ASTM D1796-04(2009)
(Test Method)Standard Test Method for Water and Sediment in Fuel Oils by the Centrifuge Method (Laboratory Procedure)
Standard Test Method for Water and Sediment in Fuel Oils by the Centrifuge Method (Laboratory Procedure)
SIGNIFICANCE AND USE
The water and sediment content of fuel oil is significant because it can cause corrosion of equipment and problems in processing. A determination of water and sediment content is required to measure accurately net volumes of actual fuel oil in sales, taxation, exchanges, and custody transfers.
SCOPE
1.1 This test method describes the laboratory determination of water and sediment in fuel oils in the range from 0 to 30 % volume by means of the centrifuge procedure.
Note 1—With some types of fuel oils such as residual fuel oils or distillate fuel oils containing residual components, it is difficult to obtain water or sediment contents with this test method. When this situation is encountered, Test Method D 95 (API MPMS Chapter 10.5) or Test Method D 473 (API MPMS Chapter 10.1) may be used.
Note 2—API MPMS Chapter 10.6 (Test Method D 1796) along with API MPMS Chapter 10.3 (Test Method D 4007) formerly superseded API Standard 2548.
1.2 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.
1.3 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 a specific precautionary statement, see 6.1.
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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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Designation:D1796–04 (Reapproved 2009)
Designation: Manual of Petroleum Measurement Standards (MPMS), Chapter 10.6
Standard Test Method for
Water and Sediment in Fuel Oils by the Centrifuge Method
(Laboratory Procedure)
This standard is issued under the fixed designation D1796; 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 Department of Defense.
1. Scope* D95 Test Method for Water in Petroleum Products and
Bituminous Materials by Distillation
1.1 This test method describes the laboratory determination
D473 TestMethodforSedimentinCrudeOilsandFuelOils
of water and sediment in fuel oils in the range from 0 to 30 %
by the Extraction Method
volume by means of the centrifuge procedure.
D4007 TestMethodforWaterandSedimentinCrudeOilby
NOTE 1—With some types of fuel oils such as residual fuel oils or
the Centrifuge Method (Laboratory Procedure)
distillate fuel oils containing residual components, it is difficult to obtain
D4057 Practice for Manual Sampling of Petroleum and
water or sediment contents with this test method. When this situation is
Petroleum Products
encountered,Test Method D95 (API MPMS Chapter 10.5) orTest Method
D4177 Practice for Automatic Sampling of Petroleum and
D473 (API MPMS Chapter 10.1) may be used.
Petroleum Products
NOTE 2—API MPMS Chapter 10.6 (Test Method D1796) along with
API MPMS Chapter 10.3 (Test Method D4007) formerly superseded API
D5854 PracticeforMixingandHandlingofLiquidSamples
Standard 2548.
of Petroleum and Petroleum Products
E542 Practice for Calibration of Laboratory Volumetric
1.2 The values stated in SI units are to be regarded as the
Apparatus
standard. The values given in parentheses are for information
2.2 API Standards:
only.
MPMS Chapter 8.1 Practice for Manual Sampling of Petro-
1.3 This standard does not purport to address all of the
leum and Petroleum Products (ASTM Practice D4057)
safety concerns, if any, associated with its use. It is the
MPMS Chapter 8.2 Practice for Automatic Sampling of
responsibility of the user of this standard to establish appro-
Petroleum and Petroleum Products (ASTM Practice
priate safety and health practices and determine the applica-
D4177)
bility of regulatory limitations prior to use. For a specific
MPMS Chapter 8.3 Practice for Mixing and Handling of
precautionary statement, see 6.1.
Liquid Samples of Petroleum and Petroleum Products
2. Referenced Documents
(ASTM Practice D5854)
2.1 ASTM Standards: MPMS Chapter 10.1 Test Method for Sediment in Crude
Oils by the Extraction Method (ASTM Test Method
D473)
MPMSChapter10.3 TestMethodforWaterandSedimentin
This test method is under the jurisdiction of ASTM Committee D02 on
Crude Oil by the Centrifuge Method (Laboratory Proce-
Petroleum Products and Lubricants and theAPI Committee on Petroleum Measure-
dure) (ASTM Test Method D4007)
ment, and is the direct responsibility of Subcommittee D02.02.10 on Sediment and
Water (API MPMS Chapter 10.0).
