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ASTM D3230-99(2004)

(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 regarded as standard. 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 and health practices and determine the applicability of regulatory limitations prior to use. For specific warning statements, see 7.3, 7.4, and 7.11.

General Information

Status
Historical
Publication Date
30-Apr-2004
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 D3230-99 - Standard Test Method for Salts in Crude Oil (Electrometric Method)
Effective Date
01-May-2004
Replaced By
ASTM D3230-05 - Standard Test Method for Salts in Crude Oil (Electrometric Method)
Effective Date
01-May-2005
Referred By
ASTM D7578-20 - Standard Guide for Calibration Requirements for Elemental Analysis of Petroleum Products and Lubricants
Effective Date
01-May-2004
Referred By
ASTM D7455-19 - Standard Practice for Sample Preparation of Petroleum and Lubricant Products for Elemental Analysis
Effective Date
01-May-2004
Referred By
ASTM D8056-18 - Standard Guide for Elemental Analysis of Crude Oil
Effective Date
01-May-2004
Referred By
ASTM D4057-22 - Standard Practice for Manual Sampling of Petroleum and Petroleum Products
Effective Date
01-May-2004

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ASTM D3230-99(2004) - Standard Test Method for Salts in Crude Oil (Electrometric Method)ASTM D3230-99(2004) - Standard Test Method for Salts in Crude Oil (Electrometric Method)
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ASTM D3230-99(2004) - 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.
Contact ASTM International (www.astm.org) for the latest information
An American National Standard
Designation:D3230–99 (Reapproved 2004)
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.
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 regarded as standard.
3 dissolved in a mixed alcohol solvent and placed in a test cell
Acceptable concentration units are g/m or PTB (lb/1000 bbl).
consisting of a beaker and a set of electrodes. A voltage is
1.4 This standard does not purport to address all of the
impressed on the electrodes, and the resulting current flow is
safety concerns, if any, associated with its use. It is the
measured. The chloride (salt) content is obtained by reference
responsibility of the user of this standard to establish appro-
to a calibration curve of current versus chloride concentration
priate safety and health practices and determine the applica-
of known mixtures. Calibration curves are based on standards
bility of regulatory limitations prior to use. For specific
prepared to approximate the type and concentration of chlo-
warning statements, see 7.3, 7.4, and 7.11.
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
D 91 Test Method for Precipitation Number of Lubricating
chloride content of crude oils, a knowledge of which is
Oils
important in deciding whether or not the crude oil needs
D 381 Test Method for Existent Gum in Fuels by Jet
desalting. The efficiency of the process desalter can also be
Evaporation
evaluated.
D 1193 Specification for Reagent Water
5.2 Excessivechlorideleftinthecrudeoilfrequentlyresults
D 4928 Test Method for Water in Crude Oils by Coulom-
in higher corrosion rates in refining units and also has
etric Karl Fischer Titration
detrimental effects on catalysts used in these units.
D 5002 Test Method for Density and Relative Density of
5.3 This test method provides a rapid and convenient means
Crude Oils by Digital Density Analyzer
of determining the approximate content of chlorides in crude
3. Terminology oil and is useful to crude oil processors.
3.1 Definitions of Terms Specific to This Standard:
6. Apparatus
3.1.1 PTB—lb/1000 bbl.
6.1 The apparatus (seeAnnexA1) shall consist of a control
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 May 1, 2004. Published June 2004. Originally
voltage level.
approved in 1973. Last previous edition approved in 1999 as D 3230–99.
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.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
1

---------------------- Page: 1 ----------------------
D3230–99 (2004)
present in a number of common crude oils. When the relative proportion
...

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1.3 This test method can also be applied to any petroleum mixture except liquefied petroleum gases, very light naphthas, and fractions having initial boiling points above 400 °C.  
1.4 This test method contains the following annexes and appendixes:  
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1.4.10 Appendix X2—Practice for Performance Check.  
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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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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 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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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
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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.  
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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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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1.4 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.  
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ASTM D4310-22a(Test Method)
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).  
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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 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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