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ASTM D4377-00(2011)

(Test Method)

Standard Test Method for Water in Crude Oils by Potentiometric Karl Fischer Titration (Withdrawn 2020)

Standard Test Method for Water in Crude Oils by Potentiometric Karl Fischer Titration (Withdrawn 2020)

SIGNIFICANCE AND USE
A knowledge of the water content of crude oil 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 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 standard. No other units of measurement are included in this 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.
WITHDRAWN RATIONALE
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.
Formerly under the jurisdiction of Committee D02 on Petroleum Products, Liquid Fuels, and Lubricants, this test method was withdrawn in January 2020 in accordance with section 10.6.3 of the Regulations Governing ASTM Technical Committees, which requires that standards shall be updated by the end of the eighth year since the last approval date.

General Information

Status
Withdrawn
Publication Date
31-May-2011
Withdrawal Date
08-Jan-2020
ICS
75.040 - Crude petroleum
Technical Committee
D02 - Petroleum Products, Liquid Fuels, and Lubricants
Drafting Committee
D02.02 - Hydrocarbon Measurement for Custody Transfer (Joint ASTM-API)
Current Stage
Ref Project

Relations

Referred By
ASTM F3337-19 - Standard Guide for Taking Property and Behavior Measurements on Weathered Fractions of Oil
Effective Date
01-Jun-2011
Referred By
ASTM D7829-13(2018) - Standard Guide for Sediment and Water Determination in Crude Oil
Effective Date
01-Jun-2011
Referred By
ASTM G205-16 - Standard Guide for Determining Emulsion Properties, Wetting Behavior, and Corrosion-Inhibitory Properties of Crude Oils
Effective Date
01-Jun-2011
Referred By
ASTM D6470-99(2020) - Standard Test Method for Salt in Crude Oils (Potentiometric Method)
Effective Date
01-Jun-2011
Referred By
ASTM D4052-22 - Standard Test Method for Density, Relative Density, and API Gravity of Liquids by Digital Density Meter
Effective Date
01-Jun-2011
Referred By
ASTM D7785-21 - Standard Practice for Water in Lint Cotton by Oven Evaporation Combined with Volumetric Karl Fischer Titration
Effective Date
01-Jun-2011
Referred By
ASTM D5002-22 - Standard Test Method for Density, Relative Density, and API Gravity of Crude Oils by Digital Density Analyzer
Effective Date
01-Jun-2011
Referred By
ASTM D6448-16(2022) - Standard Specification for Industrial Burner Fuels from Used Lubricating Oils
Effective Date
01-Jun-2011

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ASTM D4377-00(2011) - Standard Test Method for Water in Crude Oils by Potentiometric Karl Fischer Titration (Withdrawn 2020)ASTM D4377-00(2011) - Standard Test Method for Water in Crude Oils by Potentiometric Karl Fischer Titration (Withdrawn 2020)
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ASTM D4377-00(2011) - Standard Test Method for Water in Crude Oils by Potentiometric Karl Fischer Titration (Withdrawn 2020)
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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
Designation: D4377 − 00 (Reapproved 2011)
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 (´) 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.
3
1. Scope 2.2 API Standards:
MPMS Chapter 8.1Manual Sampling of Petroleum and
1.1 This test method covers the determination of water in
Petroleum Products (ASTM Practice D4057)
therangefrom0.02to2%incrudeoils.Mercaptanandsulfide
− MPMS Chapter 8.2Automatic Sampling of Petroleum and
(S or H S) sulfur are known to interfere with this test method
2
Petroleum Products (ASTM Practice D4177)
(see Section 5).
MPMSChapter10.2DeterminationofWaterinCrudeOilby
1.2 This test method is intended for use with standard Karl
Distillation (ASTM Test Method D4006)
Fischer reagent or pyridine-free Karl Fischer reagents.
3. Summary of Test Method
1.3 The values stated in SI units are to be regarded as
standard. No other units of measurement are included in this
3.1 After homogenizing the crude oil with a mixer, an
standard.
aliquot of the crude, in a mixed solvent, is titrated to an
electrometric end-point using Karl Fischer reagent.
1.4 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the
4. Significance and Use
responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica-
4.1 A knowledge of the water content of crude oil is
bility of regulatory limitations prior to use. Specific precau-
important in the refining, purchase, sale, or transfer of crude
tionary statements are given in Section 7.
oils.
2. Referenced Documents
5. Interferences
2
2.1 ASTM Standards:
5.1 A number of substances and class of compounds asso-
D1193Specification for Reagent Water
ciated with condensation or oxidation-reduction reactions in-
D4006Test Method for Water in Crude Oil by Distillation
terfere in the determination of water by Karl Fischer. In crude
D4057Practice for Manual Sampling of Petroleum and
oils, the most common interferences are mercaptans and
Petroleum Products
sulfides. At levels of less than 500 µg/g (ppm) (as sulfur) the
D4177Practice for Automatic Sampling of Petroleum and
interference from these compounds is insignificant. For more
Petroleum Products
informationonsubstancesthatinterfereinthedeterminationof
E203Test Method for Water Using Volumetric Karl Fischer
waterusingthe(KarlFischerreagent)titrationmethodseeTest
Titration
Method E203.
1
6. Apparatus
This test method is under the jurisdiction of ASTM Committee D02 on
Petroleum Products, Liquid Fuels, and Lubricants and the API Committee on
6.1 Karl Fischer Apparatus, using electrometric end-point.
Petroleum Measurement, and is the direct responsibility of Subcommittee D02.02
A suggested assembly of the apparatus is described in Annex
/COMQ on Hydrocarbon Measurement for Custody Transfer (Joint ASTM-API).
Current edition approved June 1, 2011. Published August 2011. Originally
A2.
approved in 1984. Last previous edition approved in 2006 as D4377–00(2006).
DOI: 10.1520/D4377-00R11.
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 Measurement Standards. Available from
Standards volume information, refer to the standard’s Document Summary page on AmericanPetroleumInstitute(API),1220L.St.,NW,Washington,DC20005-4070,
the ASTM website. http://api-ec.api.org.
© Jointly copyrighted byASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA19428-2959, USAand theAmerican Petroleum Institute (API), 1220 L Street NW, Washington DC 20005, USA
1

