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ASTM D4006-22

(Test Method)

Standard Test Method for Water in Crude Oil by Distillation

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.

General Information

Status
Published
Publication Date
30-Sep-2022
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

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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: D4006 − 22
Manual of Petroleum Measurement Standards (MPMS), Chapter 10.2
Standard Test Method for
1
Water in Crude Oil by Distillation
This standard is issued under the fixed designation D4006; 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.
1. Scope* Inhibited Mineral Oil in the Presence of Water
D1796Test Method for Water and Sediment in Fuel Oils by
1.1 This test method covers the determination of water in
the Centrifuge Method (Laboratory Procedure) (API
crude oil by distillation.
MPMS Chapter 10.6)
1.2 The values stated in SI units are to be regarded as
D4057Practice for Manual Sampling of Petroleum and
standard. No other units of measurement are included in this
Petroleum Products (API MPMS Chapter 8.1)
standard.
D4175Terminology Relating to Petroleum Products, Liquid
1.3 This standard does not purport to address all of the Fuels, and Lubricants
safety concerns, if any, associated with its use. It is the
D4177Practice for Automatic Sampling of Petroleum and
responsibility of the user of this standard to establish appro- Petroleum Products (API MPMS Chapter 8.2)
priate safety, health, and environmental practices and deter-
D4928Test Method forWater in Crude Oils by Coulometric
mine the applicability of regulatory limitations prior to use. Karl Fischer Titration (API MPMS Chapter 10.9)
For specific warning statements, see 7.1 and A1.1.
E123SpecificationforApparatusforDeterminationofWater
1.4 This international standard was developed in accor- by Distillation
dance with internationally recognized principles on standard-
2.2 API Standards:
ization established in the Decision on Principles for the MPMS Chapter 1Terms and Definitions Database
Development of International Standards, Guides and Recom-
MPMS Chapter 8.1Manual Sampling of Petroleum and
mendations issued by the World Trade Organization Technical Petroleum Products (ASTM Practice D4057)
Barriers to Trade (TBT) Committee.
MPMS Chapter 8.2Automatic Sampling of Petroleum and
Petroleum Products (ASTM Practice D4177)
2. Referenced Documents
MPMS Chapter 10.1Test Method for Sediment in Crude
2
Oils and Fuel Oils by the Extraction Method (ASTMTest
2.1 ASTM Standards:
Method D473)
D95Test Method for Water in Petroleum Products and
MPMS Chapter 10.4Determination of Water and/or Sedi-
BituminousMaterialsbyDistillation(API MPMSChapter
ment in Crude Oil by the Centrifuge Method (Field
10.5)
Procedure)
D473TestMethodforSedimentinCrudeOilsandFuelOils
MPMS Chapter 10.5Test Method for Water in Petroleum
by the Extraction Method (API MPMS Chapter 10.1)
Products and Bituminous Materials by Distillation
D665Test Method for Rust-Preventing Characteristics of
(ASTM Test Method D95)
MPMSChapter10.6TestMethodforWaterandSedimentin
1
This test method is under the jurisdiction of ASTM Committee D02 on
Fuel Oils by the Centrifuge Method (Laboratory Proce-
Petroleum Products, Liquid Fuels, and Lubricants and the API Committee on
dure) (ASTM Test Method D1796)
Petroleum Measurement and is the direct responsibility of Subcommittee D02.02
MPMSChapter10.9TestMethodforWaterinCrudeOilsby
/COMQ the joint ASTM-API Committee on Hydrocarbon Measurement for
Custody Transfer (Joint ASTM-API). This test method has been approved by the Coulometric Karl Fischer Titration (ASTM Test Method
sponsoring committees and accepted by the Cooperating Societies in accordance
D4928)
with established procedures.
Current edition approved Oct. 1, 2022. Published December 2022. Originally
3. Terminology
ɛ1
approved in 1981. Last previous edition approved in 2016 as D4006–16 . DOI:
10.1520/D4006-22.
3.1 Definitions:
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
3.1.1 For definitions of terms used in this test method, refer
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
to Terminology D4175 and the API MPMS Chapter 1 Terms
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. and Definitions Database.
*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

---------------------- Page: 1 ----------------------
D4006 − 22
trap with 0.05mL g
...

