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ASTM D3230-05a

(Test Method)

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

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

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 to 500 mg/kg or 0 to 150 lb/1000 bbl 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. Acceptable concentration units are g/m3 or PTB (lb/1000 bbl).
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 , , and .

General Information

Status
Historical
Publication Date
31-Oct-2005
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

Replaces
ASTM D3230-05 - Standard Test Method for Salts in Crude Oil (Electrometric Method)
Effective Date
01-Nov-2005
Replaced By
ASTM D3230-06 - Standard Test Method for Salts in Crude Oil (Electrometric Method)
Effective Date
01-Nov-2006
Referred By
ASTM D4057-22 - Standard Practice for Manual Sampling of Petroleum and Petroleum Products
Effective Date
01-Nov-2005
Referred By
ASTM D7455-19 - Standard Practice for Sample Preparation of Petroleum and Lubricant Products for Elemental Analysis
Effective Date
01-Nov-2005
Referred By
ASTM D8056-18 - Standard Guide for Elemental Analysis of Crude Oil
Effective Date
01-Nov-2005
Referred By
ASTM D7578-20 - Standard Guide for Calibration Requirements for Elemental Analysis of Petroleum Products and Lubricants
Effective Date
01-Nov-2005

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ASTM D3230-05a - Standard Test Method for Salts in Crude Oil (Electrometric Method)ASTM D3230-05a - Standard Test Method for Salts in Crude Oil (Electrometric Method)
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ASTM D3230-05a - Standard Test Method for Salts in Crude Oil (Electrometric Method)
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Standards Content (Sample)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Please contact ASTM International (www.astm.org) for the latest information.
An American National Standard
Designation:D3230–05a
Standard Test Method for
1
Salts in Crude Oil (Electrometric Method)
This standard is issued under the fixed designation D 3230; 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 (ϵ) indicates an editorial change since the last revision or reapproval.
1. Scope* 3.1.2 salts in crude oil—commonly, chlorides of sodium,
calcium, and magnesium dissolved in crude oil. Other inor-
1.1 This test method covers the determination of the ap-
ganic chlorides may also be present.
proximate chloride (salts) concentration in crude oil.The range
of concentration covered is 0 to 500 mg/kg or 0 to 150 lb/1000
4. Summary of Test Method
bbl as chloride concentration/volume of crude oil.
4.1 Thistestmethodmeasurestheconductivityofasolution
1.2 This test method measures conductivity in the crude oil
of crude oil in a mixed alcohol solvent when subjected to an
due to the presence of common chlorides, such as sodium,
electrical stress.This test method measures conductivity due to
calcium, and magnesium. Other conductive materials may also
the presence of inorganic chlorides, and other conductive
be present in the crude oil.
material, in the crude oil. A homogenized test specimen is
1.3 The values stated in SI units are to be regarded as
3 dissolved in a mixed alcohol solvent and placed in a test cell
standard. Acceptable concentration units are g/m or PTB
consisting of a beaker and a set of electrodes. A voltage is
(lb/1000 bbl).
impressed on the electrodes, and the resulting current flow is
1.4 This standard does not purport to address all of the
measured. The chloride (salt) content is obtained by reference
safety concerns, if any, associated with its use. It is the
to a calibration curve of current versus chloride concentration
responsibility of the user of this standard to establish appro-
of known mixtures. Calibration curves are based on standards
priate safety and health practices and determine the applica-
prepared to approximate the type and concentration of chlo-
bility of regulatory limitations prior to use. For specific
rides in the crude oils being tested.
warning statements, see 7.3, 7.4, and 7.11.
5. Significance and Use
2. Referenced Documents
2
5.1 This test method is used to determine the approximate
2.1 ASTM Standards:
chloride content of crude oils, a knowledge of which is
D91 Test Method for Precipitation Number of Lubricating
important in deciding whether or not the crude oil needs
Oils
desalting. The efficiency of the process desalter can also be
D 381 Test Method for Gum Content in Fuels by Jet
evaluated.
Evaporation
5.2 Excessivechlorideleftinthecrudeoilfrequentlyresults
D 1193 Specification for Reagent Water
in higher corrosion rates in refining units and also has
D 4928 Test Methods for Water in Crude Oils by Coulo-
detrimental effects on catalysts used in these units.
metric Karl Fischer Titration
5.3 This test method provides a rapid and convenient means
D 5002 Test Method for Density and Relative Density of
of determining the approximate content of chlorides in crude
Crude Oils by Digital Density Analyzer
oil and is useful to crude oil processors.
3. Terminology
6. Apparatus
3.1 Definitions of Terms Specific to This Standard:
6.1 The apparatus (seeAnnexA1) shall consist of a control
3.1.1 PTB—lb/1000 bbl.
unit capable of producing and displaying several voltage levels
for applying stress to a set of electrodes suspended in a test
1
This test method is under the jurisdiction of ASTM Committee D02 on
beaker containing a test solution. The apparatus shall be
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee
capable of measuring and displaying the current (mA) con-
D02.03 on Elemental Analysis.
ducted through the test solution between the electrodes at each
Current edition approved Nov. 1, 2005. Published November 2005. Originally
voltage level.
approved in 1973. Last previous edition approved in 2005 as D 3230–05.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
NOTE 1—Some apparatus are capable of measuring voltage and current
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
internally and, after comparison to internal calibration curves, of display-
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. ing the resultant concentration.
*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

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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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1.3 Procedure B, Sections 15–20—Flame AAS is used to analyze a sample diluted with an organic solvent for the determination of Ni, V, and Na. This test method uses oil-soluble metals for calibration to determine dissolved metals and does not purport to quantitatively determine nor detect insoluble particulates. Hence, this test method may underestimate the metal content, especially sodium, present as inorganic sodium salts.  
1.4 The concentration ranges covered by these test methods are determined by the sensitivity of the instruments, the amount of sample taken for analysis, and the dilution volume. A specific statement is given in Note 1.  
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1.6 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard, unless specifically stated. Other units that appear in this standard are included for information purposes only or because they are in embedded pictures that cannot be edited.  
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1.5 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
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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.  
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 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. For specific warning statements, see Section 7 and X1.1.5.  
1.7 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 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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