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ASTM D8149-20

(Practice)

Standard Practice for Optimization, Calibration, and Validation of Ion Chromatographic Determination of Heteroatoms and Anions in Petroleum Products and Lubricants

Standard Practice for Optimization, Calibration, and Validation of Ion Chromatographic Determination of Heteroatoms and Anions in Petroleum Products and Lubricants

SIGNIFICANCE AND USE
7.1 Accurate elemental analysis of petroleum products and lubricants is necessary for the determination of chemical properties, which are used to establish compliance with commercial and regulatory specifications.  
7.2 Ion chromatography is often used in cases where anion content of the material is desired. Some of the hetero-atoms can be converted by combustion in an oxygen atmosphere followed by aqueous dissolution to convert them into anions before ion chromatographic determination. A number of ion chromatographic ASTM standards issued are listed in Section 2. Of these, the D02, D05, and D16 Committee standards which use ion chromatography are listed in Table 1.
SCOPE
1.1 This practice covers the information on calibration, quality control, and operational guidance for anionic measurements using ion chromatography (IC).  
1.2 IC Related Standards—Chemically or electrolytically regenerated suppressed ion chromatography standards for aqueous matrices include Test Methods D2988, D4327, D5085, D5542, D5827, D5987, D5996, D6581, D7319, D7328, D7359, D7773, D7994, and D8150; IC instrumentation requirements are described in Practices E1151, and E1511.  
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 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.  
1.5 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-Jun-2020
ICS
75.080 - Petroleum products in general
75.100 - Lubricants, industrial oils and related products
Technical Committee
D02 - Petroleum Products, Liquid Fuels, and Lubricants
Drafting Committee
D02.03 - Elemental Analysis
Current Stage
Ref Project

Relations

Refers
ASTM D2988-96(2020) - Standard Test Methods for Water-Soluble Halide Ion in Halogenated Organic Solvents and Their Admixtures
Effective Date
01-Apr-2020

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ASTM D8149-20 - Standard Practice for Optimization, Calibration, and Validation of Ion Chromatographic Determination of Heteroatoms and Anions in Petroleum Products and LubricantsASTM D8149-20 - Standard Practice for Optimization, Calibration, and Validation of Ion Chromatographic Determination of Heteroatoms and Anions in Petroleum Products and Lubricants
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ASTM D8149-20 - Standard Practice for Optimization, Calibration, and Validation of Ion Chromatographic Determination of Heteroatoms and Anions in Petroleum Products and Lubricants
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REDLINE ASTM D8149-20 - Standard Practice for Optimization, Calibration, and Validation of Ion Chromatographic Determination of Heteroatoms and Anions in Petroleum Products and LubricantsREDLINE ASTM D8149-20 - Standard Practice for Optimization, Calibration, and Validation of Ion Chromatographic Determination of Heteroatoms and Anions in Petroleum Products and Lubricants
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REDLINE ASTM D8149-20 - Standard Practice for Optimization, Calibration, and Validation of Ion Chromatographic Determination of Heteroatoms and Anions in Petroleum Products and Lubricants
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Standards Content (Sample)

