ASTM D95-13(2018)
(Test Method)Standard Test Method for Water in Petroleum Products and Bituminous Materials by Distillation
Standard Test Method for Water in Petroleum Products and Bituminous Materials by Distillation
SIGNIFICANCE AND USE
5.1 A knowledge of the water content of petroleum products is important in the refining, purchase, sale, and transfer of products.
5.2 The amount of water as determined by this test method (to the nearest 0.05 % or 0.1 % by volume, depending on the trap size used) may be used to correct the volume involved in the custody transfer of petroleum products and bituminous materials.
5.3 The allowable amount of water may be specified in contracts.
SCOPE
1.1 This test method covers the determination of water in the range from 0 % to 25 % by volume in petroleum products, tars, and other bituminous materials by the distillation method.
Note 1: Volatile water-soluble material, if present, may be measured as water.
1.2 The specific products considered during the development of this test method are listed in Table 1. For bituminous emulsions refer to Test Method D244. For crude oils, refer to Test Method D4006 (API MPMS Chapter 10.2).
Note 2: With some types of oil, satisfactory results may be obtained from Test Method D1796 (API MPMS Chapter 10.6).
1.3 The values stated in SI units are to be regarded as standard. The values given in parentheses after SI units are provided for information only and are not considered standard.
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, health, and environmental practices and determine the applicability of regulatory limitations prior to use. For specific hazard statements, see Section 6.
1.5 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.
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Buy Standard
Standards Content (Sample)
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: D95 − 13 (Reapproved 2018)
Manual of Petroleum Measurement Standards (MPMS), Chapter 10.5
Standard Test Method for
Water in Petroleum Products and Bituminous Materials by
Distillation
This standard is issued under the fixed designation D95; 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.Asuperscript
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 2. Referenced Documents
2.1 ASTM Standards:
1.1 This test method covers the determination of water in
D235 Specification for Mineral Spirits (Petroleum Spirits)
the range from 0 % to 25 % by volume in petroleum products,
(Hydrocarbon Dry Cleaning Solvent)
tars, and other bituminous materials by the distillation method.
D244 Test Methods and Practices for Emulsified Asphalts
NOTE 1—Volatile water-soluble material, if present, may be measured
D1796 Test Method for Water and Sediment in Fuel Oils by
as water.
the Centrifuge Method (Laboratory Procedure) (API
1.2 The specific products considered during the develop-
MPMS Chapter 10.6)
ment of this test method are listed in Table 1. For bituminous
D4006 Test Method for Water in Crude Oil by Distillation
emulsions refer to Test Method D244. For crude oils, refer to
(API MPMSChapter 10.2)
Test Method D4006 (API MPMS Chapter 10.2).
D4057 Practice for Manual Sampling of Petroleum and
Petroleum Products (API MPMS Chapter 8.1)
NOTE 2—With some types of oil, satisfactory results may be obtained
D4177 Practice for Automatic Sampling of Petroleum and
from Test Method D1796 (API MPMS Chapter 10.6).
Petroleum Products (API MPMS Chapter 8.2)
1.3 The values stated in SI units are to be regarded as
D5854 Practice for Mixing and Handling of Liquid Samples
standard. The values given in parentheses after SI units are
of Petroleum and Petroleum Products (API MPMS Chap-
provided for information only and are not considered standard.
ter 8.3)
1.4 This standard does not purport to address all of the
E123 SpecificationforApparatusforDeterminationofWater
safety concerns, if any, associated with its use. It is the
by Distillation
responsibility of the user of this standard to establish appro-
2.2 API Standards:
priate safety, health, and environmental practices and deter-
MPMS Chapter 8.1 Manual Sampling of Petroleum and
mine the applicability of regulatory limitations prior to use.
Petroleum Products (ASTM Practice D4057)
For specific hazard statements, see Section 6.