MPMS Chapter 10.5 Test Method for Water in Petroleum
Current edition approved April 15, 2009. Published July 2009. Originally
Products and Bituminous Materials by Distillation
approved in 1960. Last previous edition approved in 2004 as D1796–04. DOI:
(ASTM Test Method D95)
10.1520/D1796-04R09.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Standards volume information, refer to the standard’s Document Summary page on Published as Manual of Petroleum Measurement Standards.Available from the
the ASTM website. American Petroleum Institute, 1220 L St., N.W., Washington, DC 20005.
*A Summary of Changes section appears at the end of this standard.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D1796–04 (2009)
2.3 IP Standard:
r/min 5 265 =rcf/d (2)
Methods Book, Appendix B Specification for Methylben-
where:
zenes (Toluenes)
rcf = relative centrifugal force, and
2.4 ISO Standard:
d = diameter of swing measured between tips of opposite
ISO 5272:1979 Toluene for Industrial Use—Specifications
tubes when in rotating position, in.
5.1.6 Calculate the relative centrifugal force from a mea-
3. Summary of Test Method
sured speed (r/min) as follows:
3.1 Equal volumes of fuel oil and water-saturated toluene
r/min
are placed in each of two cone-shaped centrifuge tubes. After
rcf 5 d (3)
S D
centrifugation, the volume of the higher density water and
sediment layer at the bottom of the tube is read.
where:
d = diameter of swing measured between tips of opposite
4. Significance and Use
tubes when in rotating position, mm, or
4.1 The water and sediment content of fuel oil is significant
r/min
because it can cause corrosion of equipment and problems in
rcf 5 d (4)
S D
processing. A determination of water and sediment content is
required to measure accurately net volumes of actual fuel oil in
where:
sales, taxation, exchanges, and custody transfers. d = diameter of swing measured between tips of opposite
tubes when in rotating position, in.
5. Apparatus
5.2 Centrifuge Tubes:
5.1 Centrifuge:
5.2.1 Each centrifuge tube shall be a cone-shaped tube,
5.1.1 Use a centrifuge capable of spinning two or more
conforming to the dimensions given in Fig. 1, and made of
filled cone-shaped 203-mm (8-in.) centrifuge tubes at a speed
thoroughly annealed glass. The graduations, numbered as
that can be controlled to give a relative centrifugal force (rcf)
shown in Fig. 1, shall be clear and distinct, and the mouth shall
of between 500 and 800 at the tip of the tubes (see 5.1.6).
be constricted in shape for closure with a cork or solvent-
5.1.2 Therevolvinghead,trunnionrings,andtrunnioncups,
resistant rubber stopper. Scale error tolerances and the smallest
including the cushions, shall be soundly constructed to with-
graduations between various calibration marks are given in
stand the maximum centrifugal force capable of being deliv-
Table 1 and apply to calibrations made with air-free water at
eredbythepowersource.Thetrunnioncupsandcushionsshall
20°C (68°F), when reading the bottom of the shaded meniscus.
firmly support the tubes when the centrifuge is in motion. The
5.2.2 Volumetrically verify or gravimetrically certify the
centrifuge shall be enclosed by a metal shield or case strong
accuracy of the graduation marks, in accordance with Practice
enough to eliminate danger if any breakage occurs.
E542 using equipment traceable through the National Institute
5.1.3 The centrifuge shall be heated and controlled thermo-
statically to avoid unsafe conditions. It shall be capable of
maintainingthesampletemperatureduringtheentireprocessat
60 6 1°C (140 6 1.8°F). The thermostatic control shall be
capable of maintaining the temperature within these limits and
operate safely if there is a flammable atmosphere.
5.1.4 Electric powered and heated centrifuges must meet all
safety requirements for use in hazardous areas.
NOTE 3—Some heated centrifuges maintain the bowl at a pressure
slightly below atmospheric pressure and reduce the hazards associated
with vapors and gasses, produced by samples and solvents used in the
tests, by discharging any vapors to a non-hazardous area.
5.1.5 Calculate the speed of the rotating head in revolutions
per minute (r/min) as follows:
r/min 5 1335 rcf/d (1)
=
where:
rcf = relative centrifugal force, and
d = diameter of swing measured between tips of opposite
tubes when in rotating position, mm,
or
Available from Energy Institute, 61 New Cavendish St., London, WIG 7AR,
U.K.