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: D8149 − 20
Standard Practice for
Optimization, Calibration, and Validation of Ion
Chromatographic Determination of Heteroatoms and Anions
1
in Petroleum Products and Lubricants
This standard is issued under the fixed designation D8149; 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* D1193 Specification for Reagent Water
D2988 Test Methods for Water-Soluble Halide Ion in Halo-
1.1 This practice covers the information on calibration,
genated Organic Solvents and Their Admixtures
quality control, and operational guidance for anionic measure-
D4057 Practice for Manual Sampling of Petroleum and
ments using ion chromatography (IC).
Petroleum Products
1.2 IC Related Standards—Chemically or electrolytically
D4177 Practice for Automatic Sampling of Petroleum and
regenerated suppressed ion chromatography standards for
Petroleum Products
aqueousmatricesincludeTestMethodsD2988,D4327,D5085,
D4327 Test Method for Anions in Water by Suppressed Ion
D5542, D5827, D5987, D5996, D6581, D7319, D7328,
Chromatography
D7359, D7773, D7994, and D8150; IC instrumentation re-
D5085 Test Method for Determination of Chloride, Nitrate,
quirements are described in Practices E1151, and E1511.
andSulfateinAtmosphericWetDepositionbyChemically
Suppressed Ion Chromatography
1.3 The values stated in SI units are to be regarded as
standard. No other units of measurement are included in this D5542 Test Methods for TraceAnions in High Purity Water
by Ion Chromatography
standard.
D5827 Test Method for Analysis of Engine Coolant for
1.4 This standard does not purport to address all of the
Chloride and Other Anions by Ion Chromatography
safety concerns, if any, associated with its use. It is the
D5987 Test Method for Total Fluorine in Coal and Coke by
responsibility of the user of this standard to establish appro-
Pyrohydrolytic Extraction and Ion Selective Electrode or
priate safety, health, and environmental practices and deter-
3
Ion Chromatograph Methods (Withdrawn 2020)
mine the applicability of regulatory limitations prior to use.
D5996 Test Method for MeasuringAnionic Contaminants in
1.5 This international standard was developed in accor-
High-Purity Water by On-Line Ion Chromatography
dance with internationally recognized principles on standard-
D6299 Practice for Applying Statistical Quality Assurance
ization established in the Decision on Principles for the
and Control Charting Techniques to Evaluate Analytical
Development of International Standards, Guides and Recom-
Measurement System Performance
mendations issued by the World Trade Organization Technical
D6581 Test Methods for Bromate, Bromide, Chlorate, and
Barriers to Trade (TBT) Committee.
Chlorite in Drinking Water by Suppressed Ion Chroma-
tography
2. Referenced Documents
D6751 Specification for Biodiesel Fuel Blend Stock (B100)
2
2.1 ASTM Standards:
for Middle Distillate Fuels
D86 Test Method for Distillation of Petroleum Products and
D6792 Practice for Quality Management Systems in Petro-
Liquid Fuels at Atmospheric Pressure
leum Products, Liquid Fuels, and Lubricants Testing
D975 Specification for Diesel Fuel
Laboratories
D7318 TestMethodforExistentInorganicSulfateinEthanol
by Potentiometric Titration
1
This test method is under the jurisdiction of ASTM Committee D02 on
D7319 Test Method for Determination of Existent and Po-
Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of
Subcommittee D02.03 on Elemental Analysis. tential Sulfate and Inorganic Chloride in Fuel Ethanol and
Current edition approved July 1, 2020. Published July 2020. Originally approved
Butanol by Direct Injection Suppressed Ion Chromatog-
in 2017. Last previous edition approved in 2017 as D8149 – 17. DOI: 10.1520/
raphy
D8149-20.
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.
*A Summary of Changes section appears at the end of this standard
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

---------------------- Page: 1 ----------------------
D8149 − 20
D7328 Test Method for Determination of Existent and Po- 3.2.5 oxidative pyrohydrolytic combu
...

