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ASTM D3230-06

(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
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.
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.
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 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-2006
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 D3230-05a - Standard Test Method for Salts in Crude Oil (Electrometric Method)
Effective Date
01-Nov-2006
Replaced By
ASTM D3230-08 - Standard Test Method for Salts in Crude Oil (Electrometric Method)
Effective Date
01-May-2008
Referred By
ASTM D7578-20 - Standard Guide for Calibration Requirements for Elemental Analysis of Petroleum Products and Lubricants
Effective Date
01-Nov-2006
Referred By
ASTM D8056-18 - Standard Guide for Elemental Analysis of Crude Oil
Effective Date
01-Nov-2006
Referred By
ASTM D7455-19 - Standard Practice for Sample Preparation of Petroleum and Lubricant Products for Elemental Analysis
Effective Date
01-Nov-2006
Referred By
ASTM D4057-22 - Standard Practice for Manual Sampling of Petroleum and Petroleum Products
Effective Date
01-Nov-2006

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ASTM D3230-06 - Standard Test Method for Salts in Crude Oil (Electrometric Method)ASTM D3230-06 - Standard Test Method for Salts in Crude Oil (Electrometric Method)
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ASTM D3230-06 - Standard Test Method for Salts in Crude Oil (Electrometric Method)
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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
An American National Standard
Designation:D3230–06
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 (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. Scope* 3. Terminology
1.1 This test method covers the determination of the ap- 3.1 Definitions of Terms Specific to This Standard:
proximate chloride (salts) concentration in crude oil.The range 3.1.1 PTB—lb/1000 bbl.
of concentration covered is 0 to 500 mg/kg or 0 to 150 lb/1000 3.1.2 salts in crude oil—commonly, chlorides of sodium,
bbl as chloride concentration/volume of crude oil. calcium, and magnesium dissolved in crude oil. Other inor-
1.2 This test method measures conductivity in the crude oil ganic chlorides may also be present.
due to the presence of common chlorides, such as sodium,
4. Summary of Test Method
calcium, and magnesium. Other conductive materials may also
4.1 Thistestmethodmeasurestheconductivityofasolution
be present in the crude oil.
1.3 The values stated in SI units are to be regarded as of crude oil in a mixed alcohol solvent when subjected to an
3
electrical stress.This test method measures conductivity due to
standard. Acceptable concentration units are g/m or PTB
(lb/1000 bbl). the presence of inorganic chlorides, and other conductive
material, in the crude oil. A homogenized test specimen is
1.4 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the dissolved in a mixed alcohol solvent and placed in a test cell
consisting of a beaker and a set of electrodes. A voltage is
responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica- impressed on the electrodes, and the resulting current flow is
measured. The chloride (salt) content is obtained by reference
bility of regulatory limitations prior to use. For specific
warning statements, see 7.3, 7.4, and 7.11. to a calibration curve of current versus chloride concentration
of known mixtures. Calibration curves are based on standards
2. Referenced Documents
prepared to approximate the type and concentration of chlo-
2
2.1 ASTM Standards: rides in the crude oils being tested.
D91 Test Method for Precipitation Number of Lubricating
5. Significance and Use
Oils
D 381 Test Method for Gum Content in Fuels by Jet 5.1 This test method is used to determine the approximate
chloride content of crude oils, a knowledge of which is
Evaporation
D 1193 Specification for Reagent Water important in deciding whether or not the crude oil needs
desalting. The efficiency of the process desalter can also be
D 4928 Test Methods for Water in Crude Oils by Coulom-
etric Karl Fischer Titration evaluated.
5.2 Excessivechlorideleftinthecrudeoilfrequentlyresults
D 5002 Test Method for Density and Relative Density of
Crude Oils by Digital Density Analyzer 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
1
This test method is under the jurisdiction of ASTM Committee D02 on
oil and is useful to crude oil processors.
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee
D02.03 on Elemental Analysis.
6. Apparatus
Current edition approved Nov. 1, 2006. Published November 2006. Originally
approved in 1973. Last previous edition approved in 2005 as D 3230–05a.
6.1 The apparatus (seeAnnexA1) shall consist of a control
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
unit capable of producing and displaying several voltage levels
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
for applying stress to a set of electrodes suspended in a test
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. beaker containing a test solution. The apparatus shall be
*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 ----------------------
D3230–06
capable of measuring and displaying the current (mA) con- 7.9 Salts, Mixed Solution (Concentrated Solution)—
ducted through the test solution between the electrodes at each Combine10.0mLoftheCaCl solution,20.0mLoftheMgCl
2 2
voltage level. solution
...