Available fromAmerican National Standards Institute (ANSI), 25 W. 43rd St.,
4th Floor, New York, NY 10036. FIG. 1 Eight-Inch (203-mm) Centrifuge Tube
D1796–04 (2009)
TABLE 1 Centrifuge Tube Calibration Tolerances for
clinging to the walls of the centrifuge tube, and to enhance the
203-mm (8-in.) Tube
distinctness of the water-oil interface.
Range, mL Subdivision, mL Volume Tolerance, mL
6.2.2 When using a demulsifier, it should be mixed accord-
0to0.1 0.05 60.02
ing to the manufacturer’s recommendations and should never
Above 0.1 to 0.3 0.05 60.03
be added to the volume of sediment and water determined.
Above 0.3 to 0.5 0.05 60.05
Alwaysusethedemulsifierintheformofademulsifier-solvent
Above 0.5 to 1.0 0.10 60.05
Above 1.0 to 2.0 0.10 60.10 stocksolutionorbepremixedwiththesolventtobeusedinthe
Above 2.0 to 3.0 0.20 60.10
test.
Above 3.0 to 5.0 0.50 60.20
Above 5.0 to 10 1.00 60.50
7. Sampling
Above 10 to 25 5.00 61.00
Above 25 to 100 25.00 61.00
7.1 Sampling is defined as all steps required to obtain an
aliquot of the contents of any pipe, tank, or other system and to
place them into the laboratory test container.
7.2 Only representative samples obtained as specified in
for Standards and Technology (NIST) or other national
Practice D4057 (API MPMS Chapter 8.1) and Practice D4177
standards. Include the verification or certification for each
(API MPMS Chapter 8.2) shall be used for this test method.
mark through the 0.5-mL mark; of the 1, 1.5 and 2-mL marks;
7.3 Practice D5854 (API MPMS Chapter 8.3) contains
and of the 50 and 100-mL marks. Do not use the tube if the
additional information on sampling and homogenization effi-
scale error exceeds the applicable tolerance in Table 1.
ciency of an untested mixer. Do not use this test method
5.3 Bath—The bath shall be either a solid metal block bath
without strict adherence to Practice D5854 (API MPMS
or a liquid bath of sufficient depth for immersing the centrifuge
Chapter 8.3).
tube in the vertical position to the 100-mL mark. Provide the
means for maintaining the temperature at 60 6 1°C (140 6
8. Procedure
1.8°F). See Note 4.
8.1 Fill each of two centrifuge tubes (5.2) to the 50-mL
NOTE 4—It has been observed for some fuel oils that temperatures
mark with the well-mixed sample directly from the sample
higher than 60°C (140°F) may be required to obtain correct sediment and
container. Using a pipette, add 50 mL of the water-saturated
water content. If temperatures higher than 60°C are necessary, they may
solvent (6.1). Read the top of the meniscus at both the 50 and
be used only with the consent of the parties involved. Water saturation of
100 mL marks. Stopper the tubes tightly and shake vigorously
toluene may also be carried out at this higher testing temperature. (See
until the contents are thoroughly mixed. Loosen the stoppers
Annex A1.)
on the tubes and immerse the tubes to the 100-mL mark for
6. Reagents
10 min in the bath maintained at 60 6 1°C (140 6 1.8°F).
8.2 Tighten the stoppers and again invert the tubes to ensure
6.1 Toluene, conforming to the IP Specification for Methyl-
that the oil and solvent are uniformly mixed and shake
benzenes (Toluenes) or to ISO 5272. (Warning—Flammable.
cautiously. (Warning—In general, the vapor pressures of
Keep away from heat, sparks, and open flame. Vapor harmful.
hydrocarbons at 60°C (140°F) are approximately double those
Toluene is toxic. Particular care must be taken to avoid
at 40°C (104°F). Consequently, invert the tubes at a position
breathing the vapor and to protect the eyes. Keep container
below eye level so that contact will be avoided if the stopper is
closed. Use with adequate ventilation. Avoid prolonged or
blown out.)
repeated contact with the skin.)
