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ASTM D7260-12

(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

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
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.
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, , D7040, D7111, D7303, and D7691) published for the analysis of fossil fuels and related materials. These have been briefly summarized by Nadkarni.  
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.
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 and health practices and determine the applicability of regulatory limitations prior to use.

General Information

Status
Historical
Publication Date
31-May-2012
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

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ASTM D7260-12 - Standard Practice for Optimization, Calibration, and Validation of Inductively Coupled Plasma-Atomic Emission Spectrometry (ICP-AES) for Elemental Analysis of Petroleum Products and LubricantsASTM D7260-12 - Standard Practice for Optimization, Calibration, and Validation of Inductively Coupled Plasma-Atomic Emission Spectrometry (ICP-AES) for Elemental Analysis of Petroleum Products and Lubricants
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REDLINE ASTM D7260-12 - Standard Practice for Optimization, Calibration, and Validation of Inductively Coupled Plasma-Atomic Emission Spectrometry (ICP-AES) for Elemental Analysis of Petroleum Products and LubricantsREDLINE ASTM D7260-12 - Standard Practice for Optimization, Calibration, and Validation of Inductively Coupled Plasma-Atomic Emission Spectrometry (ICP-AES) for Elemental Analysis of Petroleum Products and Lubricants
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REDLINE ASTM D7260-12 - Standard Practice for Optimization, Calibration, and Validation of Inductively Coupled Plasma-Atomic Emission Spectrometry (ICP-AES) for Elemental Analysis of Petroleum Products and Lubricants
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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: D7260 − 12
Standard Practice for
Optimization, Calibration, and Validation of Inductively
Coupled Plasma-Atomic Emission Spectrometry (ICP-AES)
for Elemental Analysis of Petroleum Products and
1
Lubricants
This standard is issued under the fixed designation D7260; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision.Anumber in parentheses indicates the year of last reapproval.A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope* D1976Test Method for Elements in Water by Inductively-
Coupled Argon Plasma Atomic Emission Spectroscopy
1.1 This practice covers information on the calibration and
D4951TestMethodforDeterminationofAdditiveElements
operational guidance for the multi-element measurements us-
in Lubricating Oils by Inductively Coupled Plasma
ing inductively coupled plasma-atomic emission spectrometry
Atomic Emission Spectrometry
(ICP-AES).
D5184Test Methods for Determination of Aluminum and
1.2 This standard does not purport to address all of the
Silicon in Fuel Oils by Ashing, Fusion, Inductively
safety concerns, if any, associated with its use. It is the
Coupled Plasma Atomic Emission Spectrometry, and
responsibility of the user of this standard to establish appro-
Atomic Absorption Spectrometry
priate safety and health practices and determine the applica-
D5185TestMethodforDeterminationofAdditiveElements,
bility of regulatory limitations prior to use.
Wear Metals, and Contaminants in Used Lubricating Oils
and Determination of Selected Elements in Base Oils by
2. Referenced Documents
Inductively Coupled Plasma Atomic Emission Spectrom-
2
2.1 ASTM Standards:
etry (ICP-AES)
D4057Practice for Manual Sampling of Petroleum and
D5600Test Method for Trace Metals in Petroleum Coke by
Petroleum Products
Inductively Coupled Plasma Atomic Emission Spectrom-
D4307Practice for Preparation of Liquid Blends for Use as
etry (ICP-AES)
Analytical Standards
D5708 Test Methods for Determination of Nickel,
D6299Practice for Applying Statistical Quality Assurance
Vanadium, and Iron in Crude Oils and Residual Fuels by
and Control Charting Techniques to Evaluate Analytical
Inductively Coupled Plasma (ICP) Atomic Emission
Measurement System Performance
Spectrometry
D6792Practice for Quality System in Petroleum Products
D6130Test Method for Determination of Silicon and Other
and Lubricants Testing Laboratories
Elements in Engine Coolant by Inductively Coupled
2.2 ICP-AES Related Standards:
Plasma-Atomic Emission Spectroscopy
C1111Test Method for Determining Elements in Waste
D6349Test Method for Determination of Major and Minor
StreamsbyInductivelyCoupledPlasma-AtomicEmission Elements in Coal, Coke, and Solid Residues from Com-
Spectroscopy
bustion of Coal and Coke by Inductively Coupled
C1109Practice for Analysis of Aqueous Leachates from Plasma—Atomic Emission Spectrometry
Nuclear Waste Materials Using Inductively Coupled
D6357TestMethodsforDeterminationofTraceElementsin
Plasma-Atomic Emission Spectroscopy Coal, Coke, and Combustion Residues from Coal Utiliza-
tion Processes by Inductively Coupled Plasma Atomic
Emission Spectrometry, Inductively Coupled Plasma
1
This practice is under the jurisdiction ofASTM Committee D02 on Petroleum
Mass Spectrometry, and Graphite Furnace Atomic Ab
ProductsandLubricantsandisthedirectresponsibilityofSubcommitteeD02.03on
D7040Test Method for Determination of Low Levels of
Elemental Analysis.
Phosphorus in ILSAC GF 4 and Similar Grade Engine
Current edition approved June 1, 2012. Published August 2012. Originally
Oils by Inductively Coupled Plasma Atomic Emission
approved in 2006. Last previous edition approved in 2006 as D7260–06. DOI:
10.1520/D7260-12.
Spectrometry
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
D7111Test Method for Determination of Trace Elements in
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Middle Distillate Fuels by Inductively Coupled Plasma
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. Atomic Emission Spectrometry (ICP-AES)
*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 ----------------------
D7260 − 12
D7303Test Method for Determination of Metals in Lubri- required. The spectrometer may be of the simultaneous multi-
cating Greases by Inductively Coupled Plasma Atomic elemental or sequential scanning type. The spectrometer may
Emission Spectrometry be of the air path, inert gas path, or vacuum type, with spectral
D7691TestMethodforMultielementAnalysisofCrudeOils lines selected app
...