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1.2 This test method details procedures for the production of a liquefied gas, distillate fractions, and residuum of standardized quality on which analytical data can be obtained, and the determination of yields of the above fractions by both mass and volume. From the preceding information, a graph of temperature versus mass % distilled can be produced. This distillation curve corresponds to a laboratory technique, which is defined at 15/5 (15 theoretical plate column, 5:1 reflux ratio) or TBP (true boiling point).  
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1.4 This test method contains the following annexes and appendixes:  
1.4.1 Annex A1—Test Method for the Determination of the Efficiency of a Distillation Column,  
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1.4.9 Appendix X1—Test Method for Dehydration of a Sample of Wet Crude Oil, and  
1.4.10 Appendix X2—Practice for Performance Check.  
1.5 The values stated in SI units are to be regarded as standard. The values given in parentheses after SI units are provided for information only and are not considered standard.  
1.6 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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1.1 This test method covers the quantitative determination of total vanadium and nickel in crude and residual oil in the concentration ranges shown in Table 1 using X-ray fluorescence (XRF) spectrometry.  
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4.1 Theoretically, all of the sediment and water determination methods are valid for crude oils containing from 0 % to 100 % by volume sediment and water; the range of application is specified within the scope of each method. The round robins for all methods were conducted on relatively dry oil. All precision and bias statements included in the methods are based upon the round robin data. Analysis becomes more challenging with crude oils containing higher water contents due to the difficulty in obtaining a representative sample, and maintaining the sample quality until analysis begins.  
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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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SCOPE
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Standard Test Method for Determination of Intrinsic Stability of Asphaltene-Containing Residues, Heavy Fuel Oils, and Crude Oils (n-Heptane Phase Separation; Optical Detection)

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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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ASTM D5863-22(Test Method)
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.
SCOPE
1.1 These test methods cover the determination of nickel, vanadium, iron, and sodium in crude oils and residual fuels by flame atomic absorption spectrometry (AAS). Two different test methods are presented.  
1.2 Procedure A, Sections 8–14—Flame AAS is used to analyze a sample that is decomposed with acid for the determination of total Ni, V, and Fe.  
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.  
1.5 For each element, each test method has its own unique precision. The user can select the appropriate test method based on the precision required for the specific analysis.  
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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5.1 This test method determines methane (nC1) to hexane (nC6), cut point carbon fraction intervals to nC24 and recovery (nC24+) of live crude oils and condensates without depressurizing, thereby avoiding the loss of highly volatile components and maintaining sample integrity. This test method provides a highly resolved light end profile which can aid in determining and improving appropriate safety measures and product custody transport procedures. Decisions in regards to marketing, scheduling, and processing of crude oils may rely on light end compositional results.  
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1.1 This test method covers the determination of light hydrocarbons and cut point intervals by gas chromatography in live crude oils and condensates with VPCR4 (see Note 1) up to 500 kPa at 37.8 °C.
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1.3 This test method may be used for the determination of cut point carbon fraction intervals (see 3.2.1) of live crude oils and condensates from initial boiling point (IBP) to 391 °C (nC24). The nC24 plus fraction is reported.  
1.4 Dead oils or condensates sampled in accordance with 12.1 may also be analyzed.  
1.5 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.5.1 Exception—Where there is no direct SI equivalent such as tubing size.  
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 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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Standard Test Method for Determination of Sludging and Corrosion Tendencies of Inhibited Mineral Oils

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5.1 Insoluble material may form in oils that are subjected to oxidizing conditions.  
5.2 Significant formation of oil insolubles or metal corrosion products, or both, during this test may indicate that the oil will form insolubles or corrode metals, or both, during field service. However, no correlation with field service has been established.
SCOPE
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.  
Note 1: During round robin testing copper and iron in the oil, water and sludge phases were measured. However, the values for the total iron were found to be so low (that is, below 0.8 mg), that statistical analysis was inappropriate. The results of the cooperative test program are available (see Section 16).  
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.  
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 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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