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ASTM D7623-10

(Test Method)

Standard Test Method for Total Mercury in Crude Oil Using Combustion-Gold Amalgamation and Cold Vapor Atomic Absorption Method

Standard Test Method for Total Mercury in Crude Oil Using Combustion-Gold Amalgamation and Cold Vapor Atomic Absorption Method

SIGNIFICANCE AND USE
The emission of mercury during crude oil refining is an environmental concern. The emission of mercury may also contaminate refined products and form amalgams with metals, such as aluminum.
When representative test portions are analyzed according to this procedure, the total mercury is representative of concentrations in the sample.
SCOPE
1.1 This test method covers the procedures to determine the total mercury content in a sample of crude oil.
1.2 The test method may be applied to crude oil samples containing between 5 to 400 ng/mL of mercury. The results may be converted to mass basis, and reported as ng/g of mercury.
1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.4 WARNING—Mercury has been designated by many regulatory agencies as a hazardous material that can cause central nervous system, kidney and liver damage. Mercury, or its vapor, may be hazardous to health and corrosive to materials. Caution should be taken when handling mercury and mercury containing products. See the applicable product Material Safety Data Sheet (MSDS) for details and EPA’s websitehttp://www.epa.gov/mercury/faq.htmfor additional information. Users should be aware that selling mercury and/or mercury containing products into your state or country may be prohibited by law.
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 and health practices and determine the applicability of regulatory limitations prior to use.

General Information

Status
Historical
Publication Date
30-Apr-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 D7740-20 - Standard Practice for Optimization, Calibration, and Validation of Atomic Absorption Spectrometry for Metal Analysis of Petroleum Products and Lubricants
Effective Date
01-May-2010
Referred By
ASTM D8056-18 - Standard Guide for Elemental Analysis of Crude Oil
Effective Date
01-May-2010
Referred By
ASTM D7622-20 - Standard Test Method for Total Mercury in Crude Oil Using Combustion and Direct Cold Vapor Atomic Absorption Method with Zeeman Background Correction
Effective Date
01-May-2010
Referred By
ASTM D7455-19 - Standard Practice for Sample Preparation of Petroleum and Lubricant Products for Elemental Analysis
Effective Date
01-May-2010
Referred By
ASTM D7578-20 - Standard Guide for Calibration Requirements for Elemental Analysis of Petroleum Products and Lubricants
Effective Date
01-May-2010
Referred By
ASTM D7482-17(2023) - Standard Practice for Sampling, Storage, and Handling of Hydrocarbons for Mercury Analysis
Effective Date
01-May-2010

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ASTM D7623-10 - Standard Test Method for Total Mercury in Crude Oil Using Combustion-Gold Amalgamation and Cold Vapor Atomic Absorption MethodASTM D7623-10 - Standard Test Method for Total Mercury in Crude Oil Using Combustion-Gold Amalgamation and Cold Vapor Atomic Absorption Method
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ASTM D7623-10 - Standard Test Method for Total Mercury in Crude Oil Using Combustion-Gold Amalgamation and Cold Vapor Atomic Absorption 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
Designation: D7623 − 10
StandardTest Method for
Total Mercury in Crude Oil Using Combustion-Gold
1
Amalgamation and Cold Vapor Atomic Absorption Method
This standard is issued under the fixed designation D7623; 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 D4175 Terminology Relating to Petroleum, Petroleum
Products, and Lubricants
1.1 This test method covers the procedures to determine the
D4177 Practice for Automatic Sampling of Petroleum and
total mercury content in a sample of crude oil.
Petroleum Products
1.2 The test method may be applied to crude oil samples
D6299 Practice for Applying Statistical Quality Assurance
containing between 5 to 400 ng/mL of mercury. The results
and Control Charting Techniques to Evaluate Analytical
may be converted to mass basis, and reported as ng/g of
Measurement System Performance
mercury.
D6300 Practice for Determination of Precision and Bias
1.3 The values stated in SI units are to be regarded as Data for Use in Test Methods for Petroleum Products and
Lubricants
standard. No other units of measurement are included in this
standard. D6792 Practice for Quality System in Petroleum Products
and Lubricants Testing Laboratories
1.4 WARNING—Mercury has been designated by many
D7482 Practice for Sampling, Storage, and Handling of
regulatory agencies as a hazardous material that can cause
Hydrocarbons for Mercury Analysis
central nervous system, kidney and liver damage. Mercury, or
D7622 Test Method for Total Mercury in Crude Oil Using
its vapor, may be hazardous to health and corrosive to
Combustion and Direct Cold Vapor Atomic Absorption
materials.Cautionshouldbetakenwhenhandlingmercuryand
Method with Zeeman Background Correction
mercury containing products. See the applicable product Ma-
terial Safety Data Sheet (MSDS) for details and EPA’s
3. Terminology
website—http://www.epa.gov/mercury/faq.htm—for addi-
3.1 For definitions of terms used in this standard, refer to
tional information. Users should be aware that selling mercury
Terminology D4175.
and/or mercury containing products into your state or country
may be prohibited by law.
4. Summary of Test Method
1.5 This standard does not purport to address all of the
4.1 Controlled heating of the analysis sample in oxygen is
safety concerns, if any, associated with its use. It is the
usedtoliberatemercury.Thesampleisheatedtodrynessinthe
responsibility of the user of this standard to establish appro-
instrumentandthenthermally(atabout700°C)andchemically
priate safety and health practices and determine the applica-
decomposed. The decomposition products are carried by flow-
bility of regulatory limitations prior to use.
ing treated air to the catalytic section of the furnace (at about
2. Referenced Documents
850°C), where oxidation is completed. The decomposition
2
2.1 ASTM Standards: products are carried to a gold amalgamator that selectively
traps mercury. After the system is flushed with oxygen to
D1193 Specification for Reagent Water
D4057 Practice for Manual Sampling of Petroleum and remove any remaining decomposition products other than
mercury, the amalgamator is rapidly heated to about 600°C,
Petroleum Products
releasing mercury vapor. Flowing oxygen carries the mercury
1
vapor through absorbance cells positioned in the light path of
This test method is under the jurisdiction of ASTM Committee D02 on
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee
single wavelength cold vapor atomic absorption spectropho-
D02.03 on Elemental Analysis.
tometer.Absorbance peak height or peak area, as a function of
Current edition approved May 1, 2010. Published July 2010.
2 mercury concentration, is measured at 253.65 nm.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
NOTE 1—Mercury and mercury salts can be volatized at low tempera-
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
tures. Precautions against inadvertent mercury loss should be taken when
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. using this test method.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

