ASTM D1796-97(2002)

Standard Test Method for Water and Sediment in Fuel Oils by the Centrifuge Method (Laboratory Procedure)

SCOPE
1.1 This test method covers the laboratory test for determination of water and sediment in fuel oils by using the centrifuge method in the range from 0 to 30 % volume. This chapter, along with API MPMS Chapter 10.3 (Test Method D 4007, IP 359), supersedes the previous edition of Test Method D 1796 (API Standard D 2548, IP 75).
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, Method D 95 (API MPMS Chapter 10.5) or Test Method D 473 (API MPMS Chapter 10.1) may be used.
1.2 contains a procedure for saturating toluene with water.
1.3 The values stated in SI units are to be regarded as the standard. The values in parentheses are for information only.
1.4 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.

General Information

• Status: Historical
• Publication Date: 09-Dec-2002
• ICS: 75.160.20 - Liquid fuels
• Technical Committee: D02 - Petroleum Products, Liquid Fuels, and Lubricants
• Drafting Committee: D02.02 - Hydrocarbon Measurement for Custody Transfer (Joint ASTM-API)

Relations

• Replaces: ASTM D1796-97e1 - Standard Test Method for Water and Sediment in Fuel Oils by the Centrifuge Method (Laboratory Procedure)
• Effective Date: 10-Dec-2002
• Replaced By: ASTM D1796-04 - Standard Test Method for Water and Sediment in Fuel Oils by the Centrifuge Method (Laboratory Procedure)
• Effective Date: 01-Dec-2004
• Referred By: ASTM D4868-17 - Standard Test Method for Estimation of Net and Gross Heat of Combustion of Hydrocarbon Burner and Diesel Fuels
• Effective Date: 10-Dec-2002
• Referred By: ASTM F2084/F2084M-01(2018) - Standard Guide for Collecting Containment Boom Performance Data in Controlled Environments
• Effective Date: 10-Dec-2002
• Referred By: ASTM D1290-95(2021) - Standard Test Method for Sediment in Water-Emulsion Polishes by Centrifuge
• Effective Date: 10-Dec-2002
• Referred By: ASTM D2880-23 - Standard Specification for Gas Turbine Fuel Oils
• Effective Date: 10-Dec-2002
• Referred By: ASTM D5828-97(2023) - Standard Test Method for Compatibility of Supplemental Coolant Additives (SCAs) and Engine Coolant Concentrates
• Effective Date: 10-Dec-2002
• Referred By: ASTM D6823-08(2021) - Standard Specification for Commercial Boiler Fuels With Used Lubricating Oils
• Effective Date: 10-Dec-2002
• Referred By: ASTM D2158-21 - Standard Test Method for Residues in Liquefied Petroleum (LP) Gases
• Effective Date: 10-Dec-2002
• Referred By: ASTM D7666-12(2019) - Standard Specification for Triglyceride Burner Fuel
• Effective Date: 10-Dec-2002
• Referred By: ASTM D2711-22 - Standard Test Method for Demulsibility Characteristics of Lubricating Oils
• Effective Date: 10-Dec-2002
• Referred By: ASTM D2709-22 - Standard Test Method for Water and Sediment in Middle Distillate Fuels by Centrifuge
• Effective Date: 10-Dec-2002
• Referred By: ASTM D6666-20 - Standard Guide for Evaluation of Aqueous Polymer Quenchants
• Effective Date: 10-Dec-2002
• Referred By: ASTM D6750-23 - Standard Test Methods for Evaluation of Engine Oils in a High-Speed, Single-Cylinder Diesel Engine—1K Procedure (0.4 % Fuel Sulfur) and 1N Procedure (0.04 % Fuel Sulfur)
• Effective Date: 10-Dec-2002
• Referred By: ASTM D6618-23 - Standard Test Method for Evaluation of Engine Oils in Diesel Four-Stroke Cycle Supercharged 1M-PC Single Cylinder Oil Test Engine
• Effective Date: 10-Dec-2002

