ASTM D8252-19e1

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.  
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.

General Information

• Status: Historical
• Publication Date: 31-Jul-2019
• ICS: 75.040 - Crude petroleum
• ICS: 75.160.20 - Liquid fuels
• Technical Committee: D02 - Petroleum Products, Liquid Fuels, and Lubricants
• Drafting Committee: D02.03 - Elemental Analysis

Relations

• Replaces: ASTM D8252-19 - Standard Test Method for Vanadium and Nickel in Crude and Residual Oil by X-ray Spectrometry
• Effective Date: 01-Aug-2019
• Replaced By: ASTM D8252-23 - Standard Test Method for Vanadium and Nickel in Crude and Residual Oil by X-ray Spectrometry
• Effective Date: 01-Nov-2023
• Refers: ASTM D6299-17b - Standard Practice for Applying Statistical Quality Assurance and Control Charting Techniques to Evaluate Analytical Measurement System Performance
• Effective Date: 15-Dec-2017
• Refers: ASTM D6299-17a - Standard Practice for Applying Statistical Quality Assurance and Control Charting Techniques to Evaluate Analytical Measurement System Performance
• Effective Date: 15-Nov-2017
• Refers: ASTM D7343-12(2017) - Standard Practice for Optimization, Sample Handling, Calibration, and Validation of X-ray Fluorescence Spectrometry Methods for Elemental Analysis of Petroleum Products and Lubricants
• Effective Date: 01-Jun-2017
• Refers: ASTM D6299-17 - Standard Practice for Applying Statistical Quality Assurance and Control Charting Techniques to Evaluate Analytical Measurement System Performance
• Effective Date: 01-Jan-2017
• Refers: ASTM D4294-16 - Standard Test Method for Sulfur in Petroleum and Petroleum Products by Energy Dispersive X-ray Fluorescence Spectrometry
• Effective Date: 01-Jan-2016
• Refers: ASTM D6299-13e1 - Standard Practice for Applying Statistical Quality Assurance and Control Charting Techniques to Evaluate Analytical Measurement System Performance
• Effective Date: 01-Oct-2013
• Refers: ASTM D4057-06(2011) - Standard Practice for Manual Sampling of Petroleum and Petroleum Products
• Effective Date: 01-Jun-2011
• Refers: ASTM D6259-98(2010) - Standard Practice for Determination of a Pooled Limit of Quantitation
• Effective Date: 01-Jul-2010
• Refers: ASTM D6299-10 - Standard Practice for Applying Statistical Quality Assurance and Control Charting Techniques to Evaluate Analytical Measurement System Performance
• Effective Date: 01-Mar-2010
• Refers: ASTM D6299-10e2 - Standard Practice for Applying Statistical Quality Assurance and Control Charting Techniques to Evaluate Analytical Measurement System Performance
• Effective Date: 01-Mar-2010
• Refers: ASTM D6299-09 - Standard Practice for Applying Statistical Quality Assurance and Control Charting Techniques to Evaluate Analytical Measurement System Performance
• Effective Date: 01-Nov-2009
• Refers: ASTM D6299-08 - Standard Practice for Applying Statistical Quality Assurance and Control Charting Techniques to Evaluate Analytical Measurement System Performance
• Effective Date: 15-Oct-2008
• Refers: ASTM D4294-08a - Standard Test Method for Sulfur in Petroleum and Petroleum Products by Energy Dispersive X-ray Fluorescence Spectrometry
• Effective Date: 15-Oct-2008

