Nuclear Instruments and Methods in Physics Research B 266 (2008) 4782–4787

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Nuclear Instruments and Methods in Physics Research B

journal homepage: www.elsevier.com/locate/nimb

PIXE as a complement to trace metal analysis of sediments by ICP-OES

J.M. Lunderberg, R.J. Bartlett, A.M. Behm, C. Contreras, P.A. DeYoung *, N.L. Hoogeveen,
A.J. Huisman, G.F. Peaslee, J.K. Postma
Department of Chemistry, Hope College, Holland, MI 49422-9000, United States
Department of Physics, Hope College, Holland, MI 49422-9000, United States

a r t i c l e i n f o a b s t r a c t

Article history: The adverse effects of metal contamination in sediments require methods that can quickly and accurately
Received 13 May 2008 assess the extent of environmental pollution. Particle induced X-ray emission spectrometry (PIXE) is
Received in revised form 18 July 2008 demonstrated to be a viable alternative to an established method, which consists of acid digestion and
Available online 29 July 2008
Inductively coupled plasma-optical emission spectrometry (ICP-OES) to measure trace metals in sedi-
ment. The analysis of trace metal composition by both techniques on a NIST Standard Reference Material
PACS: mud gives results that are consistent with the certified values for fourteen measured metals, seven of
29.30.Kv
which are common to both methods. A comparison study conducted on a sediment core from a freshwa-
79.20.Rf
81.70. q
ter lake with a known chromium contamination in Muskegon County, MI also shows a good correlation
82.80. d between the methods for transition metals of environmental interest over a wide range of metal concen-
82.80.Ej trations. Total sample preparation and analysis time for the PIXE measurements is roughly one third that
83.80.Nb of acid digestion and ICP-OES. Also, the acid digestion step does not elute all the metal, while the nonde-
structive PIXE approach is a total metals analysis method. However the PIXE method generally has higher
Keywords: limits of detection for many environmental metal contaminants. By combining the two techniques, the
ICP-OES acid digestion elution factor can be quantified by running PIXE on an original sample and on the residue
PIXE
resulting from acid digestion.
Sediment trace metal analysis
Ó 2008 Elsevier B.V. All rights reserved.
Nondestructive

1. Introduction amount of bio-available metal in the sediment (which can depend

A widely used method for the characterization of trace metal
concentrations in sediments is based on inductively coupled plas-
ma-optical emission spectrometry (ICP-OES) [1,2]. This method has
very low detection limits for most metals, but requires the diges-
tion of the sediment sample with strong acid [3–5]. Unfortunately,
this digestion process destroys the sample material and the frac-
tion of metal that the process extracts is dependant on the geolog-
ical matrix properties of each sample [6–8]. For example, chromate
ore contains Cr3+ oxides which are very resistant to acid digestions,
while Cr6+ oxides from anthropogenic sources are readily extracted
from acid digestion of sediments. This results in measured values
that can be significantly less than the actual total values for the
metal concentrations and which can vary greatly from metal to
metal even within a single sample. Additionally, the acid-soluble
fraction of each trace metal does not typically correspond to the
* Corresponding author. Address: Department of Physics, Hope College, Holland,
MI 49422-9000, United States. Tel.: +1 616 395 7517; fax: +1 616 395 7123.
E-mail address: deyoung@hope.edu (P.A. DeYoung).
additionally on temperature, pH and Eh, for example). One previ-
ous study that focused only on arsenic found that the amount of
extracted arsenic varies greatly with the acid used and the origin
of the sample [9]. Typically, acid digestion results are reported at
only one pH in order to be reproducible [10]. Thus the analytical
measurements by ICP-OES, while very precise, do not yield abso-
lute concentrations that can be used directly without careful inter-
pretation. Particle induced X-ray emission spectrometry (PIXE) has
acceptable detection limits for many transition metals, and it is
nondestructive. This is a significant advantage if the sample quan-
tities are small or difficult to obtain. The method we developed
here is also faster, a significant advantage if there are many sam-
ples to be processed. More importantly, once the efficiency of the
detector is calibrated, the PIXE approach yields metal concentra-
tions that are consistent from metal to metal and sample to sample
without separate dilutions for each metal type. Although PIXE has
been successfully applied to the analysis of sediments previously
[11–17], the target preparation methods described here and the
use of it as a complementary technique to ICP-OES for the two sed-
iments studied is novel.
Of course all analytical techniques also have disadvantages. In
the case of PIXE, the technique requires a source of energetic