Standards Content (Sample)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
An American National Standard
Designation:D1796–97 (Reapproved 2002)
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 (e) 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 D 362 Specification for Industrial Grade Toluene
D 473 Test Method for Sediment in Crude Oils and Fuel
1.1 This test method covers the laboratory test for determi-
Oils by the Extraction Method (API MPMS Chapter 10.1)
nation of water and sediment in fuel oils by using the
D 4006 Test Method for Water in Crude Oil by Distillation
centrifuge method in the range from 0 to 30 % volume. This
(API MPMS Chapter 10.2)
chapter, along with API MPMS Chapter 10.3 (Test Method
D 4007 Test Method for Water and Sediment in Crude Oil
D 4007, IP 359), supersedes the previous edition of Test
by the Centrifuge Method (Laboratory Procedure) (API
Method D 1796 (API Standard D 2548, IP 75).
MPMS Chapter 10.3)
NOTE 1—With some types of fuel oils such as residual fuel oils or
D 4057 Practice for Manual Sampling of Petroleum and
distillate fuel oils containing residual components, it is difficult to obtain
Petroleum Products (API MPMS Chapter 8.1)
water or sediment contents with this test method. When this situation is
D 4177 Practice for Automatic Sampling of Petroleum and
encountered, Method D 95 (API MPMS Chapter 10.5) or Test Method
Petroleum Products (API MPMS Chapter 8.2)
D 473 (API MPMS Chapter 10.1) may be used.
D 4377 Test Method for Water in Crude Oils by Potentio-
1.2 Annex A2 contains a procedure for saturating toluene
metric Karl Fischer Titration (API MPMS Chapter 10.7)
with water.
D 4928 Test Method for Water in Crude Oils by Coulom-
1.3 The values stated in SI units are to be regarded as the
etric Karl Fischer Titration (API MPMS Chapter 10.9)
standard. The values in parentheses are for information only.
D 5854 Practice for Mixing and Handling of Liquid
1.4 This standard does not purport to address all of the
Samples of Petroleum and Petroleum Products (API
safety concerns, if any, associated with its use. It is the
MPMS Chapter 8.3)
responsibility of the user of this standard to establish appro-
E 542 Practice for Calibration of Laboratory Volumetric
priate safety and health practices and determine the applica-
Apparatus
bility of regulatory limitations prior to use. For a specific
2.2 API Standards:
precautionary statement see 6.1.
MPMS Chapter 8.1 Manual Sampling of Petroleum and
Petroleum Products (ASTM Practice D 4057)
2. Referenced Documents
MPMS Chapter 8.2 Automatic Sampling of Petroleum and
2.1 ASTM Standards:
Petroleum Products (ASTM Practice D 4177)
D 95 Test Method for Water in Petroleum Products and
MPMSChapter8.3 MixingandHandlingLiquidSamplesof
Bituminous Materials by Distillation (API MPMS Chapter
Petroleum and Petroleum Products (ASTM Practice
10.5)
D 5854)
MPMS Chapter 10.1 Determination of Sediment in Crude
This test method is under the jurisdiction of ASTM Committee D02 on
Petroleum Products and Lubricants and theAPI Committee on Petroleum Measure-
ment, and is the direct responsibility of Subcommittee D02.02/COMQ, the joint Discontinued—See 1988 Annual Book of ASTM Standards, Vol 06.03.
ASTM-API committee on Static Petroleum Measurement. Annual Book of ASTM Standards, Vol 05.02.
Current edition approved Dec. 10, 2002. Published March 2003. Originally Annual Book of ASTM Standards, Vol 05.03.
e1 6
approved in 1960. Last previous edition approved in 1997 as D 1796–97 . Annual Book of ASTM Standards, Vol 14.04.
2 7
Annual Book of ASTM Standards, Vol 05.01. Published as Manual of Petroleum Measurement Standards.Available from the
American Petroleum Institute, 1220 L St., N.W., Washington, DC 20005.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D1796–97 (2002)
OilbytheExtractionMethod(ASTMTestMethodD 473)
MPMS Chapter 10.2 Determination of Water in Crude Oil
by the Distillation Method (ASTM Test Method D 4006)
MPMS Chapter 10.3 Determination of Water and Sediment
in Crude Oils by the Centrifuge Method (Laboratory
Procedure) (ASTM Test Method D 4007)
MPMS Chapter 10.5 Determination of Water in Petroleum
Products and Other Bituminous Materials (ASTM Test
Method D 95)
MPMS Chapter 10.7 Determination of Water in Crude Oils
(Karl Fischer) Titration (ASTM Test Method D 4377)
MPMS Chapter 10.9 Determination of Water in Crude Oils
Coulometric Karl Fischer Titration (ASTM Test Method
D 4928)
2.3 IP Standard:
Specification for Toluol
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 gravity water and
sediment layer at the bottom of the tube is read.
FIG. 1 Eight-Inch (203-mm) Centrifuge Tube
4. Significance and Use
4.1 Thewaterandsedimentcontentoffueloilissignifi-cant
because it can cause corrosion of equipment and problems in
where:
processing. The water and sediment content must be known to
rcf = relative centrifugal force, and
measure accurately net volumes of actual fuel oil in sales,
d = diameter of swing (inches) measured between tips of
