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ASTM D7691-11

(Test Method)

Standard Test Method for Multielement Analysis of Crude Oils Using Inductively Coupled Plasma Atomic Emission Spectrometry (ICP-AES)

Standard Test Method for Multielement Analysis of Crude Oils Using Inductively Coupled Plasma Atomic Emission Spectrometry (ICP-AES)

SIGNIFICANCE AND USE
Most often determined trace elements in crude oils are nickel and vanadium, which are usually the most abundant; however, as many as 45 elements in crude oils have been reported. Knowledge of trace elements in crude oil is important because they can have an adverse effect on petroleum refining and product quality. These effects can include catalyst poisoning in the refinery and excessive atmospheric emission in combustion of fuels. Trace element concentrations are also useful in correlating production from different wells and horizons in a field. Elements such as iron, arsenic, and lead are catalyst poisons. Vanadium compounds can cause refractory damage in furnaces, and sodium compounds have been found to cause superficial fusion on fire brick. Some organometallic compounds are volatile which can lead to the contamination of distillate fractions, and a reduction in their stability or malfunctions of equipment when they are combusted.
The value of crude oil can be determined, in part, by the concentrations of nickel, vanadium, and iron.
Inductively coupled plasma-atomic emission spectrometry (ICP-AES) is a widely used technique in the oil industry. Its advantages over traditional atomic absorption spectrometry (AAS) include greater sensitivity, freedom from molecular interferences, wide dynamic range, and multi-element capability. See Practice D7260.
SCOPE
1.1 This test method covers the determination of several elements (including iron, nickel, sulfur, and vanadium) occurring in crude oils.
1.2 For analysis of any element using wavelengths below 190 nm, a vacuum or inert gas optical path is required.
1.3 Analysis for elements such as arsenic, selenium, or sulfur in whole crude oil may be difficult by this test method due to the presence of their volatile compounds of these elements in crude oil; but this test method should work for resid samples.
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.
1.4.2 From ASTM Interlaboratory Crosscheck Programs (ILCP) on crude oils data available so far, it is not clear that organic solvent dilution techniques would necessarily give lower results than those obtained using acid decomposition techniques.
1.4.3 It is also possible that, particularly in the case of silicon, low results may be obtained irrespective of whether organic dilution or acid decomposition is utilized. Silicones are present as oil field additives and can be lost in ashing. Silicates should be retained but unless hydrofluoric acid or alkali fusion is used for sample dissolution, they may not be accounted for.
1.5 This test method uses oil-soluble metals for calibration and does not purport to quantitatively determine insoluble particulates. Analytical results are particle size dependent and low results may be obtained for particles larger than a few micrometers.
1.6 The precision in Section 18 defines the concentration ranges covered in the interlaboratory study. However, lower and particularly higher concentrations can be determined by this test method. The low concentration limits are dependent on the sensitivity of the ICP instrument and the dilution factor used. The high concentration limits are determined by the product of the maximum concentration defined by the calibration curve and the sample dilution factor.
1.7 El...

General Information

Status
Historical
Publication Date
31-Dec-2010
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 D8056-18 - Standard Guide for Elemental Analysis of Crude Oil
Effective Date
01-Jan-2011
Referred By
ASTM D7455-19 - Standard Practice for Sample Preparation of Petroleum and Lubricant Products for Elemental Analysis
Effective Date
01-Jan-2011
Referred By
ASTM D7578-20 - Standard Guide for Calibration Requirements for Elemental Analysis of Petroleum Products and Lubricants
Effective Date
01-Jan-2011
Referred By
ASTM D7260-20 - Standard Practice for Optimization, Calibration, and Validation of Inductively Coupled Plasma-Atomic Emission Spectrometry (ICP-AES) for Elemental Analysis of Petroleum Products and Lubricants
Effective Date
01-Jan-2011

