ASTM D5839-15
(Test Method)Standard Test Method for Trace Element Analysis of Hazardous Waste Fuel by Energy-Dispersive X-Ray Fluorescence Spectrometry
Standard Test Method for Trace Element Analysis of Hazardous Waste Fuel by Energy-Dispersive X-Ray Fluorescence Spectrometry
SIGNIFICANCE AND USE
4.1 The analysis of trace elements is often a regulatory and process specific requirement for facilities utilizing LHWF. With proper instrument standardization, set-up, and quality control, this test method provides the user an accurate, rapid, nondestructive method for trace element determinations.
SCOPE
1.1 This test method applies to the determination of trace element concentrations by energy-dispersive X-ray fluorescence (EDXRF) spectrometry in typical liquid hazardous waste fuels (LHWF) used by industrial furnaces.
1.2 This test method has been used successfully on numerous samples of LHWF that are mixtures of solvents, oils, paints, and pigments for the determination of the following elements: Ag, As, Ba, Cd, Cr, Hg, Ni, Pb, Sb, Se, and Tl.
1.3 This test method also may be applicable to elements not listed above and to the analysis of trace metals in organic liquids other than those used as LHWF.
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 and health practices and determine the applicability of regulatory limitations prior to use.
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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: D5839 − 15
Standard Test Method for
Trace Element Analysis of Hazardous Waste Fuel by
1
Energy-Dispersive X-Ray Fluorescence Spectrometry
This standard is issued under the fixed designation D5839; 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 dish is removed from the hot plate and allowed to cool.
Graphite powder is blended with the evaporated sample until a
1.1 This test method applies to the determination of trace
homogeneous paste is produced and the sample weight is
element concentrations by energy-dispersive X-ray fluores-
recorded. The blended sample is inserted in a disposable
cence(EDXRF)spectrometryintypicalliquidhazardouswaste
sample cup and placed in the X-ray spectrometer for analysis.
fuels (LHWF) used by industrial furnaces.
3.2 TheKSpectralX-rayemissionlinesareusedforAg,As,
1.2 This test method has been used successfully on numer-
Ba, Cd, Cr, Ni, Sb, and Se.
ous samples of LHWF that are mixtures of solvents, oils,
paints, and pigments for the determination of the following
3.3 The Lspectral X-ray emission lines are used for Hg, Pb,
elements: Ag, As, Ba, Cd, Cr, Hg, Ni, Pb, Sb, Se, and Tl.
and Tl.
1.3 This test method also may be applicable to elements not
4. Significance and Use
listed above and to the analysis of trace metals in organic
liquids other than those used as LHWF.
4.1 The analysis of trace elements is often a regulatory and
process specific requirement for facilities utilizing LHWF.
1.4 This standard does not purport to address all of the
With proper instrument standardization, set-up, and quality
safety concerns, if any, associated with its use. It is the
control, this test method provides the user an accurate, rapid,
responsibility of the user of this standard to establish appro-
nondestructive method for trace element determinations.
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use.
5. Interferences
2. Referenced Documents
5.1 Spectral Overlaps:
2
2.1 ASTM Standards:
5.1.1 Samples containing a mixture of elements often ex-
C982 Guide for Selecting Components for Energy-
hibit X-ray emission line overlap. Modern Si (Li) detectors
Dispersive X-Ray Fluorescence (XRF) Systems (With-
generally provide adequate resolution to minimize the effects
3
drawn 2008)
of spectrum overlaps on the analytical results of the LHWF. In
those cases where direct emission line overlap exists, spectral
3. Summary of Test Method
deconvolution methods extract corrected analyte emission line
3.1 A weighed portion of the sample is transferred to a intensities. Table 1 lists the significant line overlaps observed
for the elements analyzed in LHWF. Follow the EDXRF
porcelain evaporating dish and placed on a hot plate. The
sample is heated for 15 to 30 min at a temperature not manufacturer’s recommendations concerning spectral decon-
volution of the emission lines.
exceeding 105°C to evaporate highly volatile components.The
NOTE1—NotallpossibleinterferencesarelistedinTable1.TheLHWF
samples to be analyzed may have other emission line interferences not
1
This guide is under the jurisdiction of ASTM Committee D34 on Waste
mentioned. Consult the manufacturer’s recommendations for optimum
Management and is the direct responsibility of Subcommittee D34.01.06 on
deconvolution methods.
Analytical Methods.
