place the membrane filter on the center
NOTE 2—Warning: Flammable. of the filter support, which is mounted on the filtering flask
7. Sampling, Test Specimens with a rubber stopper. Attach the reservoir to the filter support
and clamp it securely.
7.1 Sampling, is defined as all the steps required to obtain an
8.4 Connect the heating coil to the circulating bath and
aliquot of the contents of any pipe, tank, or other system, and
place the coil around the lower part of the reservoir. Set the
to place the sample into the laboratory test container. The
temperature of the circulating bath so as to maintain the oil in
the reservoir at 90 6 2°C.
5
The following filter was used in generating the precision: MSI Nylon 60 NOTE 4—Care should be taken not to overheat the reservoir so as to
Membrane Filter from Fisher Scientific, Catalog Number NO-4-SP047-00. Other cause evaporation of the toluene and glazing of the filter.
nylon filters of 0.45-µm porosity also may be acceptable.
6
The following mixers have been found satisfactory for samples under 300 mL: 8.5 Into a 200-mL beaker, weigh 10 g of a thoroughly mixed
Ultra Turrax Model TP 18/10, available from Tekmar Co., Cincinnati, OH; sample (see Section 7) to the nearest 0.0001 g. Add 100 mL of
Brinkman Polytron Model PT 35, available from Brinkman Instruments, Inc., toluene to the beaker and heat the mixture with stirring to 90 6
Westbury, NY; and Kraft Apparatus Model S-25, available from SGA, Bloomfield,
NJ. 2°C. Maintain the temperature at 90 6 2°C for about 15 min to
7
Reagent Chemicals, American Chemical Society Specifications, American dissolve any wax in the crude.
Chemical Society, Washington, DC. For suggestions on the testing of reagents not 8.6 Start the vacuum pump and adjust the vacuum to 200
listed by the American Chemical Society, see Analar Standards for Laboratory
Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
mm Hg. Carefully pour the sample mixture into the filter
and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville, reservoir in three portions. Generally the sample should filter in
MD. 10 to 15 min. If the nature of the crude or the amount of

2
 D 4807
sediment causes the filtration to proceed extremely slowly (for 11. Precision and Bias
example, filtering times greater than 30 min), reduce the 11.1 Repeatability—The difference between successive test
sample size to 5 g or less and repeat the test. Keep the volume results, obtained by the same operator with the same apparatus
of toluene at 100 mL. under constant operating conditions on identical test material,
NOTE 5—If the filtration of a given crude typically takes less than 10 would in the long run, in the normal and correct operation of
min and the sample stays at 90 6 2°C during this time, then external test method, exceed the following values in only one case in
heating of the filter reservoir may not be necessary. twenty (see Table 1).
8.7 Before the last portion of sample has completely fil- 0.04388 ~X1 / 2! (2)
tered, wash the reservoir and filter with 50 mL of hot toluene
where X is sample mean
(90°C) until no oil is visible on the filter. With the vacuum on,
11.2 Reproducibility—The difference between two single
leave the filter on the apparatus for 2 min.
and independent results obtained by different operations work-
8.8 Disassemble the filter apparatus by removing the clamp
ing in different laboratories on identical test material would, in
and reservoir. Inspect the condition of the filter. If the filter has
the long run, in the normal and correct operation of the test
been properly mounted, it may not be necessary to wash the
method, exceed the following values only in one case in twenty
edges after disassembly. However, if upon removing the
(see Table 1).
reservoir dark spots are observed around the edge of the filter
further washing is necessary. With the vacuum on, use a 0.1176 ~X1 / 2! (3)
dropper to wash the filter’s edges with hot toluene (90°C). where X is sample mean
8.9 If the filter is completely or partially covered with black 11.3 Bias—The data generated during the development of
or dark brown crude oil residue after the washing step above, this test method showed that more sediment is recovered from
then discard the filter and repeat the test with a smaller sample crude oil using this test method compared to the results of Test
size. Method D 473.
NOTE 6—Normally the color of the sediment on the filter is gray or light 12. Keywords
tan. A black or deep brown colored deposit on the filter is indicative of
incomplete washing. 12.1 apparatus; crude oil; membrane filtration; procedure;
reagents; sampling; sediment
8.10 If the appearance of the filter is acceptable (as in 8.9)
then carefully remove it and place it in an oven at 105°C for 15 TABLE 1 Precision Intervals
min. Cool in a desiccator and reweigh to the nearest 0.0001 g. Mass Sediment Repeatability Reproducibility
0.0050 0.0031 0.0083
9. Calculation 0.0100 0.0044 0.0118
0.0150 0.0054 0.0144
9.1 Calculate the mass percent of sediment as follows: 0.0200 0.0062 0.0166
G 0.0250 0.0069 0.0186
Mass % 5 S 3 100 (1) 0.0300 0.0076 0.0204
0.0350 0.0082 0.0220
0.0400 0.0088 0.0235
where: 0.0450 0.0093 0.0249
G = gain in mass of filter, g, and 0.0500 0.0098 0.0263
S = sample mass, g, 0.0600 0.0107 0.0288
0.0700 0.0116 0.0311
0.0800 0.0124 0.0333
10. Report 0.0900 0.0132 0.0353
10.1 Report results to the nearest 0.001 % as the mass 0.1000 0.0139 0.0372
0.1250 0.0155 0.0416
percent of sediment by membrane filtration. The test report 0.1500 0.0170 0.0455
shall reference this Test Method D 4807 as the procedure used.