This document is not anASTM standard and is intended only to provide the user of anASTM 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:D7260–06 Designation:D7260–12
Standard Practice for
Optimization, Calibration, and Validation of Inductively
Coupled Plasma-Atomic Emission Spectrometry (ICP-AES)
for Elemental Analysis of Petroleum Products and
1
Lubricants
This standard is issued under the fixed designation D7260; 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*
1.1 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 and health practices and determine the applicability of regulatory
limitations prior to use.
2. Referenced Documents
2
2.1 ASTM Standards:
D4057 Practice for Manual Sampling of Petroleum and Petroleum Products
D4307 Practice for Preparation of Liquid Blends for Use as Analytical Standards
D6299 Practice for Applying Statistical Quality Assurance and Control Charting Techniques to Evaluate Analytical
Measurement System Performance
D6792 Practice for Quality System in Petroleum Products and Lubricants Testing Laboratories
2.2 ICP-AES Related Standards:
C1111 Test Method for Determining Elements in Waste Streams by Inductively Coupled Plasma-Atomic Emission Spectros-
copy
C1109 Practice for Analysis of Aqueous Leachates from Nuclear Waste Materials Using Inductively Coupled Plasma-Atomic
Emission Spectroscopy
D1976 Test Method for Elements in Water by Inductively-Coupled Argon Plasma Atomic Emission Spectroscopy
D4951 Test Method for Determination of Additive Elements in Lubricating Oils by Inductively Coupled Plasma Atomic
Emission Spectrometry
D5184 Test Methods for Determination ofAluminum and Silicon in Fuel Oils byAshing, Fusion, Inductively Coupled Plasma
Atomic Emission Spectrometry, and Atomic Absorption Spectrometry
D5185 Test Method for Determination of Additive Elements, Wear Metals, and Contaminants in Used Lubricating Oils and
Determination of Selected Elements in Base Oils by Inductively Coupled PlasmaAtomic Emission Spectrometry (ICP-AES)
D5600 Test Method for Trace Metals in Petroleum Coke by Inductively Coupled Plasma Atomic Emission Spectrometry
(ICP-AES)
D5708 TestMethodsforDeterminationofNickel,Vanadium,andIroninCrudeOilsandResidualFuelsbyInductivelyCoupled
Plasma (ICP) Atomic Emission Spectrometry
D6130 Test Method for Determination of Silicon and Other Elements in Engine Coolant by Inductively Coupled Plasma-
Atomic Emission Spectroscopy
D6349 Test Method for Determination of Major and Minor Elements in Coal, Coke, and Solid Residues from Combustion of
Coal and Coke by Inductively Coupled PlasmaAtomic Emission Spectrometry
D6357D6357Test Test Methods for Determination of Trace Elements in Coal, Coke, and& Combustion Residues from Coal
1
This practice is under the jurisdiction of ASTM Committee D02 on Petroleum Products and Lubricants and is the direct responsibility of Subcommittee D02.03 on
Elemental Analysis.
Current edition approved May 1, 2006. Published June 2006. DOI: 10.1520/D7260-06.
Current edition approved June 1, 2012. Published August 2012. Originally approved in 2006. Last previous edition approved in 2006 as D7260–06. DOI:
10.1520/D7260-12.
2
For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM 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.
*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 ----------------------
D7260–12
Utilization Processes by Inductively Coupled PlasmaAtomic Emission Spectrometry, Emission, Inductively Coupled Plasma
Mass Spectrometry, and Mass, & Graphite Furnace Atomic Ab Absorption Spectrometry
D7040 Test Method for Determination of Low Levels of Phosphorus in ILSAC GF 4 and Similar Grade Engine Oils by
Inductively Coupled Plasma Atomic Emission Spectrometry
D7111 Test Method for Determination of Trace Elements in Middle Distillate Fuels by Ind
...

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ASTM D1159-23(Test Method)
Standard Test Method for Bromine Numbers of Petroleum Distillates and Commercial Aliphatic Olefins by Electrometric Titration

SIGNIFICANCE AND USE
5.1 The bromine number is useful as a measure of aliphatic unsaturation in petroleum samples. When used in conjunction with the calculation procedure described in Annex A2, it can be used to estimate the percentage of olefins in petroleum distillates boiling up to approximately 315 °C (600 °F).  
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SCOPE
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1.3 For petroleum hydrocarbon mixtures of bromine number less than 1.0, a more precise measure for bromine-reactive constituents can be obtained by using Test Method D2710. If the bromine number is less than 0.5, then Test Method D2710 or the comparable bromine index methods for industrial aromatic hydrocarbons, Test Methods D1492 or D5776 must be used in accordance with their respective scopes. The practice of using a factor of 1000 to convert bromine number to bromine index is not applicable for these lower values of bromine number.  
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SCOPE
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SCOPE
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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
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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  
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Sample Handling and Mixing  
13  
Control Systems  
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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.  
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 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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