MPMS Chapter 8.2 Automatic Sampling of Petroleum and
1.5 This international standard was developed in accor-
Petroleum Products (ASTM Practice D4177)
dance with internationally recognized principles on standard- MPMS Chapter 8.3 Mixing and Handling of Liquid Samples
ization established in the Decision on Principles for the
of Petroleum and Petroleum Products (ASTM Practice
Development of International Standards, Guides and Recom- D5854)
mendations issued by the World Trade Organization Technical
MPMSChapter10.2 DeterminationofWaterinCrudeOilby
Barriers to Trade (TBT) Committee.
the Distillation Method (ASTM Test Method D4006)
MPMS Chapter 10.6 Test Method for Water and Sediment in
Fuel Oils by the Centrifuge Method (Laboratory Proce-
dure) (ASTM Test Method D1796)
This test method is under the jurisdiction of ASTM Committee D02 on
Petroleum Products, Liquid Fuels, and Lubricants and the API Committee on
Petroleum Measurement, and is the direct responsibility of Subcommittee D02.02
/COMQ the joint ASTM-API Committee on Hydrocarbon Measurement for For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Custody Transfer (Joint ASTM-API). This practice has been approved by the contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
sponsoring committees and accepted by the Cooperating Societies in accordance Standards volume information, refer to the standard’s Document Summary page on
with established procedures. the ASTM website.
Current edition approved Oct. 1, 2018. Published November 2018. Originally Published as Manual of Petroleum Measurement Standards. Available from
ɛ1
approved in 1921. Last previous edition approved in 2013 as D95 – 13 . DOI: AmericanPetroleumInstitute(API),1220L.St.,NW,Washington,DC20005-4070,
10.1520/D0095-13R18. http://www.api.org.
© 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
D95 − 13 (2018)
NOTE 4—It is recommended to use a wide boiling range solvent with
3. Terminology
10 % boiling below 100 °C to help to ensure an even distillation rate.
3.1 Definitions:
6.1.3 Volatile Spirits Solvent—The following volatile spirits
3.1.1 bituminous material, n—in petroleum technology,a
solvents are acceptable:
black or dark-colored very viscous liquid or semi-solid com-
6.1.3.1 Petroleum Spirit, with a boiling range from 100 °C
posed principally of high molecular weight condensed
to 120 °C (212 °F to 248 °F). (Warning—Flammable. Vapor
aromatic, or naphthenic compounds, or both.
harmful.)
6.1.3.2 Iso-octane, of 95 % purity or better. (Warning—
4. Summary of Test Method
Extremely flammable. Harmful if inhaled. Vapors may cause
4.1 The material to be tested is heated under reflux with a
fire.)
water-immiscible solvent, which co-distills with the water in
6.2 Solvent Blank—Thewatercontentofthesolventshallbe
the sample. Condensed solvent and water are continuously
determined by distilling an equivalent amount of the same
separated in a trap, the water settling in the graduated section
solventusedforthetestsampleinthedistillationapparatusand
of the trap and the solvent returning to the still.
testingasoutlinedinSection10.Theblankshallbedetermined
5. Significance and Use
to the nearest scale division and used to correct the volume of
water in the trap in Section 11.
5.1 Aknowledge of the water content of petroleum products
is important in the refining, purchase, sale, and transfer of
7. Apparatus
products.
7.1 General—Theapparatuscomprisesaglassormetalstill,
5.2 The amount of water as determined by this test method
a heater, a reflux condenser, and a graduated glass trap. The
(to the nearest 0.05 % or 0.1 % by volume, depending on the
still, trap, and condenser may be connected by any suitable
trap size used) may be used to correct the volume involved in
method that produces a leakproof joint. Preferred connections
the custody transfer of petroleum products and bituminous
are ground joints for glass and O-rings for metal to glass.
materials.
Typical assemblies are illustrated in Fig. 1, Fig. 2, and Fig. 3.
5.3 The allowable amount of water may be specified in
The stills and traps should be chosen to cover the range of
contracts.
materials and water contents expected. On assembly, care shall
be taken to prevent the joints from freezing or sticking.Always
6. Solvent-Carrier Liquid
apply a very thin film of stopcock grease to prevent the
6.1 A water-immiscible solvent-carrier liquid that is mis-
glassware joints from seizing.
cible in the material being tested (see Table 1) shall be used.
7.2 Still—A glass or metal vessel with a short neck and
6.1.1 Aromatic Solvent—The following aromatic solvents
suitable joint for accommodating the reflux tube of the trap
are acceptable:
shall be used. Vessels of 500 mL, 1000 mL, and 2000 mL
6.1.1.1 Industrial Grade Xylene—(Warning—Flammable.
nominal capacity have proved satisfactory.
