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: D473 − 22

Manual of Petroleum Measurement Standards (MPMS), Chapter 10.1

Standard Test Method for

Sediment in Crude Oils and Fuel Oils by the Extraction
Method1
This standard is issued under the fixed designation D473; 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* D4057 Practice for Manual Sampling of Petroleum and

1.1 This test method covers the determination of sediment Petroleum Products (API MPMS Chapter 8.1)
in crude oils and fuel oils by extraction with toluene. The D4175 Terminology Relating to Petroleum Products, Liquid
precision applies to a range of sediment levels from 0.01 % to Fuels, and Lubricants
0.40 % mass, although higher levels may be determined. D4177 Practice for Automatic Sampling of Petroleum and
Petroleum Products (API MPMS Chapter 8.2)
NOTE 1—Precision on recycled oils and crankcase oils is unknown and D5854 Practice for Mixing and Handling of Liquid Samples
additional testing is required to determine that precision.
of Petroleum and Petroleum Products (API MPMS Chap-
1.2 The values stated in SI units are to be regarded as ter 8.3)
standard. No other units of measurement are included in this E29 Practice for Using Significant Digits in Test Data to
standard. Determine Conformance with Specifications
1.3 This standard does not purport to address all of the 2.2 API Standards:3
safety concerns, if any, associated with its use. It is the Chapter 1 Terms and Definitions Database
responsibility of the user of this standard to establish appro- Chapter 8.1 Manual Sampling of Petroleum and Petroleum
priate safety, health, and environmental practices and deter- Products (ASTM Practice D4057)
mine the applicability of regulatory limitations prior to use. Chapter 8.2 Automatic Sampling of Petroleum and Petro-
For specific warning statements, see 6.1.1.6 and 7.1. leum Products (ASTM Practice D4177)
1.4 This international standard was developed in accor- Chapter 8.3 Mixing and Handling of Liquid Samples of
dance with internationally recognized principles on standard- Petroleum and Petroleum Products (ASTM Practice
ization established in the Decision on Principles for the D5854)
Development of International Standards, Guides and Recom- 2.3 ISO Standard:4
mendations issued by the World Trade Organization Technical 5272 Toluene for industrial use—Specifications
Barriers to Trade (TBT) Committee.
3. Terminology
2. Referenced Documents
3.1 For definitions of terms used in this standard test
2.1 ASTM Standards:2
method, refer to Terminology D4175 and the API MPMS
Chapter 1 Terms and Definitions Database.
1
This test method is under the jurisdiction of ASTM Committee D02 on 4. Summary of Test Method
Petroleum Products, Liquid Fuels, and Lubricants and the API Committee on
Petroleum Measurement, and is the direct responsibility of Subcommittee D02.02 4.1 Extract test portion of a representative oil sample,
/COMQ, the joint ASTM-API Committee on Hydrocarbon Measurement for contained in a refractory thimble, with hot toluene until the
Custody Transfer (Joint ASTM-API). This test method has been approved by the
sponsoring committees and accepted by the Cooperating Societies in accordance residue reaches constant mass. The mass of residue, calculated
with established procedures. as a percentage, is reported as sediment by extraction.
Current edition approved July 1, 2022. Published July 2022. Originally approved
in 1938. Last previous edition approved in 2017 as D473 – 07 (2017)ɛ1. DOI:
10.1520/D0473-22.
2 3
For referenced ASTM standards, visit the ASTM website, www.astm.org, or Available from American Petroleum Institute (API), 1220 L. St., NW,
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM Washington, DC 20005-4070, http://api-ec.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.

*A Summary of Changes section appears at the end of this standard

© 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

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 D473 − 22

NOTE 1—Apparatus B shows the water cup in position.