0168-583X/$ - see front matter Ó 2008 Elsevier B.V. All rights reserved.
doi:10.1016/j.nimb.2008.07.025
 J.M. Lunderberg et al. / Nuclear Instruments and Methods in Physics Research B 266 (2008) 4782–4787
particles; typically from a small particle accelerator. Such devices
are typically more expensive than ICP-OES instruments, but for
those laboratories that already have ion beam capability, the addi-
tion of the sediment analysis methods described here can provide
another avenue to address quantitative trace metal analysis of sed-
iments. Another disadvantage of PIXE is that the detection limits,
while acceptable, are generally higher than those for ICP-OES.
There can be issues that skew results with PIXE if care is not
exercised. When one works with bulk material the preparation
and sample handling can result in skewed results. While true for
all analytical techniques, with PIXE only a subset (close to the sur-
face) of all the grains available in a sample are irradiated, which
may not accurately represent the bulk sample properties. As bulk
material is handled and either deliberately or unintentionally sha-
ken, the Brazil Nut Effect [18] can occur so that the resulting pellet
is inhomogeneous. Secondly, even avoiding this, it is easily possible
with modern beam focusing systems to achieve beam spots smal-
ler than 100 lm and such small beam spots can give skewed re-
sults if the beam is swept over a large area of the target. Lastly,
PIXE requires one to make an absolute determination of the inci-
dent particle flux for each measurement, to have an accurate deter-
mination of the any X-ray filters, and to understand the X-ray
detector efficiency well.
The work described below discusses the general normalization
of the PIXE method based on a National Institute of Standards
and Technology (NIST) reference standard and then examines
how well the PIXE method is able to reproduce a significant num-
ber of trace metals without individual corrections. Then, a compar-
ison of the results for sediments from a local lake from the PIXE
method and the ICP-OES method is presented. This comparison
shows excellent correlation between the two methods but high-
lights the problem of incomplete digestion in ICP-OES. By compar-
ing the published values of the standardized NIST SRM mud with
the summed values of ICP-OES analysis and PIXE analysis on the
resulting residue, an estimate of the fraction that eluted in the acid
digestion is possible. The use of these complementary trace ele-
ment techniques will be valuable for contaminated sediment
characterization.
2. Experimental detail
2.1. Sample material description
Two sets of sediments were analyzed by ICP-OES and PIXE in
this study. The first set of sediment samples was Trace Elements
in Soil NIST SRM 2586 [19]. This is a freeze-dried homogenized
sample with 26 known concentrations of trace elements and is cer-
tified by the National Institute of Standards and Technology (NIST).
The second set of samples was from sediment cores taken from
White Lake in Muskegon County, MI. Three 82-cm deep sediment
piston cores were obtained as part of an EPA study [20–22] and
subsequently sliced into 2-cm sections, freeze-dried, homogenized
by a mechanical shaker and stored for analysis by both PIXE and
ICP-OES. The environmental cores provided a second type of geo-
logical matrix and the extended depth provided samples with a
large range of metal concentrations. This lake was known to have
extensive historical contamination of the sediment due to chromic
acid spills from an adjacent tannery. Lastly, a set of material was
analyzed only with the PIXE approach. This material was the solid
residue remaining after acid digestion of a sample in preparation
for ICP-OES. An additional standard sediment, Buffalo River Mud
NIST SRM 2704 [23], was used as part of an absolute PIXE efficiency
calibration. All of these samples were very fine-grain sediments
and so were not expected to exhibit the Brazil Nut effect to any
great extent [18].
4783
2.2. PIXE measurements
For the PIXE measurements, solid soil targets were made from
0.5 g of loose sediment. The sediment was homogenized first by
shaking in sealed plastic vials for several minutes. This was to in-
sure that the surface measurements were representative of the
bulk volume. The homogenized sample was pressed into a self-
supporting target by 10,000 psi of pressure in a standard 1.0-cm
pellet press. For typical sediments, rich in clays and dry organic
material, no binding agent was necessary to make the target self-
supporting. In particularly sandy soils, up to 5% by weight of poly-
vinyl alcohol was added to make the targets self-supporting. The
targets were attached with a drop of cyanoacrylate glue to a thin
sheet of aluminized mylar in order to minimize charge collection
difficulties on these relatively insulating targets. The material
remaining after the acid digestion preparation for ICP measure-
ments was prepared in the same fashion. The target pellets were
placed in vacuum and irradiated with a 2.3 MeV proton beam with
an intensity of approximately 10 nA. The beam was produced at
the Hope Ion Beam Analysis Laboratory (HIBAL), with a 1.7 MV tan-
dem PelletronÒ accelerator. The target was irradiated with an ellip-
tical beam spot (1 mm by 2 mm) for 300 s. Typically, the
incident beam current was measured with a Faraday cup immedi-
ately before and after each sample run and was found not to vary
more than 10%. The X-rays emitted from the samples were de-
tected with a 10 mm diameter by 5.35 mm thick Si(Li) detector lo-
cated 135° from the incident beam. The entrance window of the
detector is a 0.025 mm beryllium foil. For each measurement two
runs were made, one where a 50 lm mylar filter was used to sup-
press back-scattered protons while allowing efficient counting of
elements such as Ca and a second with a 500 lm mylar filter used
to optimize the counting of the higher Z elements. There was no
ambiguity about the origin of the various X-ray lines in the spectra
but the energy calibration of the PIXE detector systems was still
regularly determined with a set of known metal foils. A typical
spectrum of the NIST SRM 2586 with the thick filter is shown in
Fig. 1.
In many measurements the size of the beam spot is only of sec-
ondary concern. However, here we note that a spot which irradi-
ates a significant area, relative to the average grain size, helps
insure that one does not bias the PIXE measurements by sampling
individual grains in the sediment sample that are not representa-
Ca Ti Cr Fe Cu Zn Pb
10000
1000
Counts
100
10
1
0 2 4 6 8 10 12 14
X_Ray Energy (keV)
Fig. 1. A typical X-ray spectrum from the irradiation of a pressed pellet of Trace
Elements in Soil NIST SRM 2586. Selected lines are identified. In this spectrum, a
500 lm mylar filter was placed between the target and detector to suppress the
yield from lighter elements.
4784 J.M. Lunderberg et al. / Nuclear Instruments and Methods in Physics Research B 266 (2008) 4782–4787