Vapor harmful.)
7.3 Heater—Asuitable gas burner or electric heater may be
6.1.1.2 Ablend of 20 % by volume industrial grade toluene
used with the glass still. A gas ring burner with ports on the
and 80 % by volume industrial grade xylene. (Warning—
inside circumference shall be used with the metal still. The gas
Flammable. Vapor harmful.)
ring burner shall be of such dimensions that it may be moved
6.1.1.3 Petroleum Naphtha or Coal Tar Naphtha, free of
water,yieldingnotmorethan5 %distillatesat125 °C(257 °F)
and not less than 20 % at 160 °C (320 °F) and with a relative
density (specific gravity) not lower than 0.8545 at
15.56 °C⁄15.56 °C (60 °F⁄60 °F). (Warning—Extremely
flammable. Harmful if inhaled. Vapors may cause fire.)
6.1.2 Petroleum Distillate Solvent—A petroleum distillate
solvent containing at least 2 % (V/V) aromatics and with an
initial boiling point (IBP) greater than 80 °C (176 °F); and a
final boiling point (FBP) below 250 °C (482 °F) shall be used.
NOTE 3—Examples of suitable solvents include Types I and IV and
Classes A and B of Specification D235.
TABLE 1 Type of Solvent-Carrier Liquid to Use Versus Material to
Be Tested
Type of Solvent-Carrier Liquid Material to be Tested
Aromatic asphalt, bitumen, tar, and related products
Petroleum distillate fuel oil, lubricating oil, lubricating oil additives
Volatile spirits greases
FIG. 1 Typical Assembly with Glass Still
D95 − 13 (2018)
ogy (NIST) traceable equipment. Verification shall be with a
traceable 5 mLMicro Burette or Micro Pipette, readable to the
nearest 0.01 mL.
9.1.1 In styles A, B, C, and D, as specified in Table 2
(Table 1 in Specification E123), each subdivision (that is,
0.1 mLthrough 1.0 mL) in the conical portion of the tube shall
be verified.Thereafter, each major subdivision (that is, 2.0 mL,
3.0 mL, 4.0 mL, and up to the total volume of the trap) shall be
verified.
9.1.2 In styles E and F, as specified in Table 2, each major
subdivision (0.1 mL, 1.0 mL, 2.0 mL, 4.0 mL, and 5.0 mL in
the case of Style E; 0.05 mL, 0.5 mL, 1.0 mL, 1.5 mL, and
2.0 mL in the case of Style F) shall be verified.
9.2 The entire glassware assembly shall be verified prior to
first use and at a regular frequency thereafter as follows.
9.2.1 Put 400 mLof 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 10.
When complete, discard the contents of the trap and add the
FIG. 2 Tw
...
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
Designation: D95 − 13 (Reapproved 2018)
Manual of Petroleum Measurement Standards (MPMS), Chapter 10.5
Standard Test Method for
Water in Petroleum Products and Bituminous Materials by
Distillation
This standard is issued under the fixed designation D95; 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 2. Referenced Documents
2.1 ASTM Standards:
1.1 This test method covers the determination of water in
D235 Specification for Mineral Spirits (Petroleum Spirits)
the range from 0 % to 25 % by volume in petroleum products,
(Hydrocarbon Dry Cleaning Solvent)
tars, and other bituminous materials by the distillation method.
D244 Test Methods and Practices for Emulsified Asphalts
NOTE 1—Volatile water-soluble material, if present, may be measured
D1796 Test Method for Water and Sediment in Fuel Oils by
as water.
the Centrifuge Method (Laboratory Procedure) (API
1.2 The specific products considered during the develop-
MPMS Chapter 10.6)
ment of this test method are listed in Table 1. For bituminous
D4006 Test Method for Water in Crude Oil by Distillation
emulsions refer to Test Method D244. For crude oils, refer to
(API MPMSChapter 10.2)
Test Method D4006 (API MPMS Chapter 10.2).