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ASTM D7691-11 - Standard Test Method for Multielement Analysis of Crude Oils Using Inductively Coupled Plasma Atomic Emission Spectrometry (ICP-AES)ASTM D7691-11 - Standard Test Method for Multielement Analysis of Crude Oils Using Inductively Coupled Plasma Atomic Emission Spectrometry (ICP-AES)
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ASTM D7691-11 - Standard Test Method for Multielement Analysis of Crude Oils Using Inductively Coupled Plasma Atomic Emission Spectrometry (ICP-AES)
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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
Designation: D7691 − 11
StandardTest Method for
Multielement Analysis of Crude Oils Using Inductively
1
Coupled Plasma Atomic Emission Spectrometry (ICP-AES)
This standard is issued under the fixed designation D7691; 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 1.5 This test method uses oil-soluble metals for calibration
and does not purport to quantitatively determine insoluble
1.1 This test method covers the determination of several
particulates. Analytical results are particle size dependent and
elements (including iron, nickel, sulfur, and vanadium) occur-
low results may be obtained for particles larger than a few
ring in crude oils.
micrometers.
1.2 For analysis of any element using wavelengths below
1.6 The precision in Section 18 defines the concentration
190 nm, a vacuum or inert gas optical path is required.
ranges covered in the interlaboratory study. However, lower
1.3 Analysis for elements such as arsenic, selenium, or
and particularly higher concentrations can be determined by
sulfur in whole crude oil may be difficult by this test method
thistestmethod.Thelowconcentrationlimitsaredependenton
due to the presence of their volatile compounds of these
the sensitivity of the ICP instrument and the dilution factor
elements in crude oil; but this test method should work for
used. The high concentration limits are determined by the
resid samples.
product of the maximum concentration defined by the calibra-
1.4 Because of the particulates present in crude oil samples,
tion curve and the sample dilution factor.
iftheydonotdissolveintheorganicsolventsusedoriftheydo
1.7 Elementspresentatconcentrationsabovetheupperlimit
not get aspirated in the nebulizer, low elemental values may
of the calibration curves can be determined with additional
result, particularly for iron and sodium. This can also occur if
appropriate dilutions and with no degradation of precision.
the elements are associated with water which can drop out of
1.8 As a generality based on this interlaboratory study (see
the solution when diluted with solvent.
18.1), the trace elements identifiable in crude oils can be
1.4.1 An alternative in such cases is using Test Method
divided into three categories:
D5708, Procedure B, which involves wet decomposition of the
oil sample and measurement by ICP-AES for nickel, 1.8.1 Element levels that are too low for valid detection by
ICP-AESandhence,cannotbedetermined:aluminum,barium,
vanadium, and iron, or Test Method D5863, Procedure A,
which also uses wet acid decomposition and determines lead, magnesium, manganese, and silicon.
vanadium, nickel, iron, and sodium using atomic absorption 1.8.2 Elements that are just at the detection levels of the
spectrometry.
ICP-AESmethodandhence,cannotbedeterminedwithagreat
1.4.2 From ASTM Interlaboratory Crosscheck Programs deal of confidence: boron, calcium, chromium, copper,
(ILCP) on crude oils data available so far, it is not clear that
molybdenum, phosphorus, potassium, sodium, and zinc. Per-
organic solvent dilution techniques would necessarily give haps the determination of these elements can be considered as
lower results than those obtained using acid decomposition
semi-quantitative.
techniques.
1.8.3 Elements that are at higher levels of concentration and
1.4.3 It is also possible that, particularly in the case of
canbedeterminedwithgoodprecision:iron,nickel,sulfur,and
silicon, low results may be obtained irrespective of whether
vanadium.
organicdilutionoraciddecompositionisutilized.Siliconesare
1.9 The detection limits for elements not determined by this
present as oil field additives and can be lost in ashing. Silicates
test method follow. This information should serve as an
should be retained but unless hydrofluoric acid or alkali fusion
indication as to what elements are not present above the
is used for sample dissolution, they may not be accounted for.
detection limits typically obtainable by ICP-AES instruments.
Element mg/kg
Aluminum 1
1
Barium 0.2
This test method is under the jurisdiction of ASTM Committee D02 on
Boron 1
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee
Calcium 0.1
D02.03 on Elemental Analysis.
Chromium 0.1
Current edition approved Jan. 1, 2011. Published February 2011. DOI: 10.1520/
Copper 0.1
D7691–11.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

---------------------- Page: 1 ----------------------
D7691 − 11
D6792 Practice for Quality System in Petroleum Products
Lead 1.4
Magnesium 1
and Lubricants Testin
...