This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
Designation: D8149 − 17 D8149 − 20
Standard Practice for
Optimization, Calibration, and Validation of Ion
Chromatographic Determination of Heteroatoms and Anions
1
in Petroleum Products and Lubricants
This standard is issued under the fixed designation D8149; 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 Scope*
1.1 This practice covers the information on calibration, quality control, and operational guidance for anionic measurements
using ion chromatography (IC).
1.2 IC Related Standards—Chemically or electrolytically regenerated suppressed ion chromatography standards for aqueous
matrices include Test Methods D2988, D4327, D5085, D5542, D5827, D5987, D5996, D6581, D7319, D7328, D7359, D7773,
D7994, and D8150; IC instrumentation requirements are described in Practices E1151, and E1511.
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 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.
1.5 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.
2. Referenced Documents
2
2.1 ASTM Standards:
D86 Test Method for Distillation of Petroleum Products and Liquid Fuels at Atmospheric Pressure
D975 Specification for Diesel Fuel
D1193 Specification for Reagent Water
D2988 Test Methods for Water-Soluble Halide Ion in Halogenated Organic Solvents and Their Admixtures
D4057 Practice for Manual Sampling of Petroleum and Petroleum Products
D4177 Practice for Automatic Sampling of Petroleum and Petroleum Products
D4327 Test Method for Anions in Water by Suppressed Ion Chromatography
D5085 Test Method for Determination of Chloride, Nitrate, and Sulfate in Atmospheric Wet Deposition by Chemically
Suppressed Ion Chromatography
D5542 Test Methods for Trace Anions in High Purity Water by Ion Chromatography
D5827 Test Method for Analysis of Engine Coolant for Chloride and Other Anions by Ion Chromatography
D5987 Test Method for Total Fluorine in Coal and Coke by Pyrohydrolytic Extraction and Ion Selective Electrode or Ion
3
Chromatograph Methods (Withdrawn 2020)
D5996 Test Method for Measuring Anionic Contaminants in High-Purity Water by On-Line Ion Chromatography
D6299 Practice for Applying Statistical Quality Assurance and Control Charting Techniques to Evaluate Analytical Measure-
ment System Performance
D6581 Test Methods for Bromate, Bromide, Chlorate, and Chlorite in Drinking Water by Suppressed Ion Chromatography
D6751 Specification for Biodiesel Fuel Blend Stock (B100) for Middle Distillate Fuels
1
This test method is under the jurisdiction of ASTM Committee D02 on Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of Subcommittee
D02.03 on Elemental Analysis.
Current edition approved Dec. 1, 2017July 1, 2020. Published February 2018July 2020. Originally approved in 2017. Last previous edition approved in 2017 as
D8149 – 17. DOI: 10.1520/D8149-17.10.1520/D8149-20.
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 Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
3
The last approved version of this historical standard is referenced on www.astm.org.
*A Summary of Changes section appears at the end of this standard
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

---------------------- Page: 1 ----------------------
D8149 − 20
D6792 Practice for Quality Management Systems in Petroleum Products, Liquid Fuels, and Lubricants Testing Laboratories
D7318 Test Method for Existent Inorganic Sulfate in Ethanol by Potentiometric Titration
D7319 Test Method for Determination of Existent and Potential Sulfate and Inorgani
...

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Standard Terminology Relating to Petroleum Products, Liquid Fuels, and Lubricants

SCOPE
1.1 This terminology standard covers the compilation of terminology developed by Committee D02 on Petroleum Products, Liquid Fuels, and Lubricants, except that it does not include terms/definitions specific only to the standards in which they appear.  
1.1.1 The terminology, mostly definitions, is unique to petroleum, petroleum products, lubricants, and certain products from biomass and chemical synthesis. Meanings of the same terms outside of applications to petroleum, petroleum products, and lubricants can be found in other compilations and in dictionaries of general usage.  
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SIGNIFICANCE AND USE
4.1 A petroleum products, liquid fuels, and lubricants testing laboratory plays a crucial role in product quality management and customer satisfaction. It is essential for a laboratory to provide quality data. This document provides guidance for establishing and maintaining a quality management system in a laboratory.  
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SCOPE
1.1 This practice covers the establishment and maintenance of the essentials of a quality management system in laboratories engaged in the analysis of petroleum products, liquid fuels, and lubricants. It is designed to be used in conjunction with Practice D6299.
Note 1: This practice is based on the quality management concepts and principles advocated in ANSI/ISO/ASQ Q9000 standards, ISO/IEC 17025, ASQ Manual,2 and ASTM standards such as D3244, D4182, D4621, D6299, D6300, D7372, E29, E177, E456, E548, E882, E994, E1301, E1323, STP 15D,3 and STP 1209.4  
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ASTM D7873-22a(Test Method)
Standard Test Method for Determination of Oxidation Stability and Insolubles Formation of Inhibited Turbine Oils at 120 °C Without the Inclusion of Water (Dry TOST Method)