D4057 Practice for Manual Sampling of Petroleum and
Petroleum Products (API MPMS Chapter 8.1)
NOTE 2—With some types of oil, satisfactory results may be obtained
D4177 Practice for Automatic Sampling of Petroleum and
from Test Method D1796 (API MPMS Chapter 10.6).
Petroleum Products (API MPMS Chapter 8.2)
1.3 The values stated in SI units are to be regarded as
D5854 Practice for Mixing and Handling of Liquid Samples
standard. The values given in parentheses after SI units are
of Petroleum and Petroleum Products (API MPMS Chap-
provided for information only and are not considered standard.
ter 8.3)
1.4 This standard does not purport to address all of the
E123 Specification for Apparatus for Determination of Water
safety concerns, if any, associated with its use. It is the
by Distillation
responsibility of the user of this standard to establish appro-
2.2 API Standards:
priate safety, health, and environmental practices and deter-
MPMS Chapter 8.1 Manual Sampling of Petroleum and
mine the applicability of regulatory limitations prior to use.
Petroleum Products (ASTM Practice D4057)
For specific hazard statements, see Section 6.
MPMS Chapter 8.2 Automatic Sampling of Petroleum and
1.5 This international standard was developed in accor- Petroleum Products (ASTM Practice D4177)
dance with internationally recognized principles on standard-
MPMS Chapter 8.3 Mixing and Handling of Liquid Samples
ization established in the Decision on Principles for the of Petroleum and Petroleum Products (ASTM Practice
Development of International Standards, Guides and Recom-
D5854)
mendations issued by the World Trade Organization Technical
MPMS Chapter 10.2 Determination of Water in Crude Oil by
Barriers to Trade (TBT) Committee.
the Distillation Method (ASTM Test Method D4006)
MPMS Chapter 10.6 Test Method for Water and Sediment in
Fuel Oils by the Centrifuge Method (Laboratory Proce-
dure) (ASTM Test Method D1796)
This test method is under the jurisdiction of ASTM Committee D02 on
Petroleum Products, Liquid Fuels, and Lubricants and the API Committee on
Petroleum Measurement, and is the direct responsibility of Subcommittee D02.02
/COMQ the joint ASTM-API Committee on Hydrocarbon Measurement for For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Custody Transfer (Joint ASTM-API). This practice has been approved by the contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
sponsoring committees and accepted by the Cooperating Societies in accordance Standards volume information, refer to the standard’s Document Summary page on
with established procedures. the ASTM website.
Current edition approved Oct. 1, 2018. Published November 2018. Originally Published as Manual of Petroleum Measurement Standards. Available from
ɛ1
approved in 1921. Last previous edition approved in 2013 as D95 – 13 . DOI: American Petroleum Institute (API), 1220 L. St., NW, Washington, DC 20005-4070,
10.1520/D0095-13R18. http://www.api.org.
© 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
D95 − 13 (2018)
NOTE 4—It is recommended to use a wide boiling range solvent with
3. Terminology
10 % boiling below 100 °C to help to ensure an even distillation rate.
3.1 Definitions:
6.1.3 Volatile Spirits Solvent—The following volatile spirits
3.1.1 bituminous material, n—in petroleum technology, a
solvents are acceptable:
black or dark-colored very viscous liquid or semi-solid com-
6.1.3.1 Petroleum Spirit, with a boiling range from 100 °C
posed principally of high molecular weight condensed
to 120 °C (212 °F to 248 °F). (Warning—Flammable. Vapor
aromatic, or naphthenic compounds, or both.
harmful.)
6.1.3.2 Iso-octane, of 95 % purity or better. (Warning—
4. Summary of Test Method
Extremely flammable. Harmful if inhaled. Vapors may cause
4.1 The material to be tested is heated under reflux with a
fire.)
water-immiscible solvent, which co-distills with the water in
6.2 Solvent Blank—The water content of the solvent shall be
the sample. Condensed solvent and water are continuously
determined by distilling an equivalent amount of the same
separated in a trap, the water settling in the graduated section
solvent used for the test sample in the distillation apparatus and
of the trap and the solvent returning to the still.
testing as outlined in Section 10. The blank shall be determined
5. Significance and Use
to the nearest scale division and used to correct the volume of
water in the trap in Section 11.
5.1 A knowledge of the water content of petroleum products
is important in the refining, purchase, sale, and transfer of
7. Apparatus
products.