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ASTM D2892-23(Test Method)
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SIGNIFICANCE AND USE
5.1 This test method is one of a number of tests conducted on a crude oil to determine its value. It provides an estimate of the yields of fractions of various boiling ranges and is therefore valuable in technical discussions of a commercial nature.  
5.2 This test method corresponds to the standard laboratory distillation efficiency referred to as 15/5. The fractions produced can be analyzed as produced or combined to produce samples for analytical studies, engineering, and product quality evaluations. The preparation and evaluation of such blends is not part of this test method.  
5.3 This test method can be used as an analytical tool for examination of other petroleum mixtures with the exception of LPG, very light naphthas, and mixtures with initial boiling points above 400 °C.
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1.1 This test method covers the procedure for the distillation of stabilized crude petroleum (see Note 1) to a final cut temperature of 400 °C Atmospheric Equivalent Temperature (AET). This test method employs a fractionating column having an efficiency of 14 to 18 theoretical plates operated at a reflux ratio of 5:1. Performance criteria for the necessary equipment is specified. Some typical examples of acceptable apparatus are presented in schematic form. This test method offers a compromise between efficiency and time in order to facilitate the comparison of distillation data between laboratories.
Note 1: Defined as having a Reid vapor pressure less than 82.7 kPa (12 psi).  
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).  
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:  
1.4.1 Annex A1—Test Method for the Determination of the Efficiency of a Distillation Column,  
1.4.2 Annex A2—Test Method for the Determination of the Dynamic Holdup of a Distillation Column,  
1.4.3 Annex A3—Test Method for the Determination of the Heat Loss in a Distillation Column (Static Conditions),  
1.4.4 Annex A4—Test Method for the Verification of Temperature Sensor Location,  
1.4.5 Annex A5—Test Method for Determination of the Temperature Response Time,  
1.4.6 Annex A6—Practice for the Calibration of Sensors,  
1.4.7 Annex A7—Test Method for the Verification of Reflux Dividing Valves,  
1.4.8 Annex A8—Practice for Conversion of Observed Vapor Temperature to Atmospheric Equivalent Temperature (AET),  
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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ASTM D8252-23(Test Method)
Standard Test Method for Vanadium and Nickel in Crude and Residual Oil by X-ray Spectrometry

SIGNIFICANCE AND USE
5.1 This test method provides a rapid and precise elemental measurement with simple sample preparation. Typical analysis times are approximately 4 min to 5 min per sample with a preparation time of approximately 1 min to 3 min per sample.  
5.2 The quality of crude oil is related to the amount of sulfur present. Knowledge of the vanadium and nickel concentration is necessary for processing purposes as well as contractual agreements.  
5.3 The presence of vanadium and nickel presents significant risks for contamination of the cracking catalysts in the refining process.  
5.4 This test method provides a means of determining whether the vanadium and nickel content of crude meets the operational limits of the refinery and whether the metal content will have a deleterious effect on the refining process or when used as a fuel.
SCOPE
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.  
1.2 Sulfur is measured for analytical purposes only for the compensation of X-ray absorption matrix effects affecting the vanadium and nickel X-rays. For measurement of sulfur by standard test method use Test Methods D4294, D2622 or other suitable standard test method for sulfur in crude and residual oils.  
1.3 This test method is limited to the use of X-ray fluorescence (XRF) spectrometers employing an X-ray tube for excitation in conjunction with wavelength dispersive detection system or energy dispersive high resolution semiconductor detector with the ability to separate signals of adjacent and near-adjacent elements.  
1.4 This test method uses inter-element correction factors calculated from XRF theory, the fundamental parameters (FP) approach, or best fit regression.  
1.5 Samples containing higher concentrations than shown in Table 1 must be diluted to bring the elemental concentration of the diluted material within the scope of this test method.  
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 concentrations units are mg/kg for vanadium and nickel.  
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.  
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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.  
4.2 Currently, Karl Fischer is generally used for dry crude oils containing less than 5 % water. Distillation is most commonly used for dry and wet crude oils and where separate sediment analysis is available or in situations where the sediment result is not significant. The laboratory centrifuge methods allow for determination of total sediment and water in a single analysis. The field centrifuge method is used when access to controlled laboratory conditions are not available.  
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SCOPE
1.1 This guide covers a summary of the water and sediment determination methods from the API MPMS Chapter 10 for crude oils. The purpose of this guide is to provide a quick reference to these methodologies such that the reader can make the appropriate decision regarding which method to use based on the associated benefits, uses, drawbacks and limitations.  
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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.  
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ASTM D7691-23(Test Method)
Standard Test Method for Multielement Analysis of Crude Oils Using Inductively Coupled Plasma Atomic Emission Spectrometry (ICP-AES)