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 D 4807
ANNEX

(Mandatory Information)

A1. HOMOGENIZATION EFFICIENCY OF UNKNOWN MIXERS

A1.1 The homogenization efficiency of each unknown content 1 % above the base level found in A1.2. From a
mixer shall be evaluated before use. The grade of crude oil, the water-filled syringe previously weighed (nearest 0.1 mg), inject
sample size, and the sample container expected to be used with the water below the surface of the crude near the inlet to the
the mixer should be used in this test. The specifications of this mixer. Reweigh the syringe (to the nearest 0.1 mg) and
test should be met before running this test method and any determine the amount of water added. Any oil on the needle
changes in the mixing procedure should be re-evaluated by this should be wiped off before weighing. Mix the sample in the
test. The mixing efficiency is measured by following the water same manner as in A1.2. Determine the water content of the
content as described in Test Method D 4377. The crude oil used crude immediately after mixing. Sample the crude just below
in this test should be dry (less than 0.1 % water), otherwise the liquid level.
perform a preliminary distillation to remove the water as
described in Test Method D 2892. A1.4 Without additionally mixing the crude, determine the
water content of the crude 15 and 30 min after the initial
A1.2 Weigh the sample container to the nearest 0.01 g. Fill mixing in A1.3.
the container halfway (or the level normally used) with the dry
crude. Immerse the mixer into the crude with the bottom of the A1.5 Remix the sample in the same manner as A1.2.
mixer 5 mm above the bottom of the container and mix the Immediately after mixing, determine the water content in
crude at the speed and for the amount of time you expect to duplicate.
use. Suggested mixing time is between 1 and 5 min at 5 to 7000
r/min. Immediately determine the water content in duplicate A1.6 The water contents of the crude determined in A1.3,
(see Test Method D 4377) of the dry crude. Obtain the average A1.4, and A1.5 minus the base determined in A1.2 should
of the duplicate results. agree within 0.05 % absolute of the added water and to each
other. If they do not agree, this test should be repeated while
A1.3 Weigh the crude and container to the nearest 0.01 g. changing the mixing time, the mixing speed, or the height of
Immerse the mixer into the crude as in A1.2. Knowing the the mixer in the crude, or a combination thereof until these
weight of the crude, add enough water to increase the water conditions are met.

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