7.1 General—The apparatus comprises a glass or metal still,
5.2 The amount of water as determined by this test method
a heater, a reflux condenser, and a graduated glass trap. The
(to the nearest 0.05 % or 0.1 % by volume, depending on the
still, trap, and condenser may be connected by any suitable
trap size used) may be used to correct the volume involved in
method that produces a leakproof joint. Preferred connections
the custody transfer of petroleum products and bituminous
are ground joints for glass and O-rings for metal to glass.
materials.
Typical assemblies are illustrated in Fig. 1, Fig. 2, and Fig. 3.
5.3 The allowable amount of water may be specified in
The stills and traps should be chosen to cover the range of
contracts.
materials and water contents expected. On assembly, care shall
be taken to prevent the joints from freezing or sticking. Always
6. Solvent-Carrier Liquid
apply a very thin film of stopcock grease to prevent the
6.1 A water-immiscible solvent-carrier liquid that is mis-
glassware joints from seizing.
cible in the material being tested (see Table 1) shall be used.
7.2 Still—A glass or metal vessel with a short neck and
6.1.1 Aromatic Solvent—The following aromatic solvents
suitable joint for accommodating the reflux tube of the trap
are acceptable:
shall be used. Vessels of 500 mL, 1000 mL, and 2000 mL
6.1.1.1 Industrial Grade Xylene—(Warning—Flammable.
nominal capacity have proved satisfactory.
Vapor harmful.)
7.3 Heater—A suitable gas burner or electric heater may be
6.1.1.2 A blend of 20 % by volume industrial grade toluene
used with the glass still. A gas ring burner with ports on the
and 80 % by volume industrial grade xylene. (Warning—
inside circumference shall be used with the metal still. The gas
Flammable. Vapor harmful.)
ring burner shall be of such dimensions that it may be moved
6.1.1.3 Petroleum Naphtha or Coal Tar Naphtha, free of
water, 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 (specific gravity) not lower than 0.8545 at
15.56 °C ⁄15.56 °C (60 °F ⁄60 °F). (Warning—Extremely
flammable. Harmful if inhaled. Vapors may cause fire.)
6.1.2 Petroleum Distillate Solvent—A petroleum distillate
solvent containing at least 2 % (V/V) aromatics and with an
initial boiling point (IBP) greater than 80 °C (176 °F); and a
final boiling point (FBP) below 250 °C (482 °F) shall be used.
NOTE 3—Examples of suitable solvents include Types I and IV and
Classes A and B of Specification D235.
TABLE 1 Type of Solvent-Carrier Liquid to Use Versus Material to
Be Tested
Type of Solvent-Carrier Liquid Material to be Tested
Aromatic asphalt, bitumen, tar, and related products
Petroleum distillate fuel oil, lubricating oil, lubricating oil additives
Volatile spirits greases
FIG. 1 Typical Assembly with Glass Still
D95 − 13 (2018)
ogy (NIST) traceable equipment. Verification shall be with a
traceable 5 mL Micro Burette or Micro Pipette, readable to the
nearest 0.01 mL.
9.1.1 In styles A, B, C, and D, as specified in Table 2
(Table 1 in Specification E123), each subdivision (that is,
0.1 mL through 1.0 mL) in the conical portion of the tube shall
be verified. Thereafter, each major subdivision (that is, 2.0 mL,
3.0 mL, 4.0 mL, and up to the total volume of the trap) shall be
verified.
9.1.2 In styles E and F, as specified in Table 2, each major
subdivision (0.1 mL, 1.0 mL, 2.0 mL, 4.0 mL, and 5.0 mL in
the case of Style E; 0.05 mL, 0.5 mL, 1.0 mL, 1.5 mL, and
2.0 mL in the case of Style F) shall be verified.
9.2 The entire glassware assembly shall be verified prior to
first use and at a regular frequency thereafter as follows.
9.2.1 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 10.
When complete, discard the contents of the trap and add the
FIG. 2 Two-millilitre Receiver Showing Alternative Connections to
volum
...
This document is not an ASTM standard and is intended only to provide the user of an ASTM 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.
