ASTM D8110-17

Standard Test Method for Elemental Analysis of Distillate Products by Inductively Coupled Plasma Mass Spectrometry (ICP-MS)

SIGNIFICANCE AND USE
5.1 Petroleum products may contain elements either in trace concentrations (for example, ng/g (ppb mass)) or in minor to major levels (ppm to mass %). These elements might be characteristic of the crude petroleum or might originate from specific inclusions of additives for beneficial effect in the refined product. Often, such additives have product specifications which control the quality of a product in commerce. Hence, it is important to determine these elements as accurately as possible. Other elements present at trace levels may be harmful to combustion engines causing wear or reduced performance, may cause poisoning of catalysts, or may be of environmental concern as combustion emissions. ICP-MS instrumentation is well-suited for determining these elements and is particularly useful for the determination of the trace level elements that may not be readily achieved by other techniques.  
5.2 Various elemental analytical techniques such as atomic absorption spectrometry (AAS), for example, Test Method D3605 and D4628; inductively coupled plasma atomic emission spectrometry (ICP-AES), for example, Test Methods D7111, D4951, and D5185; X-ray fluorescence (XRF), for example, Practice D7343, Test Method D7220, Test Methods D4927, and Test Method D6443; or graphite furnace atomic absorption spectrometry (GFAAS), for example, Test Method D6732 are used for this purpose. This test method is the first example where ICP-MS is used for elemental analysis of petroleum products.  
5.3 This test method covers the rapid determination of seven elements in distillate petroleum products. Test times approximate a few minutes per test specimen, and quantification for most elements is in the low to sub ng/g (ppb mass) range. High analysis sensitivity can be achieved for some elements that are difficult to determine by other techniques.
SCOPE
1.1 This test method describes the procedure for the determination of trace elements in light and middle distillate petroleum products using inductively coupled plasma mass spectrometry (ICP-MS).  
1.2 This test method should be used by analysts experienced in the use of inductively coupled plasma mass spectrometry (ICP-MS) with knowledge of interpretation of spectral, isobaric, polyatomic, and matrix interferences, as well as procedures for their correction or reduction.  
1.3 The table in 6.1 lists elements for which the test method applies along with recommended isotope. Actual working detection limits are sample dependent and, as the sample matrix varies, these detection limits may also vary.  
1.4 The concentration range of this test method is typically from low to sub ng/g (ppb mass) to 1000 ng/g (ppb mass), however the precision and bias statement is specified for a smaller concentration range based on test samples analyzed in the ILS, see the table in Section 18. The test method may be used for concentrations outside of this range; however, the precision statements may not be applicable.  
1.4.1 This test method shall be further developed to extend that table to include additional elements.  
1.5 This test method uses metallo-organic standards (organometallic or organosoluble metal complex) for calibration and does not purport to quantitatively determine insoluble particulates. Analytical results are particle size dependent, and low results are obtained for particles larger than a few micrometers as these particles may settle out in the sample container and are not effectively transported through the sample introduction system.  
1.6 Elements present at concentrations above the upper limit of the calibration curves can be determined with additional, appropriate dilutions and with no degradation of precision.  
1.7 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.8 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the r...

General Information

• Status: Published
• Publication Date: 30-Apr-2017
• ICS: 75.160.20 - Liquid fuels
• Technical Committee: D02 - Petroleum Products, Liquid Fuels, and Lubricants
• Drafting Committee: D02.03 - Elemental Analysis

Relations

• 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 D4307-99(2015) - Standard Practice for Preparation of Liquid Blends for Use as Analytical Standards
• Effective Date: 01-Oct-2015
• Refers: ASTM D4306-15 - Standard Practice for Aviation Fuel Sample Containers for Tests Affected by Trace Contamination
• Effective Date: 01-Oct-2015
• Refers: ASTM D5185-18 - Standard Test Method for Multielement Determination of Used and Unused Lubricating Oils and Base Oils by Inductively Coupled Plasma Atomic Emission Spectrometry (ICP-AES)
• Effective Date: 01-Apr-2018
• Refers: ASTM D4927-14 - Standard Test Methods for Elemental Analysis of Lubricant and Additive Components—Barium, Calcium, Phosphorus, Sulfur, and Zinc by Wavelength-Dispersive X-Ray Fluorescence Spectroscopy
• Effective Date: 01-Dec-2014
• Refers: ASTM D7111-15 - Standard Test Method for Determination of Trace Elements in Middle Distillate Fuels by Inductively Coupled Plasma Atomic Emission Spectrometry (ICP-AES)
• Effective Date: 01-Apr-2015
• Refers: ASTM D6300-15 - Standard Practice for Determination of Precision and Bias Data for Use in Test Methods for Petroleum Products and Lubricants
• Effective Date: 01-Jun-2015
• Refers: ASTM D6300-16 - Standard Practice for Determination of Precision and Bias Data for Use in Test Methods for Petroleum Products and Lubricants
• Effective Date: 01-Apr-2016
• 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 D6299-17a - Standard Practice for Applying Statistical Quality Assurance and Control Charting Techniques to Evaluate Analytical Measurement System Performance
• Effective Date: 15-Nov-2017
• Refers: ASTM 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 D6443-14 - Standard Test Method for Determination of Calcium, Chlorine, Copper, Magnesium, Phosphorus, Sulfur, and Zinc in Unused Lubricating Oils and Additives by Wavelength Dispersive X-ray Fluorescence Spectrometry (Mathematical Correction Procedure)
• Effective Date: 01-Dec-2014
• Refers: ASTM D6443-14(2019)e1 - Standard Test Method for Determination of Calcium, Chlorine, Copper, Magnesium, Phosphorus, Sulfur, and Zinc in Unused Lubricating Oils and Additives by Wavelength Dispersive X-ray Fluorescence Spectrometry (Mathematical Correction Procedure)
• Effective Date: 01-May-2019
• Refers: ASTM D6300-19a - Standard Practice for Determination of Precision and Bias Data for Use in Test Methods for Petroleum Products and Lubricants
• Effective Date: 01-Dec-2019
• Refers: ASTM D6732-04(2020) - Standard Test Method for Determination of Copper in Jet Fuels by Graphite Furnace Atomic Absorption Spectrometry
• Effective Date: 01-May-2020
• Refers: ASTM D4628-14 - Standard Test Method for Analysis of Barium, Calcium, Magnesium, and Zinc in Unused Lubricating Oils by Atomic Absorption Spectrometry
• Effective Date: 01-Dec-2014
• Referred By: ASTM D7260-20 - Standard Practice for Optimization, Calibration, and Validation of Inductively Coupled Plasma-Atomic Emission Spectrometry (ICP-AES) for Elemental Analysis of Petroleum Products and Lubricants
• Effective Date: 01-May-2017
• Referred By: ASTM D7578-20 - Standard Guide for Calibration Requirements for Elemental Analysis of Petroleum Products and Lubricants
• Effective Date: 01-May-2017
• Referred By: ASTM D7455-19 - Standard Practice for Sample Preparation of Petroleum and Lubricant Products for Elemental Analysis
• Effective Date: 01-May-2017

