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ASTM D6470-99(2020)

(Test Method)

Standard Test Method for Salt in Crude Oils (Potentiometric Method)

Standard Test Method for Salt in Crude Oils (Potentiometric Method)

SIGNIFICANCE AND USE
4.1 A knowledge of water extractable inorganic halides in oil is important when deciding whether or not the oils need desalting. Excessive halide, especially in crude oil, frequently results in higher corrosion rates in refining units.
SCOPE
1.1 This test method covers the determination of salt in crude oils. For the purpose of this test method, salt is expressed as % (m/m) NaCl (sodium chloride) and covers the range from 0.0005 % to 0.15 % (m/m).  
1.2 The limit of detection is 0.0002 % (m/m) for salt (as NaCl).  
1.3 The test method is applicable to nearly all of the heavier petroleum products, such as crude oils, residues, and fuel oils. It may also be applied to used turbine oil and marine diesel fuel to estimate seawater contamination. Water extractable salts, originating from additives present in oils, are codetermined.  
1.4 The values stated in SI units are to be regarded as the standard.  
1.5 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.  
1.6 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-2020
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

Referred By
ASTM D4057-22 - Standard Practice for Manual Sampling of Petroleum and Petroleum Products
Effective Date
01-May-2020
Referred By
ASTM D7578-20 - Standard Guide for Calibration Requirements for Elemental Analysis of Petroleum Products and Lubricants
Effective Date
01-May-2020

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ASTM D6470-99(2020) - Standard Test Method for Salt in Crude Oils (Potentiometric Method)ASTM D6470-99(2020) - Standard Test Method for Salt in Crude Oils (Potentiometric Method)
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ASTM D6470-99(2020) - Standard Test Method for Salt in Crude Oils (Potentiometric Method)
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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: D6470 − 99 (Reapproved 2020)
Standard Test Method for
1
Salt in Crude Oils (Potentiometric Method)
This standard is issued under the fixed designation D6470; 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.
1. Scope D4057 Practice for Manual Sampling of Petroleum and
Petroleum Products
1.1 This test method covers the determination of salt in
D4177 Practice for Automatic Sampling of Petroleum and
crudeoils.Forthepurposeofthistestmethod,saltisexpressed
Petroleum Products
as % (m/m) NaCl (sodium chloride) and covers the range from
D4377 Test Method forWater in Crude Oils by Potentiomet-
0.0005 % to 0.15 % (m/m).
3
ric Karl Fischer Titration (Withdrawn 2020)
1.2 The limit of detection is 0.0002 % (m/m) for salt (as
D4928 Test Method for Water in Crude Oils by Coulometric
NaCl).
Karl Fischer Titration
1.3 The test method is applicable to nearly all of the heavier E200 Practice for Preparation, Standardization, and Storage
of Standard and Reagent Solutions for ChemicalAnalysis
petroleum products, such as crude oils, residues, and fuel oils.
Itmayalsobeappliedtousedturbineoilandmarinedieselfuel
3. Summary of Test Method
to estimate seawater contamination. Water extractable salts,
originating from additives present in oils, are codetermined. 3.1 After homogenizing the crude oil with a mixer, a
weighed aliquot is dissolved in xylene at 65 °C and extracted
1.4 The values stated in SI units are to be regarded as the
with specified volumes of alcohol, acetone, and water in an
standard.
electrically heated extraction apparatus. A portion of the
1.5 This standard does not purport to address all of the
aqueous extract is analyzed for total halides by potentiometric
safety concerns, if any, associated with its use. It is the
titration.
responsibility of the user of this standard to establish appro-
priate safety, health, and environmental practices and deter-
4. Significance and Use
mine the applicability of regulatory limitations prior to use.
4.1 A knowledge of water extractable inorganic halides in
1.6 This international standard was developed in accor-
oil is important when deciding whether or not the oils need
dance with internationally recognized principles on standard-
desalting. Excessive halide, especially in crude oil, frequently
ization established in the Decision on Principles for the
results in higher corrosion rates in refining units.
Development of International Standards, Guides and Recom-
mendations issued by the World Trade Organization Technical
5. Apparatus
Barriers to Trade (TBT) Committee.
5.1 Extraction Apparatus, made of borosilicate glass, con-
formingtothedimensionsgiveninFig.1,andconsistingofthe
2. Referenced Documents
following component parts:
2
2.1 ASTM Standards:
5.1.1 Boiling Flask, 500 mL capacity.
D329 Specification for Acetone
5.1.2 Hopkins Reflux Condenser, having a vapor outlet
D770 Specification for Isopropyl Alcohol
connected by a rubber tube to an outside vent or to a suction
D843 Specification for Nitration Grade Xylene
hood.
D1193 Specification for Reagent Water
5.1.3 Thistle Tube, approximately 70 mL capacity, with a
D4006 Test Method for Water in Crude Oil by Distillation
line to indicate approximately the 50 mL level.
5.1.4 Heating Tube, containing a chimney for increasing
1
convection in the liquid.
This test method is under the jurisdiction of ASTM Committee D02 on
Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of
5.1.5 Heating Coil, 250 W, consisting of a suitable gage of
Subcommittee D02.03 on Elemental Analysis.
Nichrome wire.
Current edition approved May 1, 2020. Published June 2020. Originally
5.1.6 Rheostat, of suitable resistance and capacity, for
approved in 1999. Last previous edition approved in 2015 as D6470 – 99 (2015).
DOI: 10.1520/D6470-99R20. regulating the heater.
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
3
Standards volume information, refer to the standard’s Document Summary page on The last approved version of this historical standard is referenced on
the ASTM website. www.astm.org.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

---------------------- Page: 1 ----------------------
D6470 − 99 (2020)
NOTE 1—Hopkins-type condenser is used.
FIG. 1 Extraction Apparatus
5.2 Safety Sh
...

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1.4 Because of the particulates present in crude oil samples, if they do not dissolve in the organic solvents used or if they do not get aspirated in the nebulizer, low elemental values may result, particularly for iron and sodium. This can also occur if the elements are associated with water which can drop out of the solution when diluted with solvent.  
1.4.1 An alternative in such cases is using Test Method D5708, Procedure B, which involves wet decomposition of the oil sample and measurement by ICP-AES for nickel, vanadium, and iron, or Test Method D5863, Procedure A, which also uses wet acid decomposition and determines vanadium, nickel, iron, and sodium using atomic absorption spectrometry.  
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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 D8045-17(2023)(Test Method)
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SIGNIFICANCE AND USE
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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1.1 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.
Note 1: As described in Test Method D6377.  
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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.  
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1.5.1 Exception—Where there is no direct SI equivalent such as tubing size.  
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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).
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1.1 This test method covers the determination of water in crude oil by distillation.  
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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).  
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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.  
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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.  
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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).
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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.  
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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.

  • Standard
    16 pages
    English language
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  • Standard
    16 pages
    English language
    sale 15% off