SIGNIFICANCE AND USE
5.1 Most often determined trace elements in crude oils are nickel and vanadium, which are usually the most abundant; however, as many as 45 elements in crude oils have been reported. Knowledge of trace elements in crude oil is important because they can have an adverse effect on petroleum refining and product quality. These effects can include catalyst poisoning in the refinery and excessive atmospheric emission in combustion of fuels. Trace element concentrations are also useful in correlating production from different wells and horizons in a field. Elements such as iron, arsenic, and lead are catalyst poisons. Vanadium compounds can cause refractory damage in furnaces, and sodium compounds have been found to cause superficial fusion on fire brick. Some organometallic compounds are volatile which can lead to the contamination of distillate fractions, and a reduction in their stability or malfunctions of equipment when they are combusted.  
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1.1 This test method covers the determination of several elements (including iron, nickel, sulfur, and vanadium) occurring in crude oils.  
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Standard Test Method for Acid Number of Crude Oils and Petroleum Products by Catalytic Thermometric Titration

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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.  
5.2 Acid number of crude and distilled petroleum fractions has been measured by Test Method D664. Test Method D664 was developed for the analysis of lubricants and biodiesel. The titration solvent used in Test Method D664 does not properly address dissolving difficult samples such as crude oil, bitumen, and high wax samples addressed in this test method. Refer to Appendix X1.  
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SCOPE
1.1 This test method covers the determination of acidic components in crude oil and petroleum products including waxes, bitumen, base stocks, and asphalts that are soluble in mixtures of xylenes and propan-2-ol. It is applicable for the determination of acids whose dissociation constants in water are larger than 10–9; extremely weak acids whose dissociation constants are smaller than 10–9 do not interfere. The values obtained by this test method may not be numerically equivalent to other acid value measurements. The range of KOH acid numbers included in the precision statement is 0.1 mg/g to 16 mg/g.  
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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.  
5.2 This test method can be used by petroleum refiners to control and optimize the refinery processes and by blenders and marketers to assess the intrinsic stability of blended asphaltene-containing heavy fuel oils.
SCOPE
1.1 This test method covers procedures for quantifying the intrinsic stability of the asphaltenes in an oil by automatic instruments using optical detection.  
1.2 This test method is applicable to residual products from thermal and hydrocracking processes, to products typical of Specifications D396 Grades No. 5L, 5H, and 6, and D2880 Grades No. 3-GT and 4-GT, and to crude oils, providing these products contain 0.5 % by mass or greater concentration of asphaltenes (see Test Method D6560).  
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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.

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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

SIGNIFICANCE AND USE
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.  
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. Specific warning statements are given in 8.1, 9.2, 9.5, 11.2, 11.4, and 16.1.  
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 D8003-22(Test Method)
Standard Test Method for Determination of Light Hydrocarbons and Cut Point Intervals in Live Crude Oils and Condensates by Gas Chromatography

SIGNIFICANCE AND USE
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.  
5.2 Equation of state calculations can be applied to variables provided by this method to allow for additional sample characterization.
SCOPE
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.  
1.2 Methane (C1) to hexane (nC6) and benzene are speciated and quantitated. Samples containing mass fractions of up to 0.5 % methane, 2.0 % ethane, 10 % propane, or 15 % isobutane may be analyzed. A mass fraction with a lower limit of 0.001 % exists for these compounds.  
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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ASTM
ASTM D4310-22a(Test Method)
Standard Test Method for Determination of Sludging and Corrosion Tendencies of Inhibited Mineral Oils

SIGNIFICANCE AND USE
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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