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: D4006 − 16 D4006 − 22
Manual of Petroleum Measurement Standards (MPMS), Chapter 10.2
Standard Test Method for
1
Water in Crude Oil by Distillation
This standard is issued under the fixed designation D4006; 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
ε NOTE—Subsections 5.1 and X1.3.3.2 were revised editorially in November 2016.
1. 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 safety, health, and healthenvironmental practices and determine the
applicability of regulatory limitations prior to use. For specific warning statements, see 6.17.1 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.
2. Referenced Documents
2
2.1 ASTM Standards:
D95 Test Method for Water in Petroleum Products and Bituminous Materials by Distillation (API MPMS Chapter 10.5)
D473 Test Method for Sediment in Crude Oils and Fuel Oils by the Extraction Method (API MPMS Chapter 10.1)
D665 Test Method for Rust-Preventing Characteristics of Inhibited Mineral Oil in the Presence of Water
D1796 Test Method for Water and Sediment in Fuel Oils by the Centrifuge Method (Laboratory Procedure) (API MPMS Chapter
10.6)
D4057 Practice for Manual Sampling of Petroleum and Petroleum Products (API MPMS Chapter 8.1)
D4175 Terminology Relating to Petroleum Products, Liquid Fuels, and Lubricants
D4177 Practice for Automatic Sampling of Petroleum and Petroleum Products (API MPMS Chapter 8.2)
D4928 Test Method for Water in Crude Oils by Coulometric Karl Fischer Titration (API MPMS Chapter 10.9)
E123 Specification for Apparatus for Determination of Water by Distillation
2.2 API Standards:
MPMS Chapter 1 Terms and Definitions Database
MPMS Chapter 8.1 Manual Sampling of Petroleum and Petroleum Products (ASTM Practice D4057)
1
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 Custody Transfer (Joint
ASTM-API). This test method has been approved by the sponsoring committees and accepted by the Cooperating Societies in accordance with established procedures.
Current edition approved June 1, 2016Oct. 1, 2022. Published July 2016December 2022. Originally approved in 1981. Last previous edition approved in 20122016 as
ɛ1
D4006 – 11 (2012)D4006 – 16 . DOI: 10.1520/D4006-16E01.10.1520/D4006-22.
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.
*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

---------------------- Page: 1 ----------------------
D4006 − 22
MPMS Chapter 8.2 Automatic Sampling of Petroleum and Petroleum Products (ASTM Practice D4177)
MPMS Chapter 10.1 Test Method for Sediment in Crude Oils and Fuel Oils by the Extraction Method (ASTM Test Method
D473)
MPMS Chapter 10.4 Determination of Water and/or Sediment in Crude Oil by the Centrifuge Method (Field Procedure)
MPMS Chapter 10.5 Test Method for Water in Petroleum Products and Bituminous Materials by Distillation (ASTM Test
Method D95)
MPMS Chapter 10.6 Test Method for Water and Sediment in Fuel Oils by the Centrifuge Method (Laboratory P
...

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SIGNIFICANCE AND USE
5.1 Most often determined trace elements in crude oils are nickel and vanadium, which are usually the most abundant; however, as many as 45 elements in crude oils have been reported. Knowledge of trace elements in crude oil is important because they can have an adverse effect on petroleum refining and product quality. These effects can include catalyst poisoning in the refinery and excessive atmospheric emission in combustion of fuels. Trace element concentrations are also useful in correlating production from different wells and horizons in a field. Elements such as iron, arsenic, and lead are catalyst poisons. Vanadium compounds can cause refractory damage in furnaces, and sodium compounds have been found to cause superficial fusion on fire brick. Some organometallic compounds are volatile which can lead to the contamination of distillate fractions, and a reduction in their stability or malfunctions of equipment when they are combusted.  
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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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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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SIGNIFICANCE AND USE
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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 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 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 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.  
1.2 The procedures in this test method involve 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 Procedure A covers the determination of organic chloride in the washed naphtha fraction of crude oil by sodium biphenyl reduction followed by potentiometric titration.  
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
ASTM D473-22(Test Method)
Standard Test Method for Sediment in Crude Oils and Fuel Oils by the Extraction Method

SIGNIFICANCE AND USE
5.1 A knowledge of the sediment content of crude oils and fuel oils is important both to the operation of refining and the buying or selling of these commodities.
SCOPE
1.1 This test method covers the determination of sediment in crude oils and fuel oils by extraction with toluene. The precision applies to a range of sediment levels from 0.01 % to 0.40 % mass, although higher levels may be determined.
Note 1: Precision on recycled oils and crankcase oils is unknown and additional testing is required to determine that precision.  
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 6.1.1.6 and 7.1.  
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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