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.
´1
Designation: D8252 − 19
Standard Test Method for
Vanadium and Nickel in Crude and Residual Oil by X-ray
1
Spectrometry
This standard is issued under the fixed designation D8252; 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
ε NOTE—The title of Table 7 was corrected editorially in October 2019.
1. Scope 1.8 This international standard was developed in accor-
dance with internationally recognized principles on standard-
1.1 This test method covers the quantitative determination
ization established in the Decision on Principles for the
of total vanadium and nickel in crude and residual oil in the
Development of International Standards, Guides and Recom-
concentration ranges shown in Table 1 using X-ray fluores-
mendations issued by the World Trade Organization Technical
cence (XRF) spectrometry.
Barriers to Trade (TBT) Committee.
1.2 Sulfur is measured for analytical purposes only for the
2. Referenced Documents
compensation of X-ray absorption matrix effects affecting the
2
vanadium and nickel X-rays. For measurement of sulfur by
2.1 ASTM Standards:
standard test method use Test Methods D4294, D2622 or other
D2622 Test Method for Sulfur in Petroleum Products by
suitable standard test method for sulfur in crude and residual
Wavelength Dispersive X-ray Fluorescence Spectrometry
oils.
D4057 Practice for Manual Sampling of Petroleum and
Petroleum Products
1.3 This test method is limited to the use of X-ray fluores-
D4177 Practice for Automatic Sampling of Petroleum and
cence (XRF) spectrometers employing an X-ray tube for
Petroleum Products
excitation in conjunction with wavelength dispersive detection
D4294 Test Method for Sulfur in Petroleum and Petroleum
system or energy dispersive high resolution semiconductor
Products by Energy Dispersive X-ray Fluorescence Spec-
detector with the ability to separate signals of adjacent and
trometry
near-adjacent elements.
D6259 Practice for Determination of a Pooled Limit of
1.4 This test method uses inter-element correction factors
Quantitation for a Test Method
calculated from XRF theory, the fundamental parameters (FP)
D6299 Practice for Applying Statistical Quality Assurance
approach, or best fit regression.
and Control Charting Techniques to Evaluate Analytical
1.5 Samplescontaininghigherconcentrationsthanshownin
Measurement System Performance
Table 1 must be diluted to bring the elemental concentration of
D7343 Practice for Optimization, Sample Handling,
the diluted material within the scope of this test method.
Calibration, and Validation of X-ray Fluorescence Spec-
trometry Methods for Elemental Analysis of Petroleum
1.6 The values stated in SI units are to be regarded as
Products and Lubricants
standard. No other units of measurement are included in this
E1621 Guide for ElementalAnalysis by Wavelength Disper-
standard.
sive X-Ray Fluorescence Spectrometry
1.6.1 The preferred concentrations units are mg/kg for
vanadium and nickel.
3. Terminology
1.7 This standard does not purport to address all of the
3.1 Definitions:
safety concerns, if any, associated with its use. It is the
3.1.1 alpha corrections, n—influence correction factors that
responsibility of the user of this standard to establish appro-
compensate for inter-element X-ray matrix effects; alpha cor-
priate safety, health, and environmental practices and deter-
rections may be determined by best-fit regression, XRF Fun-
mine the applicability of regulatory limitations prior to use.
damental Parameters (FP), or XRF theory (called theoretical
alphas).
1
This test method is under the jurisdiction of ASTM Committee D02 on
2
Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Subcommittee D02.03 on Elemental Analysis. contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
Current edition approved Aug. 1, 2019. Published August 2019. DOI: 10.1520/ Standards volume information, refer to the standard’s Document Summary page on
D8252-19E01 the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

---------------------- Page: 1 ----------------------
´1
D8252 − 19
TABLE 1 Elements and Ranges of Applicability
3.2.5 PLOQ—pooled limited of quantification based on
Max Concentration in pooled data of instrumentation used in the ILS (see Practice
Element P
...

