ASTM D4928-12
(Test Method)Standard Test Method for Water in Crude Oils by Coulometric Karl Fischer Titration
Standard Test Method for Water in Crude Oils by Coulometric Karl Fischer Titration
SIGNIFICANCE AND USE
5.1 The accurate analysis of a crude oil sample to determine the water content is important in the refining, purchase, sale, or transfer of crude oils.
SCOPE
1.1 This test method covers the determination of water in the range from 0.02 to 5.00 mass or volume % in crude oils. Mercaptan (RSH) and sulfide (S− or H2S) as sulfur are known to interfere with this test method, but at levels of less than 500 μg/g [ppm(m)], the interference from these compounds is insignificant (see Section 6).
1.2 This test method can be used to determine water in the 0.005 to 0.02 mass % range, but the effects of the mercaptan and sulfide interference at these levels has not been determined. For the range 0.005 to 0.02 mass %, there is no precision or bias statement.
1.3 This test method is intended for use with standard commercially available coulometric Karl Fischer reagent.
1.4 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.5 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 specific warning statements, see Section 8.
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Designation: D4928 − 12
Manual of Petroleum Measurement Standards (MPMS), Chapter 10.9
Standard Test Method for
1
Water in Crude Oils by Coulometric Karl Fischer Titration
This standard is issued under the fixed designation D4928; 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.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* D4177Practice for Automatic Sampling of Petroleum and
Petroleum Products (API MPMS Chapter 8.2)
1.1 This test method covers the determination of water in
D5854Practice for Mixing and Handling of Liquid Samples
the range from 0.02 to 5.00 mass or volume % in crude oils.
− of Petroleum and Petroleum Products (API MPMS Chap-
Mercaptan (RSH) and sulfide (S or H S) as sulfur are known
2
ter 8.3)
to interfere with this test method, but at levels of less than
E203Test Method for Water Using Volumetric Karl Fischer
500µg/g [ppm(m)], the interference from these compounds is
Titration
insignificant (see Section 6).
3
2.2 API Standards:
1.2 This test method can be used to determine water in the
MPMS Chapter 8.1Practice for Manual Sampling of Petro-
0.005 to 0.02 mass % range, but the effects of the mercaptan
leum and Petroleum Products (ASTM Practice D4057)
and sulfide interference at these levels has not been deter-
MPMS Chapter 8.2Practice for Automatic Sampling of
mined. For the range 0.005 to 0.02 mass %, there is no
Petroleum and Petroleum Products (ASTM Practice
precision or bias statement.
D4177)
1.3 This test method is intended for use with standard MPMS Chapter 8.3Practice for Mixing and Handling of
commercially available coulometric Karl Fischer reagent. Liquid Samples of Petroleum and Petroleum Products
(ASTM Practice D5854)
1.4 The values stated in SI units are to be regarded as
standard. No other units of measurement are included in this
3. Terminology
standard.
3.1 The following terms are used with respect to sampling
1.5 This standard does not purport to address all of the
(see Section 9).
safety concerns, if any, associated with its use. It is the
3.2 Definitions of Terms Specific to This Standard:
responsibility of the user of this standard to establish appro-
3.2.1 aliquot, n—asmallportionofalargersamplewhichis
priate safety and health practices and determine the applica-
analyzed and assumed to represent the whole sample.
bility of regulatory limitations prior to use. For specific
warning statements, see Section 8.
3.2.2 sample, n—portion extracted from the contents of any
pipe,tank,orothersystem,andintendedtoberepresentativeof
2. Referenced Documents
that system, placed in a primary sample container for analysis.
2
2.1 ASTM Standards:
3.2.3 test specimen, n—the representative sample taken
D1193Specification for Reagent Water
fromtheprimaryorintermediatesample(aliquot)containerfor
D4057Practice for Manual Sampling of Petroleum and
analysis. The entire test specimen is used in the analysis.
