ASTM D95-99

Standard Test Method for Water in Petroleum Products and Bituminous Materials by Distillation

SCOPE
1.1 This test method covers the determination of water in petroleum products, tars, and other bituminous materials by the distillation method. The specific products considered during the development of this test method are listed in Table 1. For bituminous emulsions refer to Test Method D244. This test method, along with ASTM Test Method D4006 (API Chapter 10.2 and IP 358), supersedes the previous edition of ASTM Test Method D95 (API Standard 2560, IP74).  Note 1-With some types of oil, satisfactory results may be obtained from ASTM Test Method D4007 (API Chapter 10.3, IP 358, and ASTM Method D1796 API Chapter 10.6).
1.2 This standard may involve hazardous materials, operations, and equipment. This standard does not purport to address all of the safety problems 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 specific hazard statements, see 5.1.1.2 and 5.1.1.3.
1.3 The values stated in SI units are to be regarded as the standard. The values in parentheses are for information only.

General Information

• Status: Historical
• Publication Date: 09-Jun-1999
• Technical Committee: D02 - Petroleum Products, Liquid Fuels, and Lubricants
• Drafting Committee: D02.02 - Hydrocarbon Measurement for Custody Transfer (Joint ASTM-API)

Relations

• Replaced By: ASTM D95-99e1 - Standard Test Method for Water in Petroleum Products and Bituminous Materials by Distillation
• Effective Date: 10-Jun-1999
• Referred By: ASTM D5372-20 - Standard Guide for Evaluation of Hydrocarbon Heat Transfer Fluids
• Effective Date: 10-Jun-1999
• Referred By: ASTM D7666-12(2019) - Standard Specification for Triglyceride Burner Fuel
• Effective Date: 10-Jun-1999
• Referred By: ASTM D2523/D2523M-13(2019)e1 - Standard Practice for Testing Load-Strain Properties of Roofing Membranes
• Effective Date: 10-Jun-1999
• Referred By: ASTM D2028/D2028M-15(2021)e1 - Standard Specification for Cutback Asphalt (Rapid-Curing Type)
• Effective Date: 10-Jun-1999
• Referred By: ASTM D2982-07(2019) - Standard Test Methods for Detecting Glycol-Base Antifreeze in Used Lubricating Oils
• Effective Date: 10-Jun-1999
• Referred By: ASTM D4072-98(2018) - Standard Test Method for Toluene-Insoluble (TI) Content of Tar and Pitch
• Effective Date: 10-Jun-1999
• Referred By: ASTM D450/D450M-07(2018) - Standard Specification for Coal-Tar Pitch Used in Roofing, Dampproofing, and Waterproofing
• Effective Date: 10-Jun-1999
• 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-Jun-1999
• Referred By: ASTM D7832/D7832M-14(2021) - Standard Guide for Performance Attributes of Waterproofing Membranes Applied to Below-Grade Walls / Vertical Surfaces (Enclosing Interior Spaces)
• Effective Date: 10-Jun-1999
• Referred By: ASTM D3326-07(2017) - Standard Practice for Preparation of Samples for Identification of Waterborne Oils
• Effective Date: 10-Jun-1999
• Referred By: ASTM E123-02(2018) - Standard Specification for Apparatus for Determination of Water by Distillation
• Effective Date: 10-Jun-1999
• Referred By: ASTM D2318-20 - Standard Test Method for Quinoline-Insoluble (QI) Content of Tar and Pitch
• Effective Date: 10-Jun-1999
• Referred By: ASTM D8125-18(2023) - Standard Specification for Re-Refined Engine Oil Bottoms (REOB)/Vacuum Tower Asphalt Extender (VTAE)
• Effective Date: 10-Jun-1999
• Referred By: ASTM D1208-96(2019) - Standard Test Methods for Common Properties of Certain Pigments
• Effective Date: 10-Jun-1999

Standards Content (Sample)