FIG. 1 Extraction Apparatus for Determination of Sediment

5. Significance and Use 6.1.1.3 Extraction Thimble5—The extraction thimble shall

5.1 A knowledge of the sediment content of crude oils and be of a refractory porous material, pore size 20.0 µm to
fuel oils is important both to the operation of refining and the 30.0 µm (as certified by the manufacturer), 25 mm in diameter
buying or selling of these commodities. by 70 mm in height, weighing not less than 15 g and not more
than 17 g. Suspend the thimble from the condenser coil by
6. Apparatus means of a basket so that it hangs approximately midway
between the surface of the extracting solvent and the bottom of
6.1 Usual laboratory apparatus and glassware, together with
the condenser coil.
the following are required for this test method.
6.1.1.4 Thimble Basket—The thimble basket shall be
6.1.1 Extraction Apparatus—Use the apparatus illustrated in
corrosion-resistant and shall be made of platinum, stainless
Figs. 1 and 2 and consisting of the elements described in
steel, nickel-chromium alloy, or similar material. Fig. 2 shows
6.1.1.1 – 6.1.1.3.
the design and dimensions of two typical baskets that have
6.1.1.1 Extraction Flask—Use a wide-neck (Erlenmeyer)
been used successfully in the industry.
flask of 1 L capacity, with a minimum external neck diameter
6.1.1.5 Water Cup—Use a water cup when testing a sample
of 50 mm, for the procedure.
determined to have a water content greater than 10 % volume
6.1.1.2 Condenser—A condenser in the form of a metal coil
(see Fig. 1, Apparatus B). The cup shall be made of glass,
approximately 25 mm in diameter and 50 mm in length at-
conical in shape, approximately 20 mm in diameter and 25 mm
tached to, and with the ends projecting through, a lid of
deep, and have a capacity of approximately 3 mL. A glass hook
sufficient diameter to cover the neck of the flask as shown in
fused on the rim at one side is so shaped that when hung on the
Fig. 1. The coil shall be made from stainless steel, tin,
condenser the cup hangs with its rim reasonably level. In this
tin-plated copper, or tin-plated brass tubing having an outside
procedure, suspend the thimble basket as shown in Fig. 1,
diameter of 5 mm to 8 mm and a wall thickness of 1.5 mm. If
Apparatus A by means of the corrosion-resistant wire looped
constructed of tin-plated copper or brass, the tin coating shall
have a minimum thickness of 0.075 mm. The exposed surface
of the coil for cooling purposes is about 115 cm2.
5
The sole source of supply of the extraction thimble, AN 485, 25 mm × 70 mm,
NOTE 2—The use of a water flowmeter/controller unit that monitors coarse porosity, drawing number QA 005163, known to the committee at this time
water flow to the condenser that shuts off the heat source when the flow is Saint-Gobain/Norton Industrial Ceramics Corporation of Worcester, MA. If you
rate drops below a pre-set limit has been found suitable to prevent are aware of alternative suppliers, please provide this information to ASTM
vaporized toluene from igniting. The use of such a device is recom- International Headquarters. Your comments will receive careful consideration at a
mended. meeting of the responsible technical committee,1 which you may attend.

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 D473 − 22

FIG. 2 Basket Thimble Support

over the bottom of the condenser coil and attached to the basket 6.3 Non-aerating Mixer—Use a non-aerating mixer, meet-
supports, or as in Fig. 1, Apparatus B, where the wire supports ing the verification of mixing efficiency requirements specified
of the basket are attached to hooks soldered to the underside of in Practice D5854 (API Chapter 8.3). Either insertion mixers or
the condenser lid. circulating mixers or circulating external mixers are acceptable
6.1.1.6 Source of Heat—Use a source of heat, preferably a provided they meet the criteria in Practice D5854 (API Chapter
hot plate operated under a ventilated hood, suitable for vapor- 8.3).
izing toluene (Warning—Flammable.)
6.4 Oven—Use an oven capable of maintaining a tempera-
6.2 Analytical Balance—Use an analytical balance, with an ture of 115 °C to 120 °C (240 °F to 250 °F).
accuracy of 0.1 mg. Verify the balance, at least annually,
against weights traceable to a national standards body such as 6.5 Cooling Vessel—Use a desiccator without desiccant as a
the National Institute of Standards and Technology (NIST). cooling vessel.

