ASTM D5839-96(2006)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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 − 96(Reapproved 2006)
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 Graphite powder is blended with the evaporated sample until a
homogeneous paste is produced and the sample weight is
1.1 This test method applies to the determination of trace
recorded. The blended sample is inserted in a disposable
element concentrations by energy-dispersive X-ray fluores-
sample cup and placed in the X-ray spectrometer for analysis.
cence(EDXRF)spectrometryintypicalliquidhazardouswaste
fuels (LHWF) used by industrial furnaces.
3.2 TheKSpectralX-rayemissionlinesareusedforAg,As,
Ba, Cd, Cr, Ni, Sb, and Se.
1.2 This test method has been used successfully on numer-
ous samples of LHWF that are mixtures of solvents, oils,
3.3 The Lspectral X-ray emission lines are used for Hg, Pb,
paints, and pigments for the determination of the following
and Tl.
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 4. Significance and Use
listed above and to the analysis of trace metals in organic
4.1 The analysis of trace elements is often a regulatory and
liquids other than those used as LHWF.
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:
5.1.1 Samples containing a mixture of elements often ex-
2.1 ASTM Standards:
hibit X-ray emission line overlap. Modern Si (Li) detectors
C982 Guide for Selecting Components for Energy-
generally provide adequate resolution to minimize the effects
Dispersive X-Ray Fluorescence (XRF) Systems (With-
of spectrum overlaps on the analytical results of the LHWF. In
drawn 2008)
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
for the elements analyzed in LHWF. Follow the EDXRF
porcelain evaporating dish and placed on a hot plate. The
manufacturer’s recommendations concerning spectral decon-
sample is heated for 15 to 30 min at a temperature not
volution of the emission lines.
exceeding 105°C to evaporate highly volatile components.The
dish is removed from the hot plate and allowed to cool.
NOTE1—NotallpossibleinterferencesarelistedinTable1.TheLHWF
samples to be analyzed may have other emission line interferences not
mentioned. Consult the manufacturer’s recommendations for optimum
This guide is under the jurisdiction of ASTM Committee D34 on Waste
deconvolution methods.
Management and is the direct responsibility of Subcommittee D34.01.06 on
5.2 Matrix Interferences:
Analytical Methods.
Current edition approved Feb. 1, 2006. Published March 2006. Originally
5.2.1 Large concentration variations of metal or matrix
approved in 1996. Last previous edition approved in 2001 as D5839 - 96(2001)
components, or both, in LHWF samples can result in non-
DOI: 10.1520/D5839-96R06.
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.
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
D5839 − 96 (2006)
TABLE 1 Common Emission Line Spectral Interferences for NOTE 2—The user should select a thin-film support that provides for
LHWF Analysis
maximum transmittance and is resistant to typical components in LHWF.
The thin-film supports used in the development of this test method were
Lines
Element Spectral Interferences
4 µm Prolene.
Determined
As Kα,Kβ Pb Lα,HgLβ,TlLα Lβ
Cr Kα,Kβ VKβ,MnKα 8. Sampling
Hg Lα,Lβ As Kβ,SeKα,PbLβ,TlLα,BrKα
8.1 Because stratification or layering of liquid samples is
Ni Kα,Kβ Cu Kβ,CuKα
Pb Lα,Lβ As Kα,SeKβ Hg Lβ Tl Lα,TlLβ,BrKα,BrKβ
possible, the laboratory sample should be thoroughly mixed by
Se Kα,Kβ Pb Lβ,HgLβ,TlLβ
shaking prior to withdrawing a portion for testing, or use a
Tl Lα,Lβ As Kα,AsKβ,SeKβ,PbLα,BrKα,HgLα,HgLβ
sampling method that assures all portions of the sample are
represented.
9. Preparation of Apparatus
6. Apparatus
9.1 Follow the manufacturer’s instructions for set-up,
6.1 Energy Dispersive X-Ray Spectrometer, capable of mea-
conditioning, preparation, and maintenance of the XRF spec-
suring the wavelengths listed in Table 1. Refer to C982 for
trometer.
system specifications.
9.2 Obtain reference spectra from pure element standards
6.2 Hot Plate, with temperature control to 105°C.
for all analytes and interelement correction metals.
6.3 Analytical Balance, capable of weighing to 0.001 g.
9.3 Address spectral interferences, as listed in 5.1.1,in
6.4 Porcelain Evaporating Dishes, 70 to 150 mL capacity.
accordance with manufacturer’s recommendations.
7. Reagents and Materials
10. Calibration and Standardization
7.1 Purity of Reagents—Use reagent grade chemicals in all
10.1 Calibrate the spectrometer to an appropriate reference
tests. Unless otherwise indicated, all reagents will conform to
element at the minimum frequency specified by the manufac-
the specifications of the Committee on Analytical Reagents of
turer.
the American Chemical Society where such specifications are
10.2 Analytical standards should be gravimetrically pre-
available. Other grades may be used, provided it is first
pared by blending the elemental standards and graphite listed
ascertainedthatthereagentisofsufficienthighpuritytopermit
in Section 7. These preparations can contain single or multiple
its use without lessening the accuracy of the determination.
elements and should be prepared at combinations and ratios to
7.2 Use graphite powder, mixing grade, 44 µm, 325 mesh.
meet the user’s individual needs. For example, a Pb and Cd
7.3 Use oil-basedAg,As, Ba, Cd, Cr, Hg, Ni, Pb, Sb and Se
standard at 125 ppm each could be prepared by gravimetrically
standards, 10 to 10 000 mg/kg depending on the user’s combining 2 g oil-based Pb standard (500 ppm), 2 g oil-based
analytical requirements. If the results of this test method are to
Cd standard (500 ppm) and 4 g graphite and blending to a
be used for compliance purposes, standards or a commercial homogeneous mixture. For this example, the Pb concentration
source must be traceable to NIST or other certifying body.
is calculated as follows:
Quality control samples for analyses done for compliance
Pb Standard Concentration 5 500 ppm
purposes may need to be prepared with standards from a
Pb Std. ~g!
different vendor or lot number.
graphite g 1Cd Std. g 1Pb Std. g
~ ! ~ ! ~ !
7.4 Use oil or solvent-based Tl standard, 10 to 1000 mg/kg
(1)
depending on the user’s analytical requirements. If the results
10.3 Themetalsstandard/graphitepasteisplacedinanXRF
of this test method are to be used for compliance purposes,
sample cup and affixed with a thin-film support. The sample
standards or a commercial source must be traceable to NISTor
6 cup is inverted and lightly tapped on a level surface until the
other certifying body.
blended paste makes full contact (no air spaces) with the
7.5 Use paraffinic base oil.
thin-film support.
7.6 Use sample cups, vented or unvented. 10.3.1 The standard blends in the sample cups are placed
into the spectrometer’s designated sample holder.Avoid touch-
7.7 Use thin-film sample support.
ing the thin-film, as this can further reduce transmittance.
Initiate data acquisition for the desired elements ac
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