8.3 Place the tubes in the trunnion cups on opposite sides of
6.1.1 Typical characteristics for this reagent are:
the centrifuge to establish a balanced condition and ensure that
Molecular weight C H CH 92.14
6 5 3
Color (APHA) 10 the tubes and stoppers do not touch adjacent or opposite tubes
A
Boiling range (initial to dry point) 2.0°C (3.6°F)
when in the extended position. Spin for 10 min at a rate,
Residue after evaporation 0.001 %
calculated from the equation given in 5.1.6, sufficient to
Substances darkened by H SO passes ACS test
2 4
Sulfur compounds (as S) 0.003 % produce a relative centrifugal force (rcf) of between 500 and
800 at the tip of the whirling tubes (see Table 2 for the
A
Recorded boiling point 110.6°C.
relationship between diameter of swing, relative centrifugal
NOTE 5—Some oils may require other solvents or solvent-demulsifier
force,andrevolutionsperminute).Maintainthetemperatureof
combinations. Those agreed upon between the purchaser and the seller
the sample during the entire centrifuging procedure at 60 6
may be used.
1°C (140 6 1.8°F). (See Note 4.)
6.1.2 The solvent shall be water-saturated at 60 6 1°C (140
8.4 Immediatelyafterthecentrifugecomestorestfollowing
6 1.8°F) but shall be free of suspended water. See Annex A1 the spin (ensure the tubes are immediately brought to a vertical
for the solvent-water saturation procedure.
position after the centrifuge stops because the results may be
6.2 Demulsifiers: affected if the tubes come to rest at an angle), read and record
6.2.1 Where necessary, use a demulsifier to promote the
the combined volume of water and sediment at the bottom of
separation of water from the sample, to prevent water from
each tube to the nearest 0.05 mLfrom 0.1 to 1-mLgraduations
and to the nearest 0.1 mL above the 1-mL graduations. Below
0.1 mL, estimate to the nearest 0.025 mL (see Fig. 2). If less
than 0.025 mL of water and sediment is visible and it is not a
Available from National Institute of Standards and Technology (NIST), 100
Bureau Dr., Stop 3460, Gaithersburg, MD 20899-3460. great enough volume to be considered 0.025 mL, record the
D1796–04 (2009)
TABLE 2 Rotation Speeds Applicable for Centrifuges of Various TABLE 3 Expression of Results, mL
Diameters of Swing
Tube 1—Volume of water Tube 2—Volume of Total Percent Water and
and sediment, mL water and sediment, Sediment, % (V/V)
NOTE—rcf = relative centrifugal force.
mL
Diameter of Swing Revolutions per Minute
No visible water No visible water 0.00
A
Millimetres Inches At 500 rcf At 800 rcf and sediment and sediment
No visible water 0.025 0.025
305 12 1710 2170
and sediment
330 13 1650 2010
0.025 0.025 0.05
356 14 1590 2000
0.025 0.05 0.075
381 15 1530 1930
0.05 0.05 0.10
406 16 1490 1870
0.05 0.075 0.125
432 17 1440 1820
0.075 0.075 0.15
457 18 1400 1770
0.075 0.10 0.175
483 19 1360 1720
0.10 0.10 0.20
508 20 1330 1680
0.10 0.15 0.25
533 21 1300 1640
559 22 1270 1600
584 23 1240 1560
610 24 1210 1530
A
For this column, the diameter of swing is measured in inches between tips of 10.2.1 Above 2.00 V/V, round to the nearest 0.1 % V/V.
op
...
This document is not anASTM standard and is intended only to provide the user of anASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
An American National Standard
Designation:D1796–97 (Reapproved 2002) Designation:D1796–04 (Reapproved 2009)
Designation: Manual of Petroleum Measurement Standards (MPMS), Chapter 10.6
Designation: 75/82
Standard Test Method for
Water and Sediment in Fuel Oils by the Centrifuge Method
(Laboratory Procedure)
This standard is issued under the fixed designation D 1796; 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 Department of Defense.
1. Scope
1.1Thistestmethodcoversthelaboratorytestfordeterminationofwaterandsedimentinfueloilsbyusingthecentrifugemethod
in the range from 0 to 30% volume. This chapter, along withAPI MPMS Chapter 10.3 (Test Method D4007, IP 359), supersedes
the previous edition of Test Method D1796 (API Standard D2548, IP75). *
1.1 This test method describes the laboratory determination of water and sediment in fuel oils in the range from 0 to 30 %
volume by means of the centrifuge procedure.
NOTE 1—With some types of fuel oils such as residual fuel oils or distillate fuel oils containing residual components, it is difficult to obtain water or
sediment contents with this test method. When this situation is encountered, Test Method D 95 (API MPMS Chapter 10.5) or Test Method D 473(API
MPMS Chapter 10.1) may be used.