---------------------- Page: 1 ----------------------
D4377 − 00 (2011)
6.1.1 Presently there is available on the market commercial 7.4.2 Pyridine-Free Karl Fischer (one-component) reagent
Karl Fischer titration assemblies, some of which automatically diluted with xylene—Dilute three parts pyridine-free Karl
6
stop the titration at the end-point. Instructions for operation of Fischer (one-component) reagent (1 mL=5 mg water) to 1
these devices are provided by the manufacturer and not part xylene. Fresh Karl Fischer reagent must be used.
described herein.This test method is not intended for use with (Warning—See 7.4.1) Must be used with solvent in 7.6.2.
coulometric Karl Fis
...

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1.1 This test method covers the determination of several elements (including iron, nickel, sulfur, and vanadium) occurring in crude oils.  
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1.4 Because of the particulates present in crude oil samples, if they do not dissolve in the organic solvents used or if they do not get aspirated in the nebulizer, low elemental values may result, particularly for iron and sodium. This can also occur if the elements are associated with water which can drop out of the solution when diluted with solvent.  
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1.5 This test method uses oil-soluble metals for calibration and does not purport to quantitatively determine insoluble particulates. Analytical results are particle size dependent and low results may be obtained for particles larger than a few micrometers.  
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5.1 This test method describes a sensitive method for estimating the intrinsic stability of an oil. The intrinsic stability is expressed as S-value. An oil with a low S-value is likely to undergo flocculation of asphaltenes when stressed (for example, extended heated storage) or blended with a range of other oils. Two oils each with a high S-value are likely to maintain asphaltenes in a peptized state and not lead to asphaltene flocculation when blended together.  
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1.1 This test method covers procedures for quantifying the intrinsic stability of the asphaltenes in an oil by automatic instruments using optical detection.  
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5.1 Crude oils and oil sands bitumen contain naturally occurring acidic species. Acidity of crude oil has been implicated in corrosion of distribution and process systems. The relative amount of these materials can be determined by titrating with bases. The acid number is a measure of this amount of acidic substance in the oil under the conditions of the test.  
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Standard Test Methods for Determination of Nickel, Vanadium, Iron, and Sodium in Crude Oils and Residual Fuels by Flame Atomic Absorption Spectrometry