NOTICE: This standard has either been superseded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
Designation: D 95 – 99 An American National Standard
American Association State
Highway Transportation Standard
AASHTO No. T55
MPMS Chapter 10.5
Designation: 74/82 (88)
AMERICAN SOCIETY FOR TESTING AND MATERIALS
100 Barr Harbor Dr., West Conshohocken, PA 19428
Reprinted from the Annual Book of ASTM Standards. Copyright ASTM
Standard Test Method for
Water in Petroleum Products and Bituminous Materials by
Distillation
This standard is issued under the fixed designation D 95; 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 committees and accepted by the cooperating organizations in accordance with
established procedures.
This standard has been approved for use by agencies of the Department of Defense.
TABLE 1 Type of Solvent-Carrier Liquid Versus Material to Be
1. Scope
Tested
1.1 This test method covers the determination of water in
Type of Solvent-Carrier Liquid Material to be Tested
the range from 0 to 25 % volume in petroleum products, tars,
Aromatic asphalt, tar, coal tar, water gas tar, road
and other bituminous materials by the distillation method.
tar, cut-back bitumin, liquid asphalt, tar
acid
NOTE 1—Volatile water-soluble material, if present, may be measured
Petroleum distillate road oil, fuel oil, lubricating oil, petroleum
as water.
sulfonates
Volatile spirits lubricating grease
1.2 The specific products considered during the develop-
ment of this test method are listed in Table 1. For bituminous
emulsions refer to Test Method D 244. For crude oils, refer to
the Centrifuge Method (Laboratory Procedure)
Test Method D 4006.
D 4006 Test Method for Water in Crude Oil by Distillation
D 4057 Practice for Manual Sampling of Petroleum and
NOTE 2—With some types of oil, satisfactory results may be obtained
Petroleum Products
from Test Method D 1796.
D 4177 Practice for Automatic Sampling of Petroleum and
1.3 The values stated in SI units are to be regarded as the
Petroleum Products
standard. The values in parentheses are for information only.
D 5854 Practice for Mixing and Handling of Liquid
1.4 This standard may involve hazardous materials, opera-
Samples of Petroleum and Petroleum Products
tions, and equipment. This standard does not purport to
E 123 Specification for Apparatus for Determination of
address all of the safety concerns, if any, associated with its
Water by Distillation
use. It is the responsibility of the user of this standard to
2.2 API Manual of Petroleum Measurements Standards:
establish appropriate safety and health practices and deter-
Chapter 8.1 Manual Sampling of Petroleum and Petroleum
mine the applicability of regulatory limitations prior to use.
Products (ASTM Practice D 4057)
For specific hazard statements, see Section 5 .
Chapter 8.2 Automatic Sampling of Petroleum and Petro-
leum Products (ASTM Practice D 4177)
2. Referenced Documents
Chapter 8.3 Mixing and Handling of Liquid Samples of
2.1 ASTM Standards:
Petroleum and Petroleum Products
D 244 Test Methods for Emulsified Asphalts
Chapter 10.2 Determination of Water in Crude Oil by the
D 1796 Test Method for Water and Sediment in Fuel Oils by
Distillation Method (ASTM Test Method D 4006)
This test method is under the jurisdiction of ASTM Committee D-2 on
Petroleum Products and Lubricants and API Committee on Petroleum Measurement Annual Book of ASTM Standards, Vol 05.01.
and is the direct responsibility of Subcommittee D02.02, the Joint ASTM-API Annual Book of ASTM Standards, Vol 05.02.
Committee on Static Petroleum Measurement. Annual Book of ASTM Standards, Vol 05.03.
Current edition approved June 10, 1999. Published August 1999. Originally Annual Book of ASTM Standards, Vol 14.02.
published as D 95.21. Last previous edition D 95 – 83 (90). Available from American Petroleum Institute, 1220 L St., N.W., Washington,
Annual Book of ASTM Standards, Vol 04.03. DC 20005.
NOTICE: This standard has either been superseded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
D95
Chapter 10.6 Determination of Water and Sediment in Fuel be determined by distilling an equivalent amount of the same
Oil by the Centrifuge Method (ASTM Test Method solvent used for the test sample in the distillation apparatus and
D 1796) testing as outlined in Section 9. The blank shall be determined
to the nearest scale division and used to correct the volume of
3. Summary of Test Method
water in the trap in Section 10.
3.1 The material to be tested is heated under reflux with a
6. Apparatus
water-immiscible solvent, which co-distills with the water in