1.2Annex A2 contains a procedure for saturating toluene with water.
1.3The values stated in SI units are to be regarded as the standard. The values in parentheses are for information only.
1.4Chapter 10.1) may be used.
NOTE 2—API MPMS Chapter 10.6 (Test Method D 1796) along with API MPMS Chapter 10.3 (Test Method D 4007) formerly superseded API
Standard 2548.
1.2 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.
1.3 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 a specific precautionary statement, see 6.1.
2. Referenced Documents
2.1 ASTM Standards:
D95 Test Method for Water in Petroleum Products and Bituminous Materials by Distillation (API MPMS Chapter 10.5)
D362Specification for Industrial Grade Toluene
D 473 Test Method for Sediment in Crude Oils and Fuel Oils by the Extraction Method (API MPMS Chapter 10.1)
D4006Test Method for Water in Crude Oil by Distillation (API MPMS Chapter 10.2)
D 4007 Test Method for Water and Sediment in Crude Oil by the Centrifuge Method (Laboratory Procedure) (API MPMS
Chapter 10.3)
D 4057 Practice for Manual Sampling of Petroleum and Petroleum Products (API MPMS Chapter 8.1)
This test method is under the jurisdiction of ASTM Committee D02 on Petroleum Products and Lubricants and the API Committee on Petroleum Measurement, and is
the direct responsibility of Subcommittee D02.02.0B /COMQ, the joint ASTM-API committee on Static Petroleum Measurement.Sampling, Sediment, Water.
Current edition approved Dec. 10, 2002.April 15, 2009. Published March 2003.July 2009. Originally approved in 1960. Last previous edition approved in 19972004 as
´1
D1796–97 .D 1796–04.
Annual Book of ASTM Standards, Vol 05.01.
For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at service@astm.org. For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
*A Summary of Changes section appears at the end of this standard.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D1796–04 (2009)
Practice for Manual Sampling of Petroleum and Petroleum Products
D 4177 Practice for Automatic Sampling of Petroleum and Petroleum Products (API MPMS Chapter 8.2)
Practice for Automatic Sampling of Petroleum and Petroleum Products
D4377Test Method for Water in Crude Oils by Potentiometric Karl Fischer Titration (API MPMS Chapter 10.7)
D4928Test Method for Water in Crude Oils by Coulometric Karl Fischer Titration (API MPMS Chapter 10.9)
D 5854 Practice for Mixing and Handling of Liquid Samples of Petroleum and Petroleum Products (API MPMS Chapter 8.3)
E 542 Practice for Calibration of Laboratory Volumetric Apparatus
2.2 API Standards:
MPMS Chapter 8.1 Practice for Manual Sampling of Petroleum and Petroleum Products (ASTM Practice D 4057)
MPMS Chapter 8.2 Practice for Automatic Sampling of Petroleum and Petroleum Products (ASTM Practice D 4177)
MPMSChapter8.3 PracticeforMixingandHandlingofLiquidSamplesofPetroleumandPetroleumProducts(ASTMPractice
D 5854)
MPMS Chapter 10.1Determination of Test Method for Sediment in Crude Oils by the Extraction Method (ASTM Test Method
D 473)
MPMS Chapter 10.2Determination of Water in Crude Oil by the Distillation Method (ASTM Test Method D4006Chapter
10.3 Test Method for Water and Sediment in Crude Oil by the Centrifuge Method (Laboratory Procedure) (ASTM Test
Method D 4007)
MPMS Chapter 10.3 Determination of Water and Sediment in Crude Oils by the Centrifuge Method (Laboratory Procedure)
(ASTM Test Method D4007)
MPMS Chapter 10.5Determination of Water in Petroleum Products and Other Bituminous Materials (ASTM Test Method D95)
MPMS Chapter 10.7 Determination of Water in Crude Oils (Karl Fischer) Titration (ASTM Test Method D4377)
MPMS Chapter 10.9Determination of Water in Crude Oils Coulometric Karl Fischer Titration (ASTM Test Method D4928)
Test Method for Water in Petroleum Products and Bituminous Materials by Distillation (ASTM Test Method D 95)
Discontinued—See 1988 Annual Book of ASTM Standards, Vol 06.03.