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 D473 − 22
TABLE 1 Typical Characteristics for ACS Reagent Grade Toluene in temperature during mixing exceeds 10 °C (20 °F), cool the
Assay 99.5+ % sample, and repeat the mixing at a lower energy input. A rise in
Color (APHA) 10 temperature greater than 10 °C (20 °F) may result in a decrease
Boiling range (initial to dry point)A 2.0 °C
Residue after evaporation 0.001 % in viscosity that is sufficient for the sediment to settle.
Substances darkened by H2SO4 passes test
Sulfur compounds (as S) 0.003 % 9. Procedure
Water (H2O) (by Karl Fischer titration) 0.03 %
9.1 For referee tests, use a new extraction thimble (6.1.1.3)
A
Recorded boiling point 110.6 °C. prepared in accordance with 9.2. For routine tests, thimbles
may be reused. When reusing thimbles, the extraction to
constant mass for one determination should be considered as
6.6 Temperature Measuring Device—Such as a the preliminary extraction for the succeeding determination.
thermometer, capable of measuring the temperature of the After several determinations (the accumulated sediment may
sample to the nearest 1 °C (2 °F). be sufficient to interfere with further determinations), follow
the procedure described in 9.3 to remove the combustible
7. Solvent portion of the accumulated sediment. Avoid excessive reuse of
7.1 Toluene—Reagent grade conforming to the specifica- thimbles, as over time the pores become clogged with inor-
tions of the Committee on Analytical Reagents of the American ganic material resulting in falsely high results. When in doubt
Chemical Society (ACS)6 or to Grade 2 of ISO 5272. regarding a higher than normal result, discard the thimble and
(Warning—Flammable. Keep away from heat, sparks and retest using a new thimble.
open flame. Vapor harmful. Toluene is toxic. Particular care 9.2 Preparation of a New Thimble—Rub the outside surface
shall be taken to avoid breathing the vapors and to protect the with fine sandpaper and remove all loosened material with a
eyes. Keep the container closed. Use with adequate ventilation. stiff brush. Give the thimble a preliminary extraction with the
Avoid prolonged or repeated contact with the skin.) toluene, allowing the solvent to drip from the thimble for at
7.1.1 The typical characteristics for the ACS reagent are least 1 h. Then dry the thimble for 1 h at a temperature of
shown in Table 1. 115 °C to 120 °C (240 °F to 250 °F); cool in a cooling vessel,
for 1 h, and weigh to the nearest 0.1 mg. Repeat the extraction
8. Sampling until the masses of the thimble after two successive extractions
8.1 Sampling shall include all steps required to obtain an do not differ by more than 0.2 mg.
aliquot of the contents of any pipe, tank, or other system and to 9.3 Preparation of a Used Thimble—Remove the combus-
place the sample into the laboratory test container. tible portion of the accumulated sediment by heating the
8.2 Only use representative samples obtained as specified in thimble to a dull red heat for 20 min (preferably in an electric
Practices D4057 (API Chapter 8.1) and D4177 (API Chapter furnace maintained at approximately 750 °C (1380 °F)). Sub-
8.2) for this test method. ject the thimble to a preliminary extraction as described in 9.2
before using it for another determination.
8.3 Draw test portions from the laboratory samples imme-
diately after thorough mixing. Heat viscous samples to a 9.4 Place an estimated 10 g test portion of the sample in the
temperature which renders the sample liquid, and homogenize thimble immediately after the sample has been mixed. Do not
using a mixer as described in 6.3, as necessary. The difficulties attempt to adjust this estimated 10 g portion to any exact
of obtaining a representative test portion for this determination predetermined amount. Weigh the thimble plus test portion to
are usually great, hence the need for great attention to the the nearest 0.01 g. Add 150 mL to 200 mL of toluene to the
mixing and aliquoting steps. flask. Place the thimble in the extraction apparatus, place on the
heat source, and extract with the hot toluene for 30 min after
8.4 As specified in Practice D5854 (API Chapter 8.3),
the solvent dripping from the thimble becomes colorless.
record the temperature of the sample before mixing. Mix the
Ensure that the rate of extraction is such that the surface of the
laboratory sample in its original container, using the mixing
mixture of oil and toluene in the thimble does not rise higher
time, mixing power (speed), and position relative to the bottom
than to within 20 mm of the top.
of the container appropriate to the crude petroleum or fuel oil
being analyzed, and as established by the verification of mixing 9.5 When testing samples determined to have a water
efficiency. To avoid the loss of light ends from crude oil or content greater than 10 % volume, use the assembly shown in
other samples containing volatile material, operate the mixer Fig. 1, Apparatus B. In this procedure, remove any water in the
through a gland in the closure of the sample container. Take the test portion as its toluene azeotrope and is collected in the
test portion for analysis immediately after mixing. Record the water cup, where it separates as a bottom layer. The toluene
temperature of the sample immediately after mixing. If the rise layer overflows into the thimble. If the cup becomes full of
water, allow the apparatus to cool and empty the cup.
6
ACS Reagent Chemicals, Specifications and Procedures for Reagents and
9.6 After the extraction is completed, dry the thimble for 1 h
Standard-Grade Reference Materials, American Chemical Society, Washington, at 115 °C to 120 °C (240 °F to 250 °F) in the oven; cool in the
DC. For suggestions on the testing of reagents not listed by the American Chemical cooling vessel, for 1 h; and weigh to the nearest 0.1 mg.
Society, see Analar Standards for Laboratory Chemicals, BDH Ltd., Poole, Dorset,
U.K., and the United States Pharmacopeia and National Formulary, U.S. Pharma- 9.7 Repeat the extraction, allowing the solvent to drip from
copeial Convention, Inc. (USPC), Rockville, MD. the thimble for at least 1 h but not longer than 1.25 h; dry, cool,