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5.1 When fuels are combusted, metals present in the fuels can form low melting compounds that are corrosive to metal parts. Metals present at trace levels in petroleum can deactivate catalysts during processing. These test methods provide a means of quantitatively determining the concentrations of vanadium, nickel, iron, and sodium. Thus, these test methods can be used to aid in determining the quality and value of the crude oil and residual oil.
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1.1 This test method covers and is used to evaluate the tendency of inhibited mineral oil based steam turbine lubricants and mineral oil based anti-wear hydraulic oils to corrode copper catalyst metal and to form sludge during oxidation in the presence of oxygen, water, and copper and iron metals at an elevated temperature. The test method is also used for testing circulating oils having a specific gravity less than that of water and containing rust and oxidation inhibitors.  
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1.2 This test method is a modification of Test Method D943 where the oxidation stability of the same kinds of oils is determined by following the acid number of oil. The number of test hours required for the oil to reach an acid number of 2.0 mg KOH/g is the oxidation lifetime.  
1.3 Procedure A of this test method requires the determination and report of the weight of the sludge and the total amount of copper in the oil, water, and sludge phases. Procedure B requires the sludge determination only. The acid number determination is optional for both procedures.  
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1.5 WARNING—Mercury has been designated by many regulatory agencies as a hazardous substance that can cause serious medical issues. Mercury, or its vapor, has been demonstrated to be hazardous to health and corrosive to materials. Use Caution when handling mercury and mercury-containing products. See the applicable product Safety Data Sheet (SDS) for additional information. The potential exists that selling mercury or mercury-containing products, or both, is prohibited by local or national law. Users must determine legality of sales in their location.  
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Standard Test Method for Water and Sediment in Crude Oil by the Centrifuge Method (Laboratory Procedure)

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5.1 The water and sediment content of crude oil is significant because it can cause corrosion of equipment and problems in processing. A determination of water and sediment content is required to measure accurately net volumes of actual oil in sales, taxation, exchanges, and custody transfers. It is not anticipated that this test method, which is written with a dedicated laboratory facility in mind, is likely to be used in field test rooms or sample rooms due to safety concerns for proper ventilation and handling.  
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SCOPE
1.1 This test method describes the laboratory determination of water and sediment in crude oils by means of the centrifuge procedure. This centrifuge method for determining water and sediment in crude oils is not entirely satisfactory. The amount of water detected is almost always lower than the actual water content. When a highly accurate value is required, the revised procedures for water by distillation, Test Method D4006 (API MPMS Chapter 10.2) (Note 1), and sediment by extraction, Test Method D473 (API MPMS Chapter 10.1), shall be used.  
Note 1: Test Method D4006 (API MPMS Chapter 10.2) has been determined to be the preferred and most accurate method for the determination of water.  
1.2 The values stated in SI units are to be regarded as standard.  
1.2.1 Exception—The values given in parentheses are for information only.  
1.3 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. Specific warning statements appear in 7.1, 9.3, and A1.5.4.  
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ASTM D4929-22(Test Method)
Standard Test Method for Determination of Organic Chloride Content in Crude Oil

SIGNIFICANCE AND USE
5.1 Organic chlorides do not occur naturally in crude oil. When present, they result from contamination in some manner, such as disposal of chlorinated solvent used in many dewaxing pipeline or other equipment operations.  
5.1.1 Uncontaminated crude oil will contain no detectable organic chloride, and most refineries can handle very small amounts without deleterious effects.
5.1.1.1 Most trade contracts specify that no organic chloride is present in the crude oil.  
5.1.2 Several pipelines have set specification limits at  
5.1.2.1 To ensure Eq 3).  
5.1.3 Organic chloride present in the crude oil (for example, methylene chloride, perchloroethylene, etc.) is usually distilled into the naphtha fraction. Some compounds break down during fractionation and produce hydrochloric acid, which has a corrosive effect. Some compounds survive fractionation and are destroyed during hydro-treating (desulfurization of the naphtha).  
5.2 Other halides can also be used for dewaxing crude oil; in such cases, any organic halides will have similar impact on the refining operations as the organic chlorides.  
5.3 Organic chloride species are potentially damaging to refinery processes. Hydrochloric acid can be produced in hydrotreating or reforming reactors and the acid accumulates in condensing regions of the refinery. Unexpected concentrations of organic chlorides cannot be effectively neutralized and damage can result. Organic chlorides are not known to be naturally present in crude oils and usually result from cleaning operations at producing sites, pipelines, or tanks. It is important for the oil industry to have common methods available for the determination of organic chlorides in crude oil, particularly when transfer of custody is involved.
SCOPE
1.1 The procedures in this test method cover the determination of organic chloride (above 1 μg/g organically-bound chlorine) in crude oils, using either distillation and sodium biphenyl reduction, distillation and microcoulometry, or distillation and X-ray fluorescence (XRF) spectrometry.  
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1.4 Procedure B covers the determination of organic chloride in the washed naphtha fraction of crude oil by oxidative combustion followed by microcoulometric titration.  
1.5 Procedure C covers the determination of organic chloride in the washed naphtha fraction of crude oil by X-ray fluorescence spectrometry.  
1.6 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.6.1 The preferred concentration units are micrograms of chloride per gram of sample, though milligrams of chloride per kilogram of sample is commonly used for Procedure C.  
1.7 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.  
1.8 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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ASTM D8150-22(Test Method)
Standard Test Method for Determination of Organic Chloride Content in Crude Oil by Distillation Followed by Detection Using Combustion Ion Chromatography