Published as Manual of Petroleum Measurement Standards. Available from the American Petroleum Institute, 1220 L St., N.W., Washington, DC 20005.
D1796–04 (2009)
2.3 IP Standard:
Specification for Toluol IP Standard:
Methods Book, Appendix B Specification for Methylbenzenes (Toluenes)
2.4 ISO Standard:
ISO 5272:1979 Toluene for Industrial Use—Specifications
3. Summary of Test Method
3.1 Equal volumes of fuel oil and water-saturated toluene are placed in each of two cone-shaped centrifuge tubes. After
centrifugation, the volume of the higher gravitydensity water and sediment layer at the bottom of the tube is read.
4. Significance and Use
4.1 The water and sediment content of fuel oil is signifi-cant because it can cause corrosion of equipment and problems in
processing. The A determination of water and sediment content must be knownis required to measure accurately net volumes of
actual fuel oil in sales, taxation, exchanges, and custody transfers.
5. Apparatus
5.1 Centrifuge:
5.1.1A 5.1.1 Use a centrifuge capable of spinning two or more filled cone-shaped 203-mm (8-in.) centrifuge tubes at a speed
whichthat can be controlled to give a relative centrifugal force (rcf) of between 500 and 800 at the tip of the tubes shall be used.
(see 5.1.6).
5.1.2 The revolving head, trunnion rings, and trunnion cups, including the cushions, shall be soundly constructed to withstand
the maximum centrifugal force capable of being delivered by the power source. The trunnion cups and cushions shall firmly
support the tubes when the centrifuge is in motion. The centrifuge shall be enclosed by a metal shield or case strong enough to
eliminate danger if any breakage occurs.
5.1.3Calculate the speed of the rotating head in revolutions per minute (rpm) as follows:
5.1.3 The centrifuge shall be heated and controlled thermostatically to avoid unsafe conditions. It shall be capable of
maintainingthesampletemperatureduringtheentireprocessat60 61°C(140 61.8°F).Thethermostaticcontrolshallbecapable
of maintaining the temperature within these limits and operate safely if there is a flammable atmosphere.
Annual Book of ASTM Standards, Vol 05.02.
Available from Energy Institute, 61 New Cavendish St., London, WIG 7AR, U.K.
Annual Book of ASTM Standards, Vol 05.03.
Available from American National Standards Institute (ANSI), 25 W. 43rd St., 4th Floor, New York, NY 10036.
FIG. 1 Eight-Inch (203-mm) Centrifuge Tube
D1796–04 (2009)
5.1.4 Electric powered and heated centrifuges must meet all safety requirements for use in hazardous areas.
NOTE 3—Some heated centrifuges maintain the bowl at a pressure slightly below atmospheric pressure and reduce the hazards associated with vapors
and gasses, produced by samples and solvents used in the tests, by discharging any vapors to a non-hazardous area.
5.1.5 Calculate the speed of the rotating head in revolutions per minute (r/min) as follows:
rpm51335=rcf/d (1)
r/min 5 1335 rcf/d (1)
=
where:
rcf = relative centrifugal force, and
d = diameter of swing, mm swing measured between tips of opposite tubes when in rotating position.position, mm,
or
rpm5265 rcf/d (2)
=
r/min 5 265 rcf/d (2)
=
where:
rcf = relative centrifugal force, and
d = diameter of swing (inches) measured between tips of opposite tubes when in rotating position, in.
5.2
5.1.6 Calculate the relative centrifugal force from a measured speed (r/min) as follows:
r/min
rcf 5 d (3)
S D
where:
d = diameter of swing measured between tips of opposite tubes when in rotating position, mm, or
r/min
rcf 5 d (4)
S D
where:
d = diameter of swing measured between tips of opposite tubes when in rotating position, in.
5.2 Centrifuge Tubes:
5.2.1 Each centrifuge tube shall be a 203-mm (8-in.) cone-shaped tube, conforming to the dimensions given in Fig. 1, and made
of thoroughly annealed glass. The graduations, numbered as shown in Fig. 1, shall be clear and distinct, and the mouth shall be
constricted in shape for closure with a cork or solvent-resistant rubber stopper. Scale error tolerances and the smallest graduations
between various calibration marks are given in Table 1 and apply to calibrations made with air-free water at 20°C (68°F), when
reading the bottom of the shaded meniscus.