´1
Designation: D95 − 13 D95 − 13 (Reapproved 2018)
Manual of Petroleum Measurement Standards (MPMS), Chapter 10.5
Standard Test Method for
Water in Petroleum Products and Bituminous Materials by
Distillation
This standard is issued under the fixed designation D95; 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.
ε NOTE—IP information was removed editorially in September 2013.
1. Scope*Scope
1.1 This test method covers the determination of water in the range from 00 % to 25 % by volume in petroleum products, tars,
and other bituminous materials by the distillation method.
NOTE 1—Volatile water-soluble material, if present, may be measured as water.
1.2 The specific products considered during the development of this test method are listed in Table 1. For bituminous emulsions
refer to Test Method D244. For crude oils, refer to Test Method D4006 (API MPMS Chapter 10.2).
NOTE 2—With some types of oil, satisfactory results may be obtained from Test Method D1796 (API MPMS Chapter 10.6).
1.3 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.after
SI units are provided for information only and are not considered standard.
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 safety, health, and healthenvironmental practices and determine the
applicability of regulatory limitations prior to use. For specific hazard statements, see Section 6.
1.5 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.
2. Referenced Documents
2.1 ASTM Standards:
D235 Specification for Mineral Spirits (Petroleum Spirits) (Hydrocarbon Dry Cleaning Solvent)
D244 Test Methods and Practices for Emulsified Asphalts
D1796 Test Method for Water and Sediment in Fuel Oils by the Centrifuge Method (Laboratory Procedure) (API MPMS Chapter
10.6)
D4006 Test Method for Water in Crude Oil by Distillation (API MPMSChapter 10.2)
D4057 Practice for Manual Sampling of Petroleum and Petroleum Products (API MPMS Chapter 8.1)
D4177 Practice for Automatic Sampling of Petroleum and Petroleum Products (API MPMS Chapter 8.2)
D5854 Practice for Mixing and Handling of Liquid Samples of Petroleum and Petroleum Products (API MPMS Chapter 8.3)
E123 Specification for Apparatus for Determination of Water by Distillation
2.2 API Standards:
MPMS Chapter 8.1 Manual Sampling of Petroleum and Petroleum Products (ASTM Practice D4057)
MPMS Chapter 8.2 Automatic Sampling of Petroleum and Petroleum Products (ASTM Practice D4177)
This test method is under the jurisdiction of ASTM Committee D02 on Petroleum Products, Liquid Fuels, and Lubricants and the API Committee on Petroleum
Measurement, and is the direct responsibility of Subcommittee D02.02 /COMQ,/COMQ the joint ASTM-API Committee on Hydrocarbon Measurement for Custody Transfer
(Joint ASTM-API). This practice has been approved by the sponsoring committees and accepted by the Cooperating Societies in accordance with established procedures.
Current edition approved May 1, 2013Oct. 1, 2018. Published July 2013November 2018. Originally approved in 1921. Last previous edition approved in 20102013 as
ɛ1
D95 – 05 (2010).D95 – 13 . DOI: 10.1520/D0095-13E01.10.1520/D0095-13R18.
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 the ASTM website.
Published as Manual of Petroleum Measurement Standards. Available from American Petroleum Institute (API), 1220 L. St., NW, Washington, DC 20005-4070,
http://www.api.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
D95 − 13 (2018)
MPMS Chapter 8.3 Mixing and Handling of Liquid Samples of Petroleum and Petroleum Products (ASTM Practice D5854)
MPMS Chapter 10.2 Determination of Water in Crude Oil by the Distillation Method (ASTM Test Method D4006)
MPMS Chapter 10.6 Test Method for Water and Sediment in Fuel Oils by the Centrifuge Method (Laboratory Procedure)
(ASTM Test Method D1796)
D95 − 13 (2018)
3. Terminology
3.1 Definitions:
3.1.1 bituminous material, n—in petroleum technology, a black or dark-colored very viscous liquid or semi-solid composed
principally of high molecular weight condensed aromatic, or naphthenic compounds, or both.
4. Summary of Test Method
4.1 The material to be tested is heated under reflux with a water-immiscible solvent, which co-distills with the water in the
sample. Condensed solvent and water are continuously separated in a trap, the water settling in the graduated section of the trap
and the solvent returning to the still.