taxation, exchanges, and custody transfers.
opposite tubes when in rotating position.
5.2 Centrifuge Tubes:
5. Apparatus
5.2.1 Each centrifuge tube shall be a 203-mm (8-in.) cone-
5.1 Centrifuge:
shaped tube, conforming to the dimensions given in Fig. 1 and
5.1.1 A centrifuge capable of spinning two or more filled
madeofthoroughlyannealedglass.Thegraduations,numbered
cone-shaped 203-mm (8-in.) centrifuge tubes at a speed which
as shown in Fig. 1, shall be clear and distinct, and the mouth
can be controlled to give a relative centrifugal force (rcf) of
shall be constricted in shape for closure with a cork or
between 500 and 800 at the tip of the tubes shall be used.
solvent-resistant rubber stopper. Scale error tolerances and the
5.1.2 Therevolvinghead,trunnionrings,andtrunnioncups,
smallest graduations between various calibration marks are
including the cushions, shall be soundly constructed to with-
given in Table 1 and apply to calibrations made with air-free
stand the maximum centrifugal force capable of being deliv-
water at 20°C (68°F), when reading the bottom of the shaded
eredbythepowersource.Thetrunnioncupsandcushionsshall
firmly support the tubes when the centrifuge is in motion. The meniscus.
centrifuge shall be enclosed by a metal shield or case strong
5.2.2 The accuracy of the graduation marks shall be volu-
enough to eliminate danger if any breakage occurs.
metrically verified or gravimetrically certified, in accordance
5.1.3 Calculate the speed of the rotating head in revolutions
with Practice E 542 using equipment traceable through the
per minute (rpm) as follows:
rpm 5 1335 rcf/d (1)
=
TABLE 1 Centrifuge Tube Calibration Tolerances for 8-in. (203-
where: mm) Tube
rcf = relative centrifugal force, and
Range, mL Subdivision, mL Volume Tolerance, mL
d = diameter of swing, mm measured between tips of
0to0.1 0.05 60.02
opposite tubes when in rotating position.
Above 0.1 to 0.3 0.05 60.03
Above 0.3 to 0.5 0.05 60.05
or
Above 0.5 to 1.0 0.10 60.05
rpm 5 265 rcf/d (2)
= 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
Available from American National Standards Institute, 25 W. 43nd Street., 4th Above 25 to 100 25.00 61.00
Floor, New York, NY 10036.
D1796–97 (2002)
National Institute for Standards and Technology (NIST). The 8. Procedure
verification or certification shall include verification for each
8.1 Filleachoftwocentrifugetubestothe50-mLmarkwith
mark through the 0.5-mL mark; of the 1, 1.5 and 2-mL marks;
the well-mixed sample directly from the sample container.
and of the 50 and 100-mLmarks. The tube shall not be used if
Then, using a pipette, add 50 mL of the water-saturated
the scale error exceeds the applicable tolerance in Table 1.
solvent. Read the top of the meniscus at both the 50 and
5.3 Bath—The bath shall be either a solid metal block bath
100-mL marks. Stopper the tubes tightly and shake vigorously
or a liquid bath of sufficient depth for immersing the centrifuge
until the contents are thoroughly mixed. Loosen the stoppers
tube in the vertical position to the 100-mL mark. Means shall
on the tubes and immerse the tubes to the 100-mLmark for 10
be provided for maintaining the temperature at 49 6 1°C (120
min in the bath maintained at 60 6 1°C (140 6 2°F).
6 2°F) and 60 6 1°C (140 6 2°F). See Note 2.
8.2 Tighten the stoppers and again invert the tubes to ensure
that the oil and solvent are uniformly mixed and shake
6. Reagents
cautiously. (Warning—In general, the vapor pressures of
6.1 Toluene (Warning—Flammable vapor harmful. See
hydrocarbons at 60°C (140°F) are approximately double those
Annex A1.) that conforms to Specification D 362 or to the IP
at 40°C (104°F). Consequently, tubes should always be in-
Specification for Toluol shall be used as the solvent.
verted at a position below eye level so that contact will be
6.1.1 The toluene shall be water saturated at 60 6 3°C (140
avoided if the stopper is blown out.)
6 5°F), but shall be free of suspended water. This may be
8.2.1 Place the tubes in the trunnion cups on opposite sides
accomplished by the addition of 2 mLof water per 1000 mLof
of the centrifuge to establish a balanced condition, and spin for
solvent. Shaking will aid in saturation, but adequate settling
10 min at a rate, calculated from the equation given in 5.1,
time is necessary to ensure that the solvent is free of suspended
sufficient to produce a relative centrifugal force (rcf)of
water before use. SeeAnnexA2 for a procedure for saturating
between 500 and 800 at the tip of the whirling tubes (seeTable
toluene with water.
2 for the relationship between diameter of swing, relative
centrifugalforce,andrevolutionsperminute).Thetemperature
NOTE 2—It has been observed for some fuel oils that temperatures
of the sample during the entire centrifuging procedure shall be
higher than 60°C (140°F) may be required to obtain correct sediment and
water content. If temperatures higher than 60°C are ne
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