Standard Test Method for Determination of Elements in Residual Fuels and Crude Oils by Microwave Plasma Atomic Emission Spectroscopy (MP-AES)

SIGNIFICANCE AND USE
5.1 This test method covers the determination of V, Ni, Ca, Na, Al, Si, Zn, P, and S for residual fuels and Fe, V, Ni,Ca, Na, K, and S for crude oils. This test method complements and extends the capabilities of Test Methods D1548 and D5708, which only apply to the determination of Ni, V, and Fe in crude oils and residual fuels.  
5.2 The metals and other elements tested for in this method may occur naturally or may be added as a result of production (that is, catalyst fines).
SCOPE
1.1 This test method covers the determination of metals and other elements in residual fuel and crude oil by microwave plasma atomic emission spectroscopy (MP-AES). The specific elements within the scope of this method are V, Ni, Ca, Na, Al, Si, Zn, P, and S for residual fuel oil and Fe, V, Ni, Ca, Na, K, and S for crude oils.  
1.2 Method working range:
high expected concentration limit = highest ILS sample mean
low expected concentration limit = lowest ILS sample mean if:
(1) lowest ILS sample mean − Rlowest ILS sample mean > 0; otherwise it is determined by solving for X using the following equation:
(2) X − RX= coarsest resolution, determined by
0.5*σr lowest ILS sample mean    
Crude Oil:  
Element  
Method Working Range  
(expected mg/kg)  
Iron  
0.70 to 161.02  
Vanadium  
2.88 to 417.50  
Nickel  
0.36 to 107.66  
Calcium  
5.41 to 96.78  
Sodium  
1.18 to 97.13  
Potassium  
7.01 to 63.83  
Sulfur  
1059 to 35194    
Residual Fuel Oil:  
Element  
Method Working Range  
(expected mg/kg)  
Vanadium  
3.88 to 370.09  
Nickel  
1.47 to 96.68  
Calcium  
4.41 to 102.01  
Sodium  
2.80 to 112.67  
Aluminum  
4.13 to 154.12  
Silicon  
5.99 to 237.56  
Zinc  
2.75 to 102.46  
Sulfur  
1314 to 30134  
1.3 This test method uses soluble metals in organic solvents for calibration and does not purport to quantitatively determine insoluble particulates. Analytical results are particle size dependent, and particles larger than a few micrometers may cause results to appear low  
1.4 Elements present at mass fractions above the upper limit of the calibration curves can be determined with additional appropriate dilutions. Elements shall be measured at the wavelengths presented in Table 1.  
1.5 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.6 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
1.7 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

General Information

Status
Published
Publication Date
31-May-2020
Current Stage
Ref Project

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ASTM D8322-20 - Standard Test Method for Determination of Elements in Residual Fuels and Crude Oils by Microwave Plasma Atomic Emission Spectroscopy (MP-AES)
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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: D8322 − 20
Standard Test Method for
Determination of Elements in Residual Fuels and Crude Oils
by Microwave Plasma Atomic Emission Spectroscopy (MP-
1
AES)
This standard is issued under the fixed designation D8322; 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 dependent, and particles larger than a few micrometers may
cause results to appear low
1.1 Thistestmethodcoversthedeterminationofmetalsand
other elements in residual fuel and crude oil by microwave 1.4 Elementspresentatmassfractionsabovetheupperlimit
plasma atomic emission spectroscopy (MP-AES). The specific of the calibration curves can be determined with additional
elementswithinthescopeofthismethodareV,Ni,Ca,Na,Al, appropriate dilutions. Elements shall be measured at the
Si, Zn, P, and S for residual fuel oil and Fe, V, Ni, Ca, Na, K, wavelengths presented in Table 1.
and S for crude oils.
1.5 The values stated in SI units are to be regarded as
1.2 Method working range: standard. No other units of measurement are included in this
high expected concentration limit = highest ILS sample mean standard.
lowexpectedconcentrationlimit=lowestILSsamplemeanif:
1.6 This standard does not purport to address all of the
(1)lowest ILS sample mean − R >0;
lowest ILS sample mean
safety concerns, if any, associated with its use. It is the
otherwiseitisdeterminedbysolvingfor Xusingthefollowing
responsibility of the user of this standard to establish appro-
equation:
priate safety, health, and environmental practices and deter-
(2) X−R = coarsest resolution, determined by
X
mine the applicability of regulatory limitations prior to use.
0.5*σ
r lowest ILS sample mean
1.7 This international standard was developed in accor-
Crude Oil:
dance with internationally recognized principles on standard-
Method Working Range
Element ization established in the Decision on Principles for the
(expected mg/kg)
Development of International Standards, Guides and Recom-
Iron 0.70 to 161.02
Vanadium 2.88 to 417.50
mendations issued by the World Trade Organization Technical
Nickel 0.36 to 107.66
Barriers to Trade (TBT) Committee.
Calcium 5.41 to 96.78
Sodium 1.18 to 97.13
2. Referenced Documents
Potassium 7.01 to 63.83
Sulfur 1059 to 35194
2
2.1 ASTM Standards:
Residual Fuel Oil:
D1298Test Method for Density, Relative Density, or API
Method Working Range
Element
(expected mg/kg) Gravity of Crude Petroleum and Liquid Petroleum Prod-
Vanadium 3.88 to 370.09
ucts by Hydrometer Method
Nickel 1.47 to 96.68
1
D1548Test Method for Vanadium in Heavy Fuel Oil
Calcium 4.41 to 102.01
3
Sodium 2.80 to 112.67 (Withdrawn 1997)
Aluminum 4.13 to 154.12
D4052Test Method for Density, Relative Density, and API
Silicon 5.99 to 237.56
Gravity of Liquids by Digital Density Meter
Zinc 2.75 to 102.46
Sulfur 1314 to 30134 D4175Terminology Relating to Petroleum Products, Liquid
Fuels, and Lubricants
1.3 Thistestmethodusessolublemetalsinorganicsolvents
D5708 Test Methods for Determination of Nickel,
forcalibrationanddoesnotpurporttoquantitativelydetermine
Vanadium, and Iron in Crude Oils and Residual Fuels by
insoluble particulates. Analytical results are particle size
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
1
This test method is under the jurisdiction of ASTM Committee D02 on contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of Standards volume information, refer to the standard’s Document Summary page on
Subcommittee D02.03 on Elemental Analysis. the ASTM website.
3
Current edition approved June 1, 2020. Published July 2020. DOI: 10.1520/ The last approved version of this historical standard is referenced on
D8322-20. www.astm.org.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

---------------------- Page: 1 ----------------------
D8322 − 20
TABLE 1 Element Wavelengths
median of the linear calibration range and 10% of the highest
massfractionstandard(seePracticeD6792forguidanceinthis
NOTE 1—These wavelengths shall be used for this method. The
area).
precision for this method is based on these wavelengths.
Element Wavelength, nm Standards Used in Each Curve
3.2.3 continuing calibration blank (CCB), n—a blank cali-
(mg/kg)
bration standard that does not contain any elements of interest,
Iron 259.940 Solvent blank, 0.1, 1
...

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