ASTM D4807-88(1999)

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An American National Standard
Designation:D4807–88(Reapproved 1999)
Designation: 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 (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
incrudeoilsbymembranefiltration.Thistestmethodhasbeen 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.
%.
5. Apparatus
1.2 This standard does not purport to address all of the
5.1 Reservoir and Filter Support Assembly—an assembly
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro- designed to hold 47-mm diameter filters was used in the
development of this test method (see Fig. 1).
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use. 5.1.1 Filter Reservoir—capable of holding from about 250
mL of solvent. The lower part of the reservoir has a 40-mm
1.3 The accepted unit of measure for this test method is
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
D473 Test Method for Sediment in Crude Oils and Fuel
electricity when filtering.
Oils by the Extraction Method
5.1.2 Filter Support/Funnel—support base for the filter has
D2892 Test Method for Distillation of Crude Petroleum
a porous scintered glass center section about 40 to 43 mm in
(15-Theoretical Plate Column)
diameter. The support base is designed to fit securely against
D4057 Practice for Manual Sampling of Petroleum and
thereservoirholdingthefilterinplaceovertheporoussection.
Petroleum Products
Thestemofthefunnelportionshouldbelongenoughtoextend
D4177 Practice for Automatic Sampling of Petroleum and
down into the filter flask such that the end is below the outlet
Petroleum Products
for the vacuum.
D4377 Test Method for Water in Crude Oils by Pontentio-
5.1.3 Clamp Assembly—spring or screw type clamp to
metric Karl Fischer Titration
secure the reservoir to the filter support. The clamp should be
tight enough to prevent the solvent from leaking through at the
3. Summary of Test Method
junction between the glass and filter membrane. The exterior
3.1 A portion of a representative crude oil sample is
dimensions of the reservoir and support/funnel are designed to
dissolved in hot toluene and filtered under vacuum through a
facilitate clamping the two pieces together.
0.45-µm porosity membrane filter. The filter with residue is
5.1.4 Rubber Stopper—asingle-hole,capableofholdingthe
washed, dried, and weighed to give the final result.
lower stem of the filter support/funnel securely onto the
filtering flask.
This test method is under the jurisdiction of ASTM Committee D-2 on
5.1.5 Vacuum Filtering Flask, 500 mL or larger.
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.
2 4
Annual Book of ASTM Standards, Vol 05.01. Afiltration assembly as supplied by Millipore Corp.,Ashly Rd., Bedford, MA
Annual Book of ASTM Standards, Vol 05.02. 01730, was found acceptable.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D4807
to place the sample into the laboratory test container. The
laboratory test container and sample volume shall be of
sufficientdimensionsandvolumetoallowmixingasdescribed
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 or D4177 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.
5.2 Membrane Filter, nylon membrane filter, 47 mm in
7.3.1 Mix the test sample of crude oil at room temperature
diameter with 0.45-µm pore size.
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.Atest 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
15-min interval mentioned above is a general guideline which may not
0.0001 g.
1 apply to all crudes, especially some light crudes which do not hold water
5.6 Heating Coil for Filter Assembly— copper tubing ( ⁄8-
in suspension for even this short a time.
in.diameter)woundaroundthereservoironthefilterapparatus
7.3.2 Mixingofthesampleshouldnotincreasethetempera-
and connected to a circulating bath to maintain the oil in the
ture of the sample more than 10°C, or a loss of water may
reservoir at 90 6 2°C (see Fig. 1). Alternative methods of
occur and this affects sample composition. The type of mixer
heating the reservoir such as heating tape or glass thermal
depends on the quantity of crude. Before any unknown mixer
jacket could also be used.
is used, the specifications for the homogenization test, Annex
5.7 Mixer —a nonaerating, high-speed mixer capable of
A,mustbemet.Themixermustbere-evaluatedfollowingany
meetingthehomogenizationefficiencytestinAnnexA1.Large
changes in the type of crude, quantity of crude, or shape of the
volume dynamic mixing systems such as those used with
sample container.
automatic crude oil sampling receptacles are also acceptable
7.3.3 For small test sample volumes, 50 to 300 mL, a
providing they comply with Annex A1.
nonaerating, high-speed, shear mixer is required. Use the
6. Reagents
mixingtime,mixingspeed,andheightabovethebottomofthe
container found to be satisfactory inAnnexA1. Clean and dry
6.1 Purity of Reagents—Reagent grade chemicals shall be
the mixer between samples.
used in all tests. Unless otherwise indicated, it is intended that
all reagents shall conform to the specifications of the Commit-
8. Procedure
tee onAnalytical Reagents of theAmerican Chemical Society,
8.1 Prepare nylon filters by heating in an oven at 105°C for
where such specifications are available. Other grades may be
15 min. Cool and store the dried filters in a desiccator (without
used, provided it is first ascertained that the reagent is of
desiccant) until needed. Use only new filters.
sufficiently high purity to permit its use without lessening the
8.2 Weigh the filter immediately before use to the nearest
accuracy of the determination.
0.0001 g.
6.2 Toluene (Warning, Flammable).
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
with a rubber stopper.Attach the reservoir to the filter support
7. Sampling, Test Specimens
and clamp it securely.
7.1 Sampling,isdefinedasallthestepsrequiredtoobtainan
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
temperature of the circulating bath so as to maintain the oil in
the reservoir at 90 6 2°C.
The following filter was used in generating the precision: MSI Nylon 60
Membrane Filter from Fisher Scientific, Catalog Number NO-4-SP047-00. Other
NOTE 4—Care sho
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