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, resulting in varnish formation during field service. The level of varnish formation in service will be dependent on many factors (turbine design, reservoir temperature, duty-cycle, for example. peaking, cycling, or base-load duty, maintenance, and so forth) and a direct correlation between results in this test and field varnish formation are yet to be established.  
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SCOPE
1.1 This test method is used to evaluate the sludging tendencies of steam and gas turbine lubricants during the oxidation process in the presence of oxygen and metal catalyst (copper and iron) at an elevated temperature. This test method may be used to evaluate industrial oils (for example, circulating oils and so forth).  
1.2 This test method is a modification of Test Method D4310 where the sludging and corrosion tendencies of the same kinds of oils are determined after 1000 h at 95 °C in the presence of water. Water is omitted in this modification.  
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ASTM D974-22(Test Method)
Standard Test Method for Acid and Base Number by Color-Indicator Titration

SIGNIFICANCE AND USE
5.1 New and used petroleum products can contain basic or acidic constituents that are present as additives or as degradation products formed during service, such as oxidation products. The relative amount of these materials can be determined by titrating with acids or bases. This number, whether expressed as acid number or base number, is a measure of this amount of acidic or basic substances, respectively, in the oil—always under the conditions of the test. This number is used as a guide in the quality control of lubricating oil formulations. It is also sometimes used as a measure of lubricant degradation in service; however, any condemning limits must be empirically established.  
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SCOPE
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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 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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SCOPE
1.1 This test method covers evaluation of the ferrous corrosion control characteristics of water–miscible metalworking fluids.  
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ASTM D4177-22e1(Practice)
Standard Practice for Automatic Sampling of Petroleum and Petroleum Products

SIGNIFICANCE AND USE
4.1 Representative samples of petroleum and petroleum products are required for the determination of chemical and physical properties, which are used to establish standard volumes, prices, and compliance with commercial terms and regulatory requirements. This practice does not cover sampling of electrical insulating oils and hydraulic fluids. This practice does not address how to sample crude at temperatures below the freezing point of water.
PART I—General
This part is applicable to all petroleum liquid sampling whether it be crude oil or refined products. Review this section before designing or installing any automatic sampling system.
SCOPE
1.1 This practice describes general procedures and equipment for automatically obtaining samples of liquid petroleum and petroleum products, crude oils, and intermediate products from the sample point into the primary container. This practice also provides additional specific information about sample container selection, preparation, and sample handling. If sampling is for the precise determination of volatility, use Practice D5842 (API MPMS Chapter 8.4) in conjunction with this practice. For sample mixing and handling, refer to Practice D5854 (API MPMS Chapter 8.3). This practice does not cover sampling of electrical insulating oils and hydraulic fluids.  
1.2 Table of Contents:    
Section  
INTRODUCTION  
Scope  
1  
Referenced Documents  
2  
Terminology  
3  
Significance and Use  
4  
PART I–GENERAL  
Representative Sampling Components  
5  
Design Criteria  
6  
Automatic Sampling Systems  
7  
Sampling Location  
8  
Mixing of the Flowing Stream  
9  
Proportionality  
10  
Sample Extractor Grab Volume  
11  
Containers  
12  
Sample Handling and Mixing  
13  
Control Systems  
14  
Sample System Security  
15  
System Proving (Performance Acceptance Tests)  
16  
Performance Monitoring  
17  
PART II–CRUDE OIL  
Crude Oil  
18  
PART III–REFINED PRODUCTS  
Refined Products  
19  
KEYWORDS  
Keywords  
20  
ANNEXES  
Calculations of the Margin of Error based on Number of Sample Grabs  
Annex A1  
Theoretical Calculations for Selecting the Sampler Probe Location  
Annex A2  
Portable Sampling Units  
Annex A3  
Profile Performance Test  
Annex A4  
Sampler Acceptance Test Data  
Annex A5  
APPENDIXES  
Design Data Sheet for Automatic Sampling System  
Appendix X1  
Comparisons of Percent Sediment and Water versus Unloading Time Period  
Appendix X2  
Sampling Frequency and Sampling System Monitoring Spreadsheet  
Appendix X3  
Sampling System Monitoring—Additional Diagnostics  
Appendix X4  
1.3 Units—The values stated in either SI units or US Customary (USC) units are to be regarded separately as standard. The values stated in each system may not be exact equivalents; therefore, each system shall be used independently of the other. Combining values from the two systems may result in non-conformance with the standard. Except where there is no direct SI equivalent, such as for National Pipe Threads/diameters, or tubing.  
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ASTM D4057-22(Practice)
Standard Practice for Manual Sampling of Petroleum and Petroleum Products

