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ASTM D3230-19

(Test Method)

Standard Test Method for Salts in Crude Oil (Electrometric Method)

Standard Test Method for Salts in Crude Oil (Electrometric Method)

SIGNIFICANCE AND USE
5.1 This test method is used to determine the approximate chloride content of crude oils, a knowledge of which is important in deciding whether or not the crude oil needs desalting. The efficiency of the process desalter can also be evaluated.  
5.2 Excessive chloride left in the crude oil frequently results in higher corrosion rates in refining units and also has detrimental effects on catalysts used in these units.  
5.3 This test method provides a rapid and convenient means of determining the approximate content of chlorides in crude oil and is useful to crude oil processors.
SCOPE
1.1 This test method covers the determination of the approximate chloride (salts) concentration in crude oil. The range of concentration covered is 3.5 mg/kg to 500 mg/kg or 1.0 lb/1000 bbl to 150 lb/1000 bbl (PTB) as chloride concentration/volume of crude oil.  
1.2 This test method measures conductivity in the crude oil due to the presence of common chlorides, such as sodium, calcium, and magnesium. Other conductive materials may also be present in the crude oil.  
1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.3.1 Exception—Acceptable concentration units are g/m3 or PTB (lb/1000 bbl).  
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 warning statements, see 7.3, 7.4, and 7.11.  
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.

General Information

Status
Published
Publication Date
30-Apr-2019
ICS
75.040 - Crude petroleum
Technical Committee
D02 - Petroleum Products, Liquid Fuels, and Lubricants
Drafting Committee
D02.03 - Elemental Analysis
Current Stage
Ref Project

Relations

Refers
ASTM D5002-15 - Standard Test Method for Density and Relative Density of Crude Oils by Digital Density Analyzer
Effective Date
15-Dec-2015

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REDLINE ASTM D3230-19 - Standard Test Method for Salts in Crude Oil (Electrometric Method)REDLINE ASTM D3230-19 - Standard Test Method for Salts in Crude Oil (Electrometric Method)
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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: D3230 − 19
Standard Test Method for
1
Salts in Crude Oil (Electrometric Method)
This standard is issued under the fixed designation D3230; 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* D1193 Specification for Reagent Water
D4928 Test Method for Water in Crude Oils by Coulometric
1.1 This test method covers the determination of the
Karl Fischer Titration
approximate chloride (salts) concentration in crude oil. The
D5002 Test Method for Density, Relative Density, and API
range of concentration covered is 3.5 mg⁄kg to 500 mg⁄kg or
Gravity of Crude Oils by Digital Density Analyzer
1.0 lb⁄1000 bbl to 150 lb⁄1000 bbl (PTB) as chloride
concentration/volume of crude oil.
3. Terminology
1.2 This test method measures conductivity in the crude oil
3.1 Definitions of Terms Specific to This Standard:
due to the presence of common chlorides, such as sodium,
3.1.1 PTB—lb/1000 bbl.
calcium, and magnesium. Other conductive materials may also
be present in the crude oil.
3.1.2 salts in crude oil—commonly, chlorides of sodium,
calcium, and magnesium dissolved in crude oil. Other inor-
1.3 The values stated in SI units are to be regarded as
ganic chlorides may also be present.
standard. No other units of measurement are included in this
standard.
3
4. Summary of Test Method
1.3.1 Exception—Acceptable concentration units are g/m
or PTB (lb/1000 bbl).
4.1 Thistestmethodmeasurestheconductivityofasolution
1.4 This standard does not purport to address all of the
of crude oil in a mixed alcohol solvent when subjected to an
safety concerns, if any, associated with its use. It is the
electrical stress.This test method measures conductivity due to
responsibility of the user of this standard to establish appro-
the presence of inorganic chlorides, and other conductive
priate safety, health, and environmental practices and deter-
material, in the crude oil. A homogenized test specimen is
mine the applicability of regulatory limitations prior to use.
dissolved in a mixed alcohol solvent and placed in a test cell
For specific warning statements, see 7.3, 7.4, and 7.11.
consisting of a beaker and a set of electrodes. A voltage is
1.5 This international standard was developed in accor-
impressed on the electrodes, and the resulting current flow is
dance with internationally recognized principles on standard-
measured. The chloride (salt) content is obtained by reference
ization established in the Decision on Principles for the
to a calibration curve of current versus chloride concentration
Development of International Standards, Guides and Recom-
of known mixtures. Calibration curves are based on standards
mendations issued by the World Trade Organization Technical
prepared to approximate the type and concentration of chlo-
Barriers to Trade (TBT) Committee.
rides in the crude oils being tested.
2. Referenced Documents
5. Significance and Use
2
2.1 ASTM Standards:
5.1 This test method is used to determine the approximate
D381 Test Method for Gum Content in Fuels by Jet Evapo-
chloride content of crude oils, a knowledge of which is
ration
important in deciding whether or not the crude oil needs
desalting. The efficiency of the process desalter can also be
1
This test method is under the jurisdiction of ASTM Committee D02 on
evaluated.
Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of
Subcommittee D02.03 on Elemental Analysis. 5.2 Excessivechlorideleftinthecrudeoilfrequentlyresults
Current edition approved May 1, 2019. Published May 2019. Originally
in higher corrosion rates in refining units and also has
approved in 1973. Last previous edition approved in 2018 as D3230 – 13 (2018).
detrimental effects on catalysts used in these units.
DOI: 10.1520/D3230-19.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
5.3 This test method provides a rapid and convenient means
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
of determining the approximate content of chlorides in crude
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. oil and is useful to crude oil processors.
*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