5. Significance and Use
5.1 A knowledge of the water content of petroleum products is important in the refining, purchase, sale, and transfer of products.
5.2 The amount of water as determined by this test method (to the nearest 0.05 or 0.1 volume %, 0.05 % or 0.1 % by volume,
depending on the trap size used) may be used to correct the volume involved in the custody transfer of petroleum products and
bituminous materials.
5.3 The allowable amount of water may be specified in contracts.
6. Solvent-Carrier Liquid
6.1 A water-immiscible solvent-carrier liquid that is miscible in the material being tested (see Table 1) shall be used.
6.1.1 Aromatic Solvent—The following aromatic solvents are acceptable:
6.1.1.1 Industrial Grade Xylene—(Warning—Flammable. Vapor harmful.)
6.1.1.2 A blend of 20 volume % 20 % by volume industrial grade toluene and 80 volume % 80 % by volume industrial grade
xylene. (Warning—Flammable. Vapor harmful.)
6.1.1.3 Petroleum Naphtha or Coal Tar Naphtha, free of water, yielding not more than 5%5 % distillates at 125°C
(257°F)125 °C (257 °F) and not less than 20%20 % at 160°C (320°F)160 °C (320 °F) and with a relative density (specific gravity)
not lower than 0.8545 at 15.56/15.56°C15.56 °C (60/60°F).⁄15.56 °C (60 °F ⁄60 °F). (Warning—Extremely flammable. Harmful
if inhaled. Vapors may cause fire.)
6.1.2 Petroleum Distillate Solvent—A petroleum distillate solvent containing at least 2%2 % (V/V) aromatics and with an initial
boiling point (IBP) greater than 80°C (176°F);80 °C (176 °F); and a final boiling point (FBP) below 250°C (482°F)250 °C (482 °F)
shall be used.
NOTE 3—Examples of suitable solvents include Types I and IV and Classes A and B of Specification D235.
NOTE 4—It is recommended to use a wide boiling range solvent with 10%10 % boiling below 100°C100 °C to help to ensure an even distillation rate.
6.1.3 Volatile Spirits Solvent—The following volatile spirits solvents are acceptable:
6.1.3.1 Petroleum Spirit, with a boiling range from 100100 °C to 120°C (212120 °C (212 °F to 248°F).248 °F). (Warning—
Flammable. Vapor harmful.)
6.1.3.2 Iso-octane, of 95%95 % purity or better. (Warning—Extremely flammable. Harmful if inhaled. Vapors may cause fire.)
6.2 Solvent Blank—The water content of the solvent shall be determined by distilling an equivalent amount of the same solvent
used for the test sample in the distillation apparatus and testing as outlined in Section 10. The blank shall be determined to the
nearest scale division and used to correct the volume of water in the trap in Section 11.
7. Apparatus
7.1 General—The apparatus comprises a glass or metal still, a heater, a reflux condenser, and a graduated glass trap. The still,
trap, and condenser may be connected by any suitable method that produces a leakproof joint. Preferred connections are ground
joints for glass and O-rings for metal to glass. Typical assemblies are illustrated in Fig. 1, Fig. 2, and Fig. 3. The stills and traps
should be chosen to cover the range of materials and water contents expected. On assembly, care shall be taken to prevent the joints
from freezing or sticking. Always apply a very thin film of stopcock grease to prevent the glassware joints from seizing.
TABLE 1 Type of Solvent-Carrier Liquid to Use Versus Material to
Be Tested
Type of Solvent-Carrier Liquid Material to be Tested
Aromatic asphalt, bitumen, tar, and related products
Petroleum distillate fuel oil, lubricating oil, lubricating oil additives
Volatile spirits greases
D95 − 13 (2018)
FIG. 1 Typical Assembly with Glass Still
FIG. 2 Two-millilitre Receiver Showing Alternative Connections to Glass Still
7.2 Still—A glass or metal vessel with a short neck and suitable joint for accommodating the reflux tube of the trap shall be used.
Vessels of 500, 1000,500 mL, 1000 mL, and 2000-mL2000 mL nominal capacity have proved satisfactory.