Current edition approved May 1, 2015. Published May 2015. Originally 5.2 Matrix Interferences:
approved in 1996. Last previous edition approved in 2006 as D5839 - 96 (2006),
5.2.1 Large concentration variations of metal or matrix
which was withdrawn in January 2015 and reinstated in May 2015. DOI:
components, or both, in LHWF samples can result in non-
10.1520/D5839-15.
2
linear metal X-ray intensity response at increasing metal
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
concentrations. Untreated matrix interactions may have a
Standards volume information, refer to the standard’s Document Summary page on
deleterious effect on metal determination accuracy. Matrix
the ASTM website.
3
interactions, if exhibited by the LHWF samples, must be
The last approved version of this historical standard is referenced on
www.astm.org. accounted for by method calibration.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1
...
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: D5839 − 15
Standard Test Method for
Trace Element Analysis of Hazardous Waste Fuel by
1
Energy-Dispersive X-Ray Fluorescence Spectrometry
This standard is issued under the fixed designation D5839; 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 dish is removed from the hot plate and allowed to cool.
Graphite powder is blended with the evaporated sample until a
1.1 This test method applies to the determination of trace
homogeneous paste is produced and the sample weight is
element concentrations by energy-dispersive X-ray fluores-
recorded. The blended sample is inserted in a disposable
cence (EDXRF) spectrometry in typical liquid hazardous waste
sample cup and placed in the X-ray spectrometer for analysis.
fuels (LHWF) used by industrial furnaces.
3.2 The K Spectral X-ray emission lines are used for Ag, As,
1.2 This test method has been used successfully on numer-
Ba, Cd, Cr, Ni, Sb, and Se.
ous samples of LHWF that are mixtures of solvents, oils,
paints, and pigments for the determination of the following
3.3 The L spectral X-ray emission lines are used for Hg, Pb,
elements: Ag, As, Ba, Cd, Cr, Hg, Ni, Pb, Sb, Se, and Tl.
and Tl.
1.3 This test method also may be applicable to elements not
4. Significance and Use
listed above and to the analysis of trace metals in organic
liquids other than those used as LHWF.
4.1 The analysis of trace elements is often a regulatory and
process specific requirement for facilities utilizing LHWF.
1.4 This standard does not purport to address all of the
With proper instrument standardization, set-up, and quality
safety concerns, if any, associated with its use. It is the
control, this test method provides the user an accurate, rapid,
responsibility of the user of this standard to establish appro-
nondestructive method for trace element determinations.
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use.
5. Interferences
2. Referenced Documents
5.1 Spectral Overlaps:
2
2.1 ASTM Standards:
5.1.1 Samples containing a mixture of elements often ex-
C982 Guide for Selecting Components for Energy-
hibit X-ray emission line overlap. Modern Si (Li) detectors
Dispersive X-Ray Fluorescence (XRF) Systems (With-
generally provide adequate resolution to minimize the effects
3
drawn 2008)
of spectrum overlaps on the analytical results of the LHWF. In
those cases where direct emission line overlap exists, spectral
3. Summary of Test Method
deconvolution methods extract corrected analyte emission line
intensities. Table 1 lists the significant line overlaps observed
3.1 A weighed portion of the sample is transferred to a
porcelain evaporating dish and placed on a hot plate. The for the elements analyzed in LHWF. Follow the EDXRF
manufacturer’s recommendations concerning spectral decon-
sample is heated for 15 to 30 min at a temperature not
exceeding 105°C to evaporate highly volatile components. The volution of the emission lines.
NOTE 1—Not all possible interferences are listed in Table 1. The LHWF
samples to be analyzed may have other emission line interferences not
1
This guide is under the jurisdiction of ASTM Committee D34 on Waste
mentioned. Consult the manufacturer’s recommendations for optimum
Management and is the direct responsibility of Subcommittee D34.01.06 on
deconvolution methods.
Analytical Methods.
Current edition approved May 1, 2015. Published May 2015. Originally 5.2 Matrix Interferences:
approved in 1996. Last previous edition approved in 2006 as D5839 - 96 (2006),
5.2.1 Large concentration variations of metal or matrix
which was withdrawn in January 2015 and reinstated in May 2015. DOI:
components, or both, in LHWF samples can result in non-
10.1520/D5839-15.
2
linear metal X-ray intensity response at increasing metal
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
concentrations. Untreated matrix interactions may have a
Standards volume information, refer to the standard’s Document Summary page on
deleterious effect on metal determination accuracy. Matrix
the ASTM website.
3 interactions, if exhibited by the LHWF samples, must be
The last approved version of this historical standard is referenced on
www.astm.org. accounted for by method calibration.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1
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D5839 − 15
TABLE 1 Common Emission Line Spectral Interferences fo
...
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