5.2.2The accuracy of the graduation marks shall be volumetrically verified or gravimetrically certified, 5.2.2 Volumetrically
verifyorgravimetricallycertifytheaccuracyofthegraduationmarks,inaccordancewithPracticeE 542usingequipmenttraceable
through the National Institute for Standards andTechnology (NIST).The verification or certification shall include(NIST) or other
national standards. Include the verification or certification for each mark through the 0.5-mLmark; of the 1, 1.5 and 2-mLmarks;
and of the 50 and 100-mL marks. The tube shall Do not be useduse the tube if the scale error exceeds the applicable tolerance in
Table 1.
Annual Book of ASTM Standards, Vol 14.04.
Available from National Institute of Standards and Technology (NIST), 100 Bureau Dr., Stop 3460, Gaithersburg, MD 20899-3460.
TABLE 1 Centrifuge Tube Calibration Tolerances for 8-in. (
203-mm (8-in.) Tube
Range, mL Subdivision, mL Volume Tolerance, mL
0to0.1 0.05 60.02
Above 0.1 to 0.3 0.05 60.03
Above 0.3 to 0.5 0.05 60.05
Above 0.5 to 1.0 0.10 60.05
Above 1.0 to 2.0 0.10 60.10
Above 2.0 to 3.0 0.20 60.10
Above 3.0 to 5.0 0.50 60.20
Above 5.0 to 10 1.00 60.50
Above 10 to 25 5.00 61.00
Above 25 to 100 25.00 61.00
D1796–04 (2009)
5.3 Bath—The bath shall be either a solid metal block bath or a liquid bath of sufficient depth for immersing the centrifuge tube
in the vertical position to the 100-mL mark. Means shall be provided for maintaining the temperature at 49 6 1°C (120 6 2°F)
and 60 6 1°C (140 6 2°F). See Note 2. —The bath shall be either a solid metal block bath or a liquid bath of sufficient depth
for immersing the centrifuge tube in the vertical position to the 100-mLmark. Provide the means for maintaining the temperature
at 60 6 1°C (140 6 1.8°F). See Note 4.
NOTE 4—It has been observed for some fuel oils that temperatures higher than 60°C (140°F) may be required to obtain correct sediment and water
content. If temperatures higher than 60°C are necessary, they may be used only with the consent of the parties involved. Water saturation of toluene may
also be carried out at this higher testing temperature. (See Annex A1.)
6. Reagents
6.1 Toluene(, conforming to the IP Specification for Methylbenzenes (Toluenes) or to ISO 5272. (Warning—Flammable
vapor harmful. See Annex A1.) that conforms to Specification D362 or to the IP Specification for Toluol shall be used as
the solvent.
6.1.1The toluene shall be water saturated at 60 6 3°C (140 6 5°F), but shall be free of suspended water. This may be
accomplished by the addition of 2 mL of water per 1000 mL of solvent. Shaking will aid in saturation, but adequate settling time
is necessary to ensure that the solvent is free of suspended water before use. SeeAnnexA2 for a procedure for saturating toluene
with water. —Flammable. Keep away from heat, sparks, and open flame. Vapor harmful. Toluene is toxic. Particular care must be
taken to avoid breathing the vapor and to protect the eyes. Keep container closed. Use with adequate ventilation.Avoid prolonged
or repeated contact with the skin.)
6.1.1 Typical characteristics for this reagent are:
Molecular weight C H CH 92.14
6 5 3
Color (APHA) 10
A
Boiling range (initial to dry point) 2.0°C (3.6°F)
Residue after evaporation 0.001 %
Substances darkened by H SO passes ACS test
2 4
Sulfur compounds (as S) 0.003 %
A
Recorded boiling point 110.6°C.
NOTE2—It has been observed for some fuel oils that temperatures higher than 60°C (140°F) may be required to obtain correct sediment and water
content. If temperatures higher than 60°C are necessary, they may be used only with the consent of the parties involved. Water saturation of toluene may
also be done at this higher testing temperature. (See Appendix X1.)
NOTE3—Some oils may require other solvents or solvent-demulsifier combinations. Those agreed upon between the purchaser and the seller may be
used.
6.2 5—Some oils may require other solvents or solvent-demulsifier combinations. Those agreed upon between the purchaser and
the seller may be used.
6.1.2 The solvent shall be water-saturated at 60 6 1°C (140 6 1.8°F) but shall be free of suspended wa
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