7.3 Heater—A suitable gas burner or electric heater may be used with the glass still. A gas ring burner with ports on the inside
circumference shall be used with the metal still. The gas ring burner shall be of such dimensions that it may be moved up and down
the vessel when testing materials that are likely to foam or solidify in the still.
7.4 Glassware—Dimensions and descriptions of typical glassware for use in this test method are provided in Specification E123.
NOTE 5—Instead of standardizing on a particular apparatus specification with respect to dimensions and style, a given apparatus will be deemed
satisfactory when accurate results are obtained by the standard addition technique described in Section 9.
8. Sampling
8.1 Sampling is defined as all steps required to obtain an aliquot of the contents of any pipe, tank, or other system and to place
the sample into the laboratory test container. Only representative samples obtained as specified in Practices D4057 (API MPMS
Chapter 8.1) and D4177 (API MPMS Chapter 8.2) shall be used for this test method.
8.2 The size of the test portion should be based on the expected water content of the sample, such that the water yield does not
exceed the capacity of the trap (unless a trap with a stopcock is used permitting excess water to be withdrawn into a graduated
cylinder).
D95 − 13 (2018)
NOTE 1—Trap shall be 15 to 16 mm in inside diameter.
FIG. 3 Typical Assemblies with Metal Still
D95 − 13 (2018)
8.3 Practice D5854 (API MPMS Chapter 8.3) contains information on sampling and homogenization efficiency of unknown
mixers. This test method should not be followed without strict adherence to Practice D5854 (API MPMS Chapter 8.3).
9. Verification
9.1 The accuracy of the graduation marks on the trap shall be certified or verified, using only national or international standards,
such as National Institute of Standards and Technology (NIST) traceable equipment. Verification shall be with a traceable 5 mL
Micro Burette or Micro Pipette, readable to the nearest 0.01 mL.0.01 mL.
9.1.1 In styles A, B, C, and D, as specified in Table 2 (Table 1 in Specification E123), each subdivision (that is, 0.1 mL through
1.0 mL) 0.1 mL through 1.0 mL) in the conical portion of the tube shall be verified. Thereafter, each major subdivision (that is,
2.0 mL, 3.0 mL, 4.0 mL, 2.0 mL, 3.0 mL, 4.0 mL, and up to the total volume of the trap) shall be verified.
9.1.2 In styles E and F, as specified in Table 2, each major subdivision (0.1 mL, 1.0 mL, 2.0 mL, 4.0 mL, and 5.0 mL (0.1 mL,
1.0 mL, 2.0 mL, 4.0 mL, and 5.0 mL in the case of Style E; 0.05 mL, 0.5 mL, 1.0 mL, 1.5 mL, and 2.0 mL 0.05 mL, 0.5 mL,
1.0 mL, 1.5 mL, and 2.0 mL in the case of Style F) shall be verified.
9.2 The entire glassware assembly shall be verified prior to first use and at a regular frequency thereafter as follows.
9.2.1 Put 400 mL 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 10. 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 10.
9.2.2 Repeat the test in 9.2.1, 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 Table 3.
9.3 A reading outside the permissible limits suggests a malfunction resulting from vapor leaks, too rapid boiling, inaccuracies
in calibration of the trap, or ingress of extraneous moisture. Eliminate these factors before repeating the verification.
10. Procedure
NOTE 6—The precision of this test method will be affected by water droplets adhering to surfaces in the apparatus and therefore not settling into the
water trap to be measured. To minimize the problem, all apparatus must be cleaned chemically at least daily to remove surface films and debris, which
hinder free drainage of water in the test apparatus. More frequent cleaning is recommended if the nature of samples being run causes persistent
contamination.
10.1 Measure a suitable amount of sample to an accuracy of 6 1% 61 % and transfer it to the still.
10.2 Measure ordinary liquid samples in a graduated cylinder of an appropriate size. Rinse the material adhering to the cylinder
with one 50-mL50 mL and two 25-mL25 mL portions of the solvent-carrier liquid (see Section 6 and Table 1). Drain the cylinder
thoroughly after the sample transfer and each rinsing.
10.3 Weigh solid or viscous materials directly into the still and add 100 mL 100 mL of the selected solvent-carrier liquid. In
cases of material with a low-water content when large samples must be used, a solvent-carrier liquid volume in excess of 100 mL
100 mL
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