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: D8110 − 17
Standard Test Method for
Elemental Analysis of Distillate Products by Inductively
1
Coupled Plasma Mass Spectrometry (ICP-MS)
This standard is issued under the fixed designation D8110; 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.
INTRODUCTION
Certain elements present in distillate petroleum can either adversely or constructively affect the
performanceoftheproductandthusimpactsitsutilityandmarketvalue.Theindustryhastraditionally
relied on inductively coupled plasma atomic emission spectrometry (ICP-AES) or atomic absorption
spectrometry (AAS) to determine the concentration of these elements present in the product. As
specifications have become more stringent, a need to extend these measurements to lower
concentrations by employing more sensitive measurement technologies has arisen. Inductively
coupled plasma mass spectrometry is ideal for this application for most distillate petroleum products.
By applying ICP-MS for elemental analysis of these products, the concentration range of detectable
elements can be extended from low to sub ng/g (ppb mass) to 1000 ng/g (ppb mass) for some
elements.
1. Scope 1.4.1 This test method shall be further developed to extend
that table to include additional elements.
1.1 This test method describes the procedure for the deter-
1.5 This test method uses metallo-organic standards (orga-
mination of trace elements in light and middle distillate
nometallicororganosolublemetalcomplex)forcalibrationand
petroleum products using inductively coupled plasma mass
does not purport to quantitatively determine insoluble particu-
spectrometry (ICP-MS).
lates. Analytical results are particle size dependent, and low
1.2 Thistestmethodshouldbeusedbyanalystsexperienced
results are obtained for particles larger than a few micrometers
in the use of inductively coupled plasma mass spectrometry
astheseparticlesmaysettleoutinthesamplecontainerandare
(ICP-MS) with knowledge of interpretation of spectral,
not effectively transported through the sample introduction
isobaric, polyatomic, and matrix interferences, as well as
system.
procedures for their correction or reduction.
1.6 Elementspresentatconcentrationsabovetheupperlimit
1.3 Thetablein6.1listselementsforwhichthetestmethod
of the calibration curves can be determined with additional,
applies along with recommended isotope. Actual working
appropriate dilutions and with no degradation of precision.
detection limits are sample dependent and, as the sample
1.7 The values stated in SI units are to be regarded as
matrix varies, these detection limits may also vary.
standard. No other units of measurement are included in this
1.4 The concentration range of this test method is typically
standard.
from low to sub ng/g (ppb mass) to 1000 ng/g (ppb mass),
1.8 This standard does not purport to address all of the
however the precision and bias statement is specified for a
safety concerns, if any, associated with its use. It is the
smaller concentration range based on test samples analyzed in
responsibility of the user of this standard to establish appro-
the ILS, see the table in Section 18. The test method may be
priate safety and health practices and determine the applica-
used for concentrations outside of this range; however, the
bility of regulatory limitations prior to use. Specific warning
precision statements may not be applicable.
statements are given in 8.2, 8.7, and Section 9.
1.9 This international standard was developed in accor-
dance with internationally recognized principles on standard-
1
This test method is under the jurisdiction of ASTM Committee D02 on
ization established in the Decision on Principles for the
Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of
Development of International Standards, Guides and Recom-
Subcommittee D02.03 on Elemental Analysis.
mendations issued by the World Trade Organization Technical
Current edition approved May 1, 2017. Published May 2017. DOI: 10.1520/
D8110-17. Barriers to Trade (TBT) Committee.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
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D8110 − 17
2. Referenced Documents Products and Lubricants
2 D7778Guide for Conducting an Interlaboratory Study to
2.1 ASTM Standards:
Determine the Precision of a Test Method
D3605Test Method for Trace Metals in Gas Turbin
...