ASTM D5839-15(2023)
(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, 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.
General Information
Relations
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: D5839 − 15 (Reapproved 2023)
Standard Test Method for
Trace Element Analysis of Hazardous Waste Fuel by
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 3. Summary of Test Method
3.1 A weighed portion of the sample is transferred to a
1.1 This test method applies to the determination of trace
element concentrations by energy-dispersive X-ray fluores- porcelain evaporating dish and placed on a hot plate. The
sample is heated for 15 to 30 min at a temperature not
cence (EDXRF) spectrometry in typical liquid hazardous waste
fuels (LHWF) used by industrial furnaces. exceeding 105 °C to evaporate highly volatile components.
The dish is removed from the hot plate and allowed to cool.
1.2 This test method has been used successfully on numer-
Graphite powder is blended with the evaporated sample until a
ous samples of LHWF that are mixtures of solvents, oils,
homogeneous paste is produced and the sample weight is
paints, and pigments for the determination of the following
recorded. The blended sample is inserted in a disposable
elements: Ag, As, Ba, Cd, Cr, Hg, Ni, Pb, Sb, Se, and Tl.
sample cup and placed in the X-ray spectrometer for analysis.
1.3 This test method also may be applicable to elements not
3.2 The K spectral X-ray emission lines are used for Ag, As,
listed above and to the analysis of trace metals in organic
Ba, Cd, Cr, Ni, Sb, and Se.
liquids other than those used as LHWF.
3.3 The L spectral X-ray emission lines are used for Hg, Pb,
1.4 This standard does not purport to address all of the
and Tl.
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro-
4. Significance and Use
priate safety, health, and environmental practices and deter-
mine the applicability of regulatory limitations prior to use. 4.1 The analysis of trace elements is often a regulatory and
process-specific requirement for facilities utilizing LHWF.
1.5 This international standard was developed in accor-
With proper instrument standardization, set-up, and quality
dance with internationally recognized principles on standard-
control, this test method provides the user an accurate, rapid,
ization established in the Decision on Principles for the
nondestructive method for trace element determinations.
Development of International Standards, Guides and Recom-
mendations issued by the World Trade Organization Technical
5. Interferences
Barriers to Trade (TBT) Committee.
5.1 Spectral Overlaps:
2. Referenced Documents
5.1.1 Samples containing a mixture of elements often ex-
hibit X-ray emission line overlap. Modern Si (Li) detectors
2.1 ASTM Standards:
generally provide adequate resolution to minimize the effects
C982 Guide for Selecting Components for Energy-
of spectrum overlaps on the analytical results of the LHWF. In
Dispersive X-Ray Fluorescence (XRF) Systems (With-
those cases where direct emission line overlap exists, spectral
drawn 2008)
deconvolution methods extract corrected analyte emission line
intensities. Table 1 lists the significant line overlaps observed
for the elements analyzed in LHWF. Follow the EDXRF
This test method is under the jurisdiction of ASTM Committee D34 on Waste
manufacturer’s recommendations concerning spectral decon-
Management and is the direct responsibility of Subcommittee D34.01.06 on
volution of the emission lines.
Analytical Methods.
Current edition approved Nov. 1, 2023. Published November 2023. Originally
NOTE 1—Not all possible interferences are listed in Table 1. The LHWF
approved in 1996. Last previous edition approved in 2015 as D5839 – 15. DOI:
samples to be analyzed may have other emission line interferences not
10.1520/D5839-15R23.
2 mentioned. Consult the manufacturer’s recommendations for optimum
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
deconvolution methods.
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Standards volume information, refer to the standard’s Document Summary page on
5.2 Matrix Interferences:
the ASTM website.
5.2.1 Large concentration variations of metal or matrix
The last approved version of this historical standard is referenced on
www.astm.org. components, or both, in LHWF samples can result in nonlinear
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D5839 − 15 (2023)
TABLE 1 Common Emission Line Spectral Interferences for
7.5 Use paraffinic base oil.
LHWF Analysis
7.6 Use sample cups, vented or unvented.
Lines
Element Spectral Interferences
Determined
7.7 Use thin-film sample support.
As Kα, Kβ Pb Lα, Hg Lβ, Tl Lα Lβ
NOTE 2—The user should select a thin-film support that provides for
Cr Kα, Kβ V Kβ, Mn Kα
maximum transmittance and is resistant to typical components in LHWF.