---------------------- Page: 1 ----------------------
D7623 − 10
5. Significance and Use 6.3 Sample Combustion Boats, porcelain, quartz, or other
material as recommended and of convenient size suitable for
5.1 The emission of mercury during crude oil refining is an
use in the instrument being used.
environmental concern. The emission of mercury may also
c
...

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ASTM D8252-23(Test Method)
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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.
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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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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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ASTM D2892-23(Test Method)
Standard Test Method for Distillation of Crude Petroleum (15-Theoretical Plate Column)

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).  
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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,  
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,  
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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.  
1.7 This standard does not purport to address all of the safety concerns, if any, asso...

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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 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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SCOPE
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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.  
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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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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.  
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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.  
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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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.  
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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 D4929-22(Test Method)
Standard Test Method for Determination of Organic Chloride Content in Crude Oil

SIGNIFICANCE AND USE
5.1 Organic chlorides do not occur naturally in crude oil. When present, they result from contamination in some manner, such as disposal of chlorinated solvent used in many dewaxing pipeline or other equipment operations.  
5.1.1 Uncontaminated crude oil will contain no detectable organic chloride, and most refineries can handle very small amounts without deleterious effects.
5.1.1.1 Most trade contracts specify that no organic chloride is present in the crude oil.  
5.1.2 Several pipelines have set specification limits at  
5.1.2.1 To ensure Eq 3).  
5.1.3 Organic chloride present in the crude oil (for example, methylene chloride, perchloroethylene, etc.) is usually distilled into the naphtha fraction. Some compounds break down during fractionation and produce hydrochloric acid, which has a corrosive effect. Some compounds survive fractionation and are destroyed during hydro-treating (desulfurization of the naphtha).  
5.2 Other halides can also be used for dewaxing crude oil; in such cases, any organic halides will have similar impact on the refining operations as the organic chlorides.  
5.3 Organic chloride species are potentially damaging to refinery processes. Hydrochloric acid can be produced in hydrotreating or reforming reactors and the acid accumulates in condensing regions of the refinery. Unexpected concentrations of organic chlorides cannot be effectively neutralized and damage can result. Organic chlorides are not known to be naturally present in crude oils and usually result from cleaning operations at producing sites, pipelines, or tanks. It is important for the oil industry to have common methods available for the determination of organic chlorides in crude oil, particularly when transfer of custody is involved.
SCOPE
1.1 The procedures in this test method cover the determination of organic chloride (above 1 μg/g organically-bound chlorine) in crude oils, using either distillation and sodium biphenyl reduction, distillation and microcoulometry, or distillation and X-ray fluorescence (XRF) spectrometry.  
1.2 The procedures in this test method involve the distillation of crude oil test specimens to obtain a naphtha fraction prior to chloride determination. The chloride content of the naphtha fraction of the whole crude oil can thereby be obtained. See Section 6 regarding potential interferences.  
1.3 Procedure A covers the determination of organic chloride in the washed naphtha fraction of crude oil by sodium biphenyl reduction followed by potentiometric titration.  
1.4 Procedure B covers the determination of organic chloride in the washed naphtha fraction of crude oil by oxidative combustion followed by microcoulometric titration.  
1.5 Procedure C covers the determination of organic chloride in the washed naphtha fraction of crude oil by X-ray fluorescence spectrometry.  
1.6 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.6.1 The preferred concentration units are micrograms of chloride per gram of sample, though milligrams of chloride per kilogram of sample is commonly used for Procedure C.  
1.7 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
1.8 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

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