SIGNIFICANCE AND USE
5.1 Organic chlorides do not occur naturally in crude oil. When present, they result from contamination in some manner, such as disposal of chlorinated solvent used in many dewaxing pipeline or other equipment operations.  
5.1.1 Uncontaminated crude oil will contain no detectable organic chloride, and most refineries can handle very small amounts without deleterious effects.
5.1.1.1 Most trade contracts specify that no organic chloride is present in the crude oil.  
5.1.2 Several pipelines have set specification limits less than 1 μg/g organic chlorides in the whole crude, and less than 5 μg/g in the light naphtha, based on the yield of naphtha being 20 % of the original sample.
5.1.2.1 To ensure less than 1 μg/g organic chloride in the crude oil, the amount measured in the naphtha fraction shall be less than 1/f (where f is the naphtha fraction calculated with Eq 1). For example, a crude oil sample with 1 μg/g of organic chloride but a 10 % yield of naphtha would create a naphtha containing 10 μg/g organic chloride. Further, a crude containing 1 μg/g of organic chloride but a 40 % yield of naphtha would create a naphtha containing 2.5 μg/g organic chloride. Due to the difference in naphtha yields, the impact on refining operations can be significantly different.
5.1.2.2 Since crude oil deposits worldwide exhibit different yields of naphtha, the working range of detection for this method shall cover a broad range, possibly as high as 50 μg/g in a naphtha fraction.  
5.1.3 Organic chloride present in the crude oil (for example, methylene chloride, perchloroethylene, etc.) is usually distilled into the naphtha fraction. Some compounds break down during fractionation and produce hydrochloric acid, which has a corrosive effect. Some compounds survive fractionation and are destroyed during hydro-treating (desulfurization of the naphtha).  
5.2 Other halides can also be used for dewaxing crude oil; in such cases, any organic halides will have similar impact on ...
SCOPE
1.1 This test method covers the determination of organic chloride (above 1 μg/g organically-bound chlorine) in crude oils, using distillation and combustion ion chromatography.  
1.2 This test method involves the distillation of crude oil test specimens to obtain a naphtha fraction prior to chloride determination. The chloride content of the naphtha fraction of the whole crude oil can thereby be obtained. See Section 6 regarding potential interferences.  
1.3 The test procedure covers the determination of organic chloride in the washed naphtha fraction of crude oil by combustion ion chromatography. Other halides can be determined but are not included in the precision statement of the test method.  
1.4 The values stated in SI units are to be regarded as standard. The preferred concentration units are micrograms of chloride per gram of sample.  
1.4.1 Exception—The values given in parentheses are for information only.  
1.5 Warning—Mercury has been designated by many regulatory agencies as a hazardous substance that can cause serious medical issues. Mercury, or its vapor, has been demonstrated to be hazardous to health and corrosive to materials. Use caution when handling mercury and mercury-containing products. See the applicable product Safety Data Sheet (SDS) for additional information. The potential exists that selling mercury or mercury-containing products, or both, is prohibited by local or national law. Users must determine legality of sales in their location.  
1.6 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.  
1.7 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision ...

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ASTM
ASTM D4006-22(Test Method)
Standard Test Method for Water in Crude Oil by Distillation

SIGNIFICANCE AND USE
5.1 A knowledge of the water content of crude oil is important in the refining, purchase, sale, or transfer of crude oils.  
5.2 This test method may not be suitable for crude oils that contain alcohols that are soluble in water. In cases where the impact on the results may be significant, the user is advised to consider using another test method, such as Test Method D4928 (API MPMS Chapter 10.9).
SCOPE
1.1 This test method covers the determination of water in crude oil by distillation.  
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.3 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 warning statements, see 7.1 and A1.1.  
1.4 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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