Petroleum Products (API MPMS Chapter 8.1)
4. Summary of Test Method
1 4.1 After homogenizing the crude oil sample, a test speci-
This test method is under the jurisdiction of ASTM Committee D02 on
Petroleum Products, Liquid Fuels, and Lubricants and the API Committee on men of that sample is injected into the titration cell of a Karl
Petroleum Measurement and is the direct responsibility of Subcommittee D02.02
Fischer apparatus in which iodine for the Karl Fischer reaction
/COMQ on Hydrocarbon Measurement for Custody Transfer (Joint ASTM-API).
is generated coulometrically at the anode. When all the water
Current edition approved Dec. 1, 2012. Published April 2013. Originally
has been titrated, excess iodine is detected by an electrometric
approved in 1989. Last previous edition approved in 2011 as D4928–11. DOI:
10.1520/D4928-12.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
3
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM Published as Manual of Petroleum Standards. Available from American
Standards volume information, refer to the standard’s Document Summary page on Petroleum Institute (API), 1220 L. St., NW, Washington, DC 20005-4070, http://
the ASTM website. 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
1
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D4928 − 12
endpoint detector and the titration is terminated. Based on the 7.2.2 Circulating Samp
...
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.
Designation: D4928 − 11 D4928 − 12
Manual of Petroleum Measurement Standards (MPMS), Chapter 10.9
Designation: 386/99
Standard Test Method for
1
Water in Crude Oils by Coulometric Karl Fischer Titration
This standard is issued under the fixed designation D4928; 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*
1.1 This test method covers the determination of water in the range from 0.02 to 55.00 mass or volume % in crude oils.
−
Mercaptan (RSH) and sulfide (S or H S) as sulfur are known to interfere with this test method, but at levels of less than 500 μg/g
2
(ppm),[ppm(m)], the interference from these compounds is insignificant (see Section 56).
1.2 This test method can be used to determine water in the 0.005 to 0.02 mass % range, but the effects of the mercaptan and
sulfide interference at these levels has not been determined. For the range 0.005 to 0.02 mass %, there is no precision or bias
statement.
1.3 This test method is intended for use with standard commercially available coulometric Karl Fischer reagent.
1.4 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.5 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 specific hazardwarning statements, see Section 78.
2. Referenced Documents
2
2.1 ASTM Standards:
D1193 Specification for Reagent Water
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)
E203 Test Method for Water Using Volumetric Karl Fischer Titration
3
2.2 API Standards:
MPMS Chapter 8.1 Practice for Manual Sampling of Petroleum and Petroleum Products (ASTM Practice D4057)
MPMS Chapter 8.2 Practice for Automatic Sampling of Petroleum and Petroleum Products (ASTM Practice D4177)
MPMS Chapter 8.3 Practice for Mixing and Handling of Liquid Samples of Petroleum and Petroleum Products (ASTM Practice
D5854)
3. Terminology
3.1 The following terms are used with respect to sampling (see Section 9).
3.2 Definitions of Terms Specific to This Standard:
3.2.1 aliquot, n—a small portion of a larger sample which is analyzed and assumed to represent the whole sample.
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 /COMQ on Hydrocarbon Measurement for Custody Transfer (Joint ASTM-API).
Current edition approved June 1, 2011Dec. 1, 2012. Published August 2011April 2013. Originally approved in 1989. Last previous edition approved in 20102011 as
D4928–00 (2010). –11. DOI: 10.1520/D4928-11.10.1520/D4928-12.
2
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.
3
Published as Manual of Petroleum 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
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1
---------------------- Page: 1 ----------------------
D4928 − 12
3.2.2 sample, n—portion extracted from the contents of any pipe, tank, or other system, and intended to be representative of that
system, placed in a primary sample container for analysis.
3.2.3 test specimen, n—the representative sample taken from the primary or intermediate sample (aliquot) container for analysis.
The entire test specimen is used in the analysis.
4. Summary of Test Method
4.1 After homogenizing the crude oil with a mixer, an aliquot sample, a test specimen of that samp
...
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