the sample. Condensed solvent and water are continuously 6.1 General—The apparatus comprises a glass or metal
separated in a trap, the water settling in the graduated section
still, a heater, a reflux condenser, and a graduated glass trap.
of the trap and the solvent returning to the still. The still, trap, and condenser may be connected by any suitable
method that produces a leakproof joint. Preferred connections
4. Significance and Use
are ground joints for glass and O-rings for metal to glass.
4.1 A knowledge of the water content of petroleum products
Typical assemblies are illustrated in Fig. 1, Fig. 2, and Fig. 3.
is important in the refining, purchase, sale, and transfer of
The stills and traps should be chosen to cover the range of
products.
materials and water contents expected. On assembly, care
4.2 The amount of water as determined by this test method
should be taken to prevent the joints from freezing or sticking.
(to the nearest 0.05 volume %) may be used to correct the
This may be prevented by the application of a very thin film of
volume involved in the custody transfer of petroleum products
stopcock grease.
and bituminous materials.
6.2 Still—A glass or metal vessel with a short neck and
4.3 The allowable amount of water may be specified in
suitable joint for accommodating the reflux tube of the trap
contracts.
shall be used. Vessels of 500, 1000, and 2000-mL nominal
capacity have proved satisfactory.
5. Solvent-Carrier Liquid
6.3 Heater—A suitable gas burner or electric heater may be
5.1 A solvent-carrier liquid appropriate to the material being
used with the glass still. A gas ring burner with ports on the
tested (see Table 1) shall be used.
inside circumference shall be used with the metal still. The gas
5.1.1 Aromatic Solvent—The following aromatic solvents
ring burner shall be of such dimensions that it may be moved
are acceptable:
up and down the vessel when testing materials that are likely to
5.1.1.1 Industrial Grade Xylene.
foam or solidify in the still.
6.4 Glassware—Dimensions and descriptions of typical
NOTE 3—Warning: Flammable. Vapor harmful.
glassware for use in this test method are provided in Specifi-
5.1.1.2 A blend of 20 volume % industrial grade toluene and
cation E 123.
80 volume % industrial grade xylene.
NOTE 9—Instead of standardizing on a particular apparatus specifica-
NOTE 4—Warning: Flammable. Vapor harmful.
tion with respect to dimensions and style, a given apparatus will be
deemed satisfactory when accurate results are obtained by the standard
5.1.1.3 Petroleum or Coal Tar Naphtha, free of water,
addition technique described in Section 8.
yielding not more than 5% distillates at 125°C (257°F) and not
less than 20% at 160°C (320°F) and with a relative density
7. Sampling
(specific gravity) not lower than 0.8545 at 15.56/15.56°C
7.1 Sampling is defined as all steps required to obtain an
(60/60°F).
aliquot of the contents of any pipe, tank, or other system and to
NOTE 5—Warning: Extremely flammable. Harmful if inhaled. Vapors
may cause fire.
5.1.2 Petroleum Distillate Solvent—A petroleum distillate
solvent, 5% boiling between 90 and 100°C (194 and 212°F)
and 90% distilling below 210°C (410°F), shall be used. Percent
may be determined by mass or by volume. These solvents are
available from most chemical companies under the name of
stoddard solvent or ligroine.
NOTE 6—Warning: Flammable. Vapor harmful.
5.1.3 Volatile Spirits Solvent—The following volatile spirits
solvents are acceptable:
5.1.3.1 Petroleum Spirit, with a boiling range from 100 to
120°C (212 to 248°F).
NOTE 7—Warning: Flammable. Vapor harmful.
5.1.3.2 Isooctane, of 95% purity or better.
NOTE 8—Warning: Extremely flammable. Harmful if inhaled. Vapors
may cause fire.
5.2 Solvent Blank—The water content of the solvent shall FIG. 1 Typical Assembly with Glass Still
NOTICE: This standard has either been superseded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
D95
8.2.1 Put 400 mL of dry (0.02 % water maximum) xylene or
the solvent to be utilized in the analysis of unknown samples
into the apparatus and test in accordance with Section 9. When
complete, discard the contents of the trap and add the volume
of water as specified as first test in Table 3 directly to the
distillation flask and test in accordance with Section 9.
8.2.2 Repeat the test in 8.2.1, and add the volume specified
as second test in Table 3 directly to the flask. The assembly of
the apparatus is satisfactory only if the trap readings are within
the tolerances specified in Ta
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