...

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: D3230 − 13 (Reapproved 2018) D3230 − 19
Standard Test Method for
1
Salts in Crude Oil (Electrometric Method)
This standard is issued under the fixed designation D3230; 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 Scope*
1.1 This test method covers the determination of the approximate chloride (salts) concentration in crude oil. The range of
concentration covered is 0 mg3.5 mg ⁄kg to 500 mg ⁄kg or 0 lb1.0 lb ⁄1000 bbl ⁄1000 bbl to 150 lb ⁄1000 bbl ⁄1000 bbl (PTB) as
chloride concentration/volume of crude oil.
1.2 This test method measures conductivity in the crude oil due to the presence of common chlorides, such as sodium, calcium,
and magnesium. Other conductive materials may also be present in the crude oil.
1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
3
1.3.1 Exception—Acceptable concentration units are g/m or PTB (lb/1000 bbl).
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 warning statements, see 7.3, 7.4, and 7.11.
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
2.1 ASTM Standards:
D381 Test Method for Gum Content in Fuels by Jet Evaporation
D1193 Specification for Reagent Water
D4928 Test Method for Water in Crude Oils by Coulometric Karl Fischer Titration
D5002 Test Method for Density, Relative Density, and API Gravity of Crude Oils by Digital Density Analyzer
3. Terminology
3.1 Definitions of Terms Specific to This Standard:
3.1.1 PTB—lb/1000 bbl.
3.1.2 salts in crude oil—commonly, chlorides of sodium, calcium, and magnesium dissolved in crude oil. Other inorganic
chlorides may also be present.
4. Summary of Test Method
4.1 This test method measures the conductivity of a solution of crude oil in a mixed alcohol solvent when subjected to an
electrical stress. This test method measures conductivity due to the presence of inorganic chlorides, and other conductive material,
in the crude oil. A homogenized test specimen is dissolved in a mixed alcohol solvent and placed in a test cell consisting of a beaker
and a set of electrodes. A voltage is impressed on the electrodes, and the resulting current flow is measured. The chloride (salt)
content is obtained by reference to a calibration curve of current versus chloride concentration of known mixtures. Calibration
curves are based on standards prepared to approximate the type and concentration of chlorides in the crude oils being tested.
1
This test method is under the jurisdiction of ASTM Committee D02 on Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of Subcommittee
D02.03 on Elemental Analysis.
Current edition approved July 1, 2018May 1, 2019. Published August 2018May 2019. Originally approved in 1973. Last previous edition approved in 20132018 as
D3230 – 13.D3230 – 13 (2018). DOI: 10.1520/D3230-13R18.10.1520/D3230-19.
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
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

---------------------- Page: 1 ----------------------
D3230 − 19
5. Significance and Use
5.1 This test method is used to determine the approximate chloride content of crude oils, a knowledge of which is important
in deciding whether or not the crude oil needs desalting. The efficiency of the process desalter can also be evaluated.
5.2 Excessive chloride
...

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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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Standard Test Method for Determination of Organic Chloride Content in Crude Oil by Distillation Followed by Detection Using Combustion Ion Chromatography

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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.  
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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 D4007-22(Test Method)
Standard Test Method for Water and Sediment in Crude Oil by the Centrifuge Method (Laboratory Procedure)

SIGNIFICANCE AND USE
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.  
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.  
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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