SIGNIFICANCE AND USE
4.1 Samples of petroleum and petroleum products are obtained for many reasons, including the determination of chemical and physical properties. These properties may be used for: calculating standard volumes; establishing product value; and often safety and regulatory reporting.  
4.2 There are inherent limitations when performing any type of sampling, any one of which may affect the representative nature of the sample. As examples, a spot sample provides a sample from only one particular point in the tank, vessel compartment, or pipeline. In the case of running or all-level samples, the sample only represents the column of material from which it was taken.  
4.3 Based on the product, and testing to be performed, this practice provides guidance on sampling equipment, container preparation, and manual sampling procedures for petroleum and petroleum products of a liquid, semi-liquid, or solid state, from the storage tanks, flowlines, pipelines, marine vessels, process vessels, drums, cans, tubes, bags, kettles, and open discharge streams into the primary sample container.
SCOPE
1.1 This practice covers procedures and equipment for manually obtaining samples of liquid petroleum and petroleum products, crude oils, and intermediate products from the sample point into the primary container are described. Procedures are also included for the sampling of free water and other heavy components associated with petroleum and petroleum products.  
1.2 This practice also addresses the sampling of semi-liquid or solid-state petroleum products. For the sampling of green petroleum coke, see Practice D8145. For the sampling of calcined petroleum coke, see Practice D6970.  
1.3 This practice provides additional specific information about sample container selection, preparation, and sample handling.  
1.4 This practice does not cover sampling of electrical insulating oils and hydraulic fluids. If sampling is for the precise determination of volatility, use Practice D5842 (API MPMS Chapter 8.4) in conjunction with this practice. For sample mixing and handling, refer to Practice D5854 (API MPMS Chapter 8.3).  
1.5 The procedures described in this practice may also be applicable in sampling most non-corrosive liquid industrial chemicals provided that all safety precautions specific to these chemicals are followed. Also, refer to Practice E300. The procedures described in this practice are also applicable to sampling liquefied petroleum gases and chemicals. Also refer to Practices D1265 and D3700. The procedure for sampling bituminous materials is described in Practice D140. Practice D4306 provides guidance on sample containers and preparation for sampling aviation fuel.  
1.6 Units—The values stated in SI units are to be regarded as the standard. USC units are reflected in parentheses.  
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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ASTM
ASTM D5291-21(Test Method)
Standard Test Methods for Instrumental Determination of Carbon, Hydrogen, and Nitrogen in Petroleum Products and Lubricants

SIGNIFICANCE AND USE
5.1 This is the first ASTM standard covering the simultaneous determination of carbon, hydrogen, and nitrogen in petroleum products and lubricants.  
5.2 Carbon, hydrogen, and particularly nitrogen analyses are useful in determining the complex nature of sample types covered by this test method. The CHN results can be used to estimate the processing and refining potentials and yields in the petrochemical industry.  
5.3 The concentration of nitrogen is a measure of the presence of nitrogen containing additives. Knowledge of its concentration can be used to predict performance. Some petroleum products also contain naturally occurring nitrogen. Knowledge of hydrogen content in samples is helpful in addressing their performance characteristics. Hydrogen to carbon ratio is useful to assess the performance of upgrading processes.
SCOPE
1.1 These test methods cover the instrumental determination of carbon, hydrogen, and nitrogen in laboratory samples of petroleum products and lubricants. Values obtained represent the total carbon, the total hydrogen, and the total nitrogen.  
1.2 These test methods are applicable to samples such as crude oils, fuel oils, additives, and residues for carbon and hydrogen and nitrogen analysis. These test methods were tested in the concentration range of at least 75 % to 87 % by mass for carbon, at least 9 % to 16 % by mass for hydrogen, and  
1.3 The nitrogen test method is not applicable to light materials or those containing  
1.3.1 However, using Test Method D levels of 0.1 % by mass nitrogen in lubricants could be determined.  
1.4 These test methods are not recommended for the analysis of volatile materials such as gasoline, gasoline-oxygenate blends, or gasoline type aviation turbine fuels.  
1.5 The results of these tests can be expressed as mass % carbon, hydrogen or nitrogen.  
1.6 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.7 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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ASTM
ASTM D6304-20(Test Method)
Standard Test Method for Determination of Water in Petroleum Products, Lubricating Oils, and Additives by Coulometric Karl Fischer Titration