Hg Lα, Lβ As Kβ, Se Kα, Pb Lβ, Tl Lα, Br Kα
Ni Kα, Kβ Cu Kβ, Cu Kα The thin-film supports used in the development of this test method were
Pb Lα, Lβ As Kα, Se Kβ Hg Lβ Tl Lα, Tl Lβ, Br Kα, Br Kβ 4 μm Prolene.
Se Kα, Kβ Pb Lβ, Hg Lβ, Tl Lβ
Tl Lα, Lβ As Kα, As Kβ, Se Kβ, Pb Lα, Br Kα, Hg Lα, Hg Lβ
8. Sampling
8.1 Because stratification or layering of liquid samples is
possible, the laboratory sample should be thoroughly mixed by
metal X-ray intensity response at increasing metal concentra-
shaking prior to withdrawing a portion for testing, or use a
tions. Untreated matrix interactions may have a deleterious
sampling method that ensures all portions of the sample are
effect on metal determination accuracy. Matrix interactions, if
represented.
exhibited by the LHWF samples, must be accounted for by
method calibration.
9. Preparation of Apparatus
9.1 Follow the manufacturer’s instructions for set-up,
6. Apparatus
conditioning, preparation, and maintenance of the XRF spec-
6.1 Energy Dispersive X-Ray Spectrometer, capable of mea-
trometer.
suring the wavelengths listed in Table 1. Refer to Guide C982
9.2 Obtain reference spectra from pure element standards
for system specifications.
for all analytes and interelement correction metals.
6.2 Hot Plate, with temperature control to 105 °C.
9.3 Address spectral interferences, as listed in 5.1.1, in
6.3 Analytical Balance, capable of weighing to 0.001 g.
accordance with manufacturer’s recommendations.
6.4 Porcelain Evaporating Dishes, 70 to 150 mL capacity.
10. Calibration and Standardization
7. Reagents and Materials
10.1 Calibrate the spectrometer to an appropriate reference
element at the minimum frequency specified by the manufac-
7.1 Purity of Reagents—Use reagent grade chemicals in all
turer.
tests. Unless otherwise indicated, all reagents will conform to
the specifications of the Committee on Analytical Reagents of
10.2 Analytical standards should be gravimetrically pre-
the American Chemical Society where such specifications are
pared by blending the elemental standards and graphite listed
available. Other grades may be used, provided it is first
in Section 7. These preparations can contain single or multiple
ascertained that the reagent is of sufficient high purity to permit
elements and should be prepared at combinations and ratios to
its use without lessening the accuracy of the determination.
meet the user’s individual needs. For example, a Pb and Cd
standard at 125 ppm each could be prepared by gravimetrically
7.2 Use graphite powder, mixing grade, 44 μm, 325 mesh.
combining 2 g oil-based Pb standard (500 ppm), 2 g oil-based
7.3 Use oil-based Ag, As, Ba, Cd, Cr, Hg, Ni, Pb, Sb, and Se
Cd standard (500 ppm), and 4 g graphite and blending to a
standards, 10 to 10 000 mg/kg depending on the user’s
homogeneous mixture. For this example, the Pb concentration
analytical requirements. If the results of this test method are to
is calculated as follows:
be used for compliance purposes, standards or a commercial
Pb Standard Concentration 5 500 ppm (1)
source must be traceable to NIST or other certifying body.
Quality control samples for analyses done for compliance
Pb Std. ~g!
×
purposes may need to be prepared with standards from a
graphite ~g!1Cd Std. ~g!1Pb Std. ~g!
different vendor or lot number.
10.3 The metals standard/graphite paste is placed in an XRF
7.4 Use oil or solvent-based Tl standard, 10 to 1000 mg/kg
sample cup and affixed with a thin-film support. The sample
depending on the user’s analytical requirements. If the results
cup is inverted and lightly tapped on a level surface until the
of this test method are to be used for compliance purposes,
blended paste makes full contact (no air spaces) with the
standards or a commercial source must be traceable to NIST or
thin-film support.
other certifying bod
...
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