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
´1
Designation: D8252 − 19
Standard Test Method for
Vanadium and Nickel in Crude and Residual Oil by X-ray
1
Spectrometry
This standard is issued under the fixed designation D8252; 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
ε NOTE—The title of Table 7 was corrected editorially in October 2019.
1. Scope 1.8 This international standard was developed in accor-
dance with internationally recognized principles on standard-
1.1 This test method covers the quantitative determination
ization established in the Decision on Principles for the
of total vanadium and nickel in crude and residual oil in the
Development of International Standards, Guides and Recom-
concentration ranges shown in Table 1 using X-ray fluores-
mendations issued by the World Trade Organization Technical
cence (XRF) spectrometry.
Barriers to Trade (TBT) Committee.
1.2 Sulfur is measured for analytical purposes only for the
2. Referenced Documents
compensation of X-ray absorption matrix effects affecting the
2
vanadium and nickel X-rays. For measurement of sulfur by
2.1 ASTM Standards:
standard test method use Test Methods D4294, D2622 or other
D2622 Test Method for Sulfur in Petroleum Products by
suitable standard test method for sulfur in crude and residual
Wavelength Dispersive X-ray Fluorescence Spectrometry
oils.
D4057 Practice for Manual Sampling of Petroleum and
Petroleum Products
1.3 This test method is limited to the use of X-ray fluores-
D4177 Practice for Automatic Sampling of Petroleum and
cence (XRF) spectrometers employing an X-ray tube for
Petroleum Products
excitation in conjunction with wavelength dispersive detection
D4294 Test Method for Sulfur in Petroleum and Petroleum
system or energy dispersive high resolution semiconductor
Products by Energy Dispersive X-ray Fluorescence Spec-
detector with the ability to separate signals of adjacent and
trometry
near-adjacent elements.
D6259 Practice for Determination of a Pooled Limit of
1.4 This test method uses inter-element correction factors
Quantitation for a Test Method
calculated from XRF theory, the fundamental parameters (FP)
D6299 Practice for Applying Statistical Quality Assurance
approach, or best fit regression.
and Control Charting Techniques to Evaluate Analytical
1.5 Samples containing higher concentrations than shown in
Measurement System Performance
Table 1 must be diluted to bring the elemental concentration of
D7343 Practice for Optimization, Sample Handling,
the diluted material within the scope of this test method.
Calibration, and Validation of X-ray Fluorescence Spec-
trometry Methods for Elemental Analysis of Petroleum
1.6 The values stated in SI units are to be regarded as
Products and Lubricants
standard. No other units of measurement are included in this
E1621 Guide for Elemental Analysis by Wavelength Disper-
standard.
sive X-Ray Fluorescence Spectrometry
1.6.1 The preferred concentrations units are mg/kg for
vanadium and nickel.
3. Terminology
1.7 This standard does not purport to address all of the
3.1 Definitions:
safety concerns, if any, associated with its use. It is the
3.1.1 alpha corrections, n—influence correction factors that
responsibility of the user of this standard to establish appro-
compensate for inter-element X-ray matrix effects; alpha cor-
priate safety, health, and environmental practices and deter-
rections may be determined by best-fit regression, XRF Fun-
mine the applicability of regulatory limitations prior to use.
damental Parameters (FP), or XRF theory (called theoretical
alphas).
1
This test method is under the jurisdiction of ASTM Committee D02 on
2
Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Subcommittee D02.03 on Elemental Analysis. contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
Current edition approved Aug. 1, 2019. Published August 2019. DOI: 10.1520/ Standards volume information, refer to the standard’s Document Summary page on
D8252-19E01 the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

---------------------- Page: 1 ----------------------
´1
D8252 − 19
TABLE 1 Elements and Ranges of Applicability
3.2.5 PLOQ—pooled limited of quantification based on
Max Concentration in pooled data of instrumentation used in the ILS (see Practice
Element PLOQ in mg/kg
mg/kg
D6259)
Vanadium 1.9 50
3.2.6 PXRF—polychromatic XRF (can be EDXRF or
Nickel 2.2 50
WDXRF)
3.2.7 ROI—region of interest
3.2.
...

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.
´1
Designation: D8252 − 19 D8252 − 19
Standard Test Method for
Vanadium and Nickel in Crude and Residual Oil by X-ray
1
Spectrometry
This standard is issued under the fixed designation D8252; 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
ε NOTE—The title of Table 7 was corrected editorially in October 2019.
1. 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.
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.
2. Referenced Documents
2
2.1 ASTM Standards:
D2622 Test Method for Sulfur in Petroleum Products by Wavelength Dispersive X-ray Fluorescence Spectrometry
D4057 Practice for Manual Sampling of Petroleum and Petroleum Products
D4177 Practice for Automatic Sampling of Petroleum and Petroleum Products
D4294 Test Method for Sulfur in Petroleum and Petroleum Products by Energy Dispersive X-ray Fluorescence Spectrometry
D6259 Practice for Determination of a Pooled Limit of Quantitation for a Test Method
D6299 Practice for Applying Statistical Quality Assurance and Control Charting Techniques to Evaluate Analytical Measure-
ment System Performance
D7343 Practice for Optimization, Sample Handling, Calibration, and Validation of X-ray Fluorescence Spectrometry Methods
for Elemental Analysis of Petroleum Products and Lubricants
E1621 Guide for Elemental Analysis by Wavelength Dispersive X-Ray Fluorescence Spectrometry
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 Aug. 1, 2019. Published August 2019. DOI: 10.1520/D8252-19.10.1520/D8252-19E01.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

---------------------- Page: 1 ----------------------
´1
D8252 − 19
TABLE 1 Elements and Ranges of Applicability
Max Concentration in
Element PLOQ in mg/kg
mg/kg
Vanadium 1.9 50
Nickel 2.2 50
3. Terminology
3.1 Definitions:
3.1.1 alpha corrections, n—influence correction factors that compensate for inter-element X-ray matrix effects; alpha
corrections may be determined by best-fit regression, XRF F
...