SIGNIFICANCE AND USE
5.1 A knowledge of the water content is important in the manufacturing, purchase, sale, or transfer of petroleum products to help in predicting their quality and performance characteristics.  
5.2 The presence of moisture could lead to premature corrosion and wear, an increase in the debris load resulting in diminished lubrication and premature plugging of filters, an impedance in the effect of additives, and undesirable support of deleterious bacterial growth.
SCOPE
1.1 This test method covers the direct determination of entrained water in petroleum products and hydrocarbons using automated instrumentation. This test method also covers the indirect analysis of water thermally removed from samples and swept with dry inert gas into the Karl Fischer titration cell. Mercaptan, sulfide (S– or H2S), sulfur, and other compounds are known to interfere with this test method (see Section 6). The precision statement of this method covers the nominal range of 20 mg/kg to 25 000 mg/kg for Procedure A, 30 mg/kg to 2100 mg/kg for Procedure B, and 20 mg/kg to 360 mg/kg for Procedure C.  
1.2 This test method is intended for use with commercially available coulometric Karl Fischer reagents and for the determination of water in additives, lube oils, base oils, automatic transmission fluids, hydrocarbon solvents, and other petroleum products. By proper choice of the sample size, this test method may be used for the determination of water from mg/kg to percent level concentrations.  
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 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.  
1.5 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 D7260-20(Practice)
Standard Practice for Optimization, Calibration, and Validation of Inductively Coupled Plasma-Atomic Emission Spectrometry (ICP-AES) for Elemental Analysis of Petroleum Products and Lubricants

SIGNIFICANCE AND USE
4.1 Accurate elemental analysis of petroleum products and lubricants is necessary for the determination of chemical properties, which are used to establish compliance with commercial and regulatory specifications.  
4.2 Inductively coupled plasma-atomic emission spectrometry is one of the more widely used analytical techniques in the oil industry for multi-element analysis as evident from at least twelve standard test methods (for example, Test Methods C1111, D1976, D4951, D5184, D5185, D5600, D5708, D6130, D6349, D6357, D7040, D7111, D7303, and D7691) published for the analysis of fossil fuels and related materials. These have been briefly summarized by Nadkarni (1).5  
4.2.1 Determination of mercury and trace metals in crude oils using atomic spectroscopic methods is discussed in Guide D8056.  
4.3 The advantages of using an ICP-AES analysis include high sensitivity for many elements of interest in the oil industry, relative freedom from interferences, linear calibration over a wide dynamic concentration range, single or multi-element capability, and ability to calibrate the instrument based on elemental standards irrespective of their elemental chemical forms, within limits described below such as solubility and volatility assuming direct liquid aspiration. Thus, the technique has become a method of choice in most of the oil industry laboratories for metal analyses of petroleum products and lubricants.  
4.4 In addition to the ICP-AES standards listed in 2.2, a new ICP-MS standard, Test Method D8110, has been issued for analysis of distillate products for multi-element determination of Al, Ca, Cu, Fe, Pb, Mg, and K.
SCOPE
1.1 This practice covers information on the calibration and operational guidance for the multi-element measurements using inductively coupled plasma-atomic emission spectrometry (ICP-AES).  
1.2 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.  
1.3 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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