Standard Test Method for Water in Crude Oils by Potentiometric Karl Fischer Titration

SCOPE
1.1 This test method covers the determination of water in the range from 0.02 to 2 % in crude oils. Mercaptan and sulfide (S or H2S) sulfur are known to interfere with this test method (see Section 5).
1.2 This test method is intended for use with standard Karl Fischer reagent or pyridine-free Karl Fischer reagents.
1.3 The values stated in SI units are to be regarded as the 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 and health practices and determine the applicability of regulatory limitations prior to use. Specific precautionary statements are given in Section 7.

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Historical
Publication Date
09-Aug-2000
Current Stage
Ref Project

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ASTM D4377-00e1 - Standard Test Method for Water in Crude Oils by Potentiometric Karl Fischer Titration
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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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
AnAmerican National Standard
e1
Designation:D4377–00
Designation: Manual of Petroleum Measurement Standards (MPMS), Chapter 10.7
Designation: 356/99
Standard Test Method for
1
Water in Crude Oils by Potentiometric Karl Fischer Titration
This standard is issued under the fixed designation D4377; 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 (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
e NOTE—Footnote 1 and the Referenced Documents were corrected editorially to comply with theASTM-API joint standard
contract in October 2002.
1. Scope E203 TestMethodforWaterUsingVolumetricKarlFischer
4
Reagent
1.1 This test method covers the determination of water in
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2.2 API Standards:
therangefrom0.02to2%incrudeoils.Mercaptanandsulfide

MPMS Chapter 8.1 Manual Sampling of Petroleum and
(S or H S) sulfur are known to interfere with this test method
2
Petroleum Products (ASTM Practice D4057)
(see Section 5).
MPMS Chapter 8.2 Automatic Sampling of Petroleum and
1.2 This test method is intended for use with standard Karl
Petroleum Products (ASTM Practice D4177)
Fischer reagent or pyridine-free Karl Fischer reagents.
MPMS Chapter 10.2 Determination of Water in Crude Oil
1.3 The values stated in SI units are to be regarded as the
by Distillation (ASTM Test Method D4006)
standard.
1.4 This standard does not purport to address all of the
3. Summary of Test Method
safety concerns, if any, associated with its use. It is the
3.1 After homogenizing the crude oil with a mixer, an
responsibility of the user of this standard to establish appro-
aliquot of the crude, in a mixed solvent, is titrated to an
priate safety and health practices and determine the applica-
electrometric end-point using Karl Fischer reagent.
bility of regulatory limitations prior to use. Specific precau-
tionary statements are given in Section 7.
4. Significance and Use
4.1 A knowledge of the water content of crude oil is
2. Referenced Documents
important in the refining, purchase, sale, or transfer of crude
2.1 ASTM Standards:
2 oils.
D1193 Specification for Reagent Water
D4006 Test Method for Water in Crude Oil by Distillation
5. Interferences
3
(API MPMS Chapter 10.2)
5.1 A number of substances and class of compounds asso-
D4057 Practice for Manual Sampling of Petroleum and
3 ciated with condensation or oxidation-reduction reactions in-
Petroleum Products (API MPMS Chapter 8.1)
terfere in the determination of water by Karl Fischer. In crude
D4177 Practice for Automatic Sampling of Petroleum and
3 oils, the most common interferences are mercaptans and
Petroleum Products (API MPMS Chapter 8.2)
sulfides. At levels of less than 500 µg/g (ppm) (as sulfur) the
interference from these compounds is insignificant. For more
informationonsubstancesthatinterfereinthedeterminationof
1
This test method is under the jurisdiction of ASTM Committee D02 on
waterusingthe(KarlFischerreagent)titrationmethodseeTest
Petroleum Products and Lubricants and theAPI Committee on Petroleum Measure-
Method E203.
ment, and is the direct responsibility of Subcommittee D02.02 /COMQ, the joint
ASTM-API Committee on Static Petroleum Measurement.
Current edition approved Aug. 10, 2000. Published October 2000. Originally
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published as D4377–84. Last previous edition D4377–93a. Annual Book of ASTM Standards, Vol 15.05.
2 5
Annual Book of ASTM Standards, Vol 11.01. Published as Manual of Petroleum Measurement Standards.Available from the
3
Annual Book of ASTM Standards, Vol 05.02. AmericanPetroleumInstitute(API),1220LSt.,NW,Washington,DC20005-4070.
Copyright ©ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA19428-2959, United States.
1

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D4377–00
6. Apparatus of water)—Fresh Karl Fischer reagent must be used. Must be
used with solvent in 7.6.1.(Warning—Combustible. Harmful
6.1 Karl Fischer Apparatus, using electrometric end-point.
if swallowed, inhaled, or absorbed through the skin.)
A suggested assembly of the apparatus is described in Annex
7.4.2 Pyridine-Free Karl Fischer (one-component) reagent
A2.
diluted with xylene—Dilute three parts pyridine-free Karl
6.1.1 Presently there is available on the market commercial
8
Fischer (one-component) reagent (1 mL=5 mg water) to 1
Karl Fischer titration assemblies, some of which automatically
part xylene. Fresh Karl Fischer reagent must be used.
stop the titration at the end-point. Instructions for operation of
(Warning—See 7.4.1) Must be used with solvent in 7.6.2.
these devices are provided by the manufacturer and not
7.5 Methano
...

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