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 D473 − 22
and weigh the thimble as described in 9.6. Repeat this D5854 (API Chapter 8.3). Report the temperature of the
extraction for further 1 h periods, if necessary, until the masses sample before and after mixing.
of the dried thimble plus sediment after two successive 11.3 The test report shall also contain all details necessary
extractions do not differ by more than 0.2 mg. for complete identification of the product tested; any deviation,
by agreement or otherwise, from the procedure specified; and
10. Calculation the date of the test.
10.1 Calculate the sediment content of the sample as a
percentage by mass of the original sample. 12. Precision and Bias
m3 2 m1
12.1 Precision—The precision of the test method, as based
S5
m2 2 m1
3 100 (1) on mass percent and as obtained by statistical examination of
interlaboratory test results in the range 0 % to 0.4 %, is
where: described in 12.1.1 and 12.1.2.
S = sediment content of the sample as a percentage by 12.1.1 Repeatability—The difference between successive
mass, test results, obtained by the same operator with the same
m1 = mass, of the thimble, g, apparatus under constant operating conditions on identical test
m2 = mass, of the thimble plus test portion, g, and material, would, in the long run, in the normal and correct
m3 = mass of the thimble plus sediment, g. operation of the test method, exceed the following value in
only one case in twenty:
11. Report
r 5 0.01710.255 S (3)
11.1 For each sample with a calculated sediment content
>0.005 % m/m as determined by Eq 1, report the sediment where:
content of the sample, as sediment by extraction, as a percent- r = repeatability of the test, and
age by mass, rounded to the nearest 0.01 % m/m following S = average result, as a percentage by mass, of the values
Practice E29 rounding conventions. For each sample with a being compared.
calculated sediment content ≤0.005 % m/m as determined in 12.1.2 Reproducibility—The difference between two single
Eq 1, report as, “0 % m/m.” The test result shall reference Test and independent test results obtained by different operators
Method D473/API MPMS Chapter 10.1 as the procedure used. working in different laboratories on identical test material,
NOTE 3—Since water and sediment values are commonly reported as would, in the long run, in the normal and correct operation of
volume percent, calculate the volume of the sediment as a percentage of the test method, exceed the following value in only one case in
the original sample. As a major portion of the sediment probably would be twenty:
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 R 5 0.03310.255 S (4)
of sand), use an arbitrary density of 2.0 for the resulting sediment. Then, where:
to obtain volume percent sediment, divide the mass percent sediment by
2.0 and multiply by the relative density of the crude or fuel oil. R = reproducibility of the test, and
S = average result, as a percentage by mass, of the values
S
Sv 5 3 relative density of the oil (2) being compared.
2.0
12.2 Bias—The procedure in this test method has no bias
where: because the value of sediment can be defined only in terms of
Sv = sediment content of the sample as a percentage by volume, and a test method.
S = sediment content of the sample as a percentage by mass.
11.2 Report that the sample mixing procedure was per- 13. Keywords
formed in accordance with the procedures specified in Practice 13.1 crude oil; extraction; fuel oil; sampling; sediment

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 D473 − 22

ANNEX

(Mandatory Information)

A1. WARNING INFORMATION

A1.1 Toluene A1.1.5 Keep container closed.

A1.1.1 Keep away from heat, sparks, and open flame. A1.1.6 Use with adequate ventilation.
A1.1.2 Vapor harmful.
A1.1.7 Avoid prolonged or repeated contact with the skin.
A1.1.3 Toluene is toxic.
A1.1.4 Particular care must be taken to avoid breathing the
vapor and to protect the eyes.

SUMMARY OF CHANGES

Subcommittee D02.02 has identified the location of selected changes to this standard since the last issue
(D473 – 07 (2017)ɛ1) that may impact the use of this standard. (Approved July 1, 2022.)

(1) Added Terminology D4175 and the API MPMS Chapter 1 (2) Added Section 3 on Terminology.
to Section 2.

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make your views known to the ASTM Committee on Standards, at the address shown below.

This standard is jointly copyrighted by ASTM International (ASTM), 100 Barr Harbor Drive, PO Box C700, West Conshohocken,
PA 19428-2959, United States, and the American Petroleum Institute (API), 1220 L Street NW, Washington DC 20005, United States.
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