tive of the whole sample. For the NIST measurements, each day the
sample pellets were irradiated, a beam was directed to a different
spot. This, too, reduces any bias associated with residual inhomo-
geneity in the sample even though the sediments were fine-
grained.
In this study the absolute efficiency of the system was deter-
mined in order to extract absolute concentrations of the various
trace elements. To determine the absolute efficiency for the White
Lake sediment measurements two NIST standards were measured
along with the White Lake samples. The detector efficiency, solid
angle and filter parameters were adjusted to match the NIST stan-
dard values. Care was taken to insure that the NIST standards were
measured with the same experimental conditions. Generally, only
small variations (<10%) were observed from day-to-day. In cases
where a large deviation in the efficiency parameters was seen,
the samples were remeasured.
All recorded X-ray spectra were analyzed off-line with the
thick-target option in GUPIXWIN [24], a commercial PIXE analysis
program where the elemental concentrations are given in parts per
million relative to the mass of the geological matrix. In addition to
the concentration of particular trace element concentrations, it
also provides an estimate of the level-of-detection (LOD). For our
system, PIXE has a higher limit of detection than the ICP technique
for most metals. Table 1 shows the NIST values, typical PIXE and
ICP measurements of the NIST SRM and LOD’s for a variety of ele-
ments in the NIST standard.
For the PIXE measurements of the NIST 2586 standard, a nor-
malization of the detector size, detector geometry and filter prop-
erties was made and it was possible to reproduce all the trace
elements shown in Table 1 with a single normalization. (The en-
ergy dependance of the efficiency was based on the fitting pro-
gram’s model of attenuation in mylar and Be along with the
intrinsic efficiency of the Si(Li) detector. No additional energy-
dependant factors were needed.)
the acidic matrix and high concentrations of interferents: Fe, Al
and Ca, the method of standard additions, or internal standards,
was employed using three spikes of a multielemental ICP standard
solution (PlasmaCAL Trace Metals I). In addition, due to the limited
linear dynamic range of most ICP-OES systems, three different
dilution factors were used with each sample (1000, 10,000,
100,000). A PerkinElmer, Inc. Optima 4300 DV ICP-OES was used
for all measurements of the eluent and the analysis was done in
Excel. The elements analyzed included aluminum, cadmium, co-
balt, chromium, copper, iron, manganese, nickel, lead, vanadium
and zinc and the measured concentrations of the elements in solu-
tion were reported in lg/l. Using a standard mass of soil diluted to
a standard volume during the digestion allows the conversion from
elemental concentrations in the eluent (lg/l) as measured by ICP-
OES to elemental concentrations in the soil (lg/g). The wave-
lengths used for ICP-OES measurements are listed in Table 2. These
are the typical wavelengths used for analysis of samples with high
iron and aluminum contaminants. Note that in Table 1 that the
uncertainty in the ICP values and the LOD for the various elements
are the same. This is a result of the use of internal standards where
known amounts of the elements are added to the samples and a
regression is performed to find the intercept which corresponds
to no added standard. The uncertainty in this intercept is then
the uncertainty in the amount of material in the original sample.
This uncertainty is also an estimate of the LOD since samples with
actual amounts of a particular element would be considered to
contain a measurable amount only if the intercept was greater that
zero plus the uncertainty. Iron, because of its high concentration,
was measured directly, leaving it without an ICP-OES-associated
uncertainity or LOD.
Table 2
The ICP wavelengths used for the various measured elements

Element Wavelength (nm)

2.3. ICP-OES measurements
Al 308.215, 394.401
As 193.696
Split samples from the same NIST and sediment samples used in Co 228.616, 230.786
the PIXE analysis were digested using EPA method 3051A [4], Cr 205.560
microwave-assisted acid digestion of sediments, sludges, soils Cu 327.393
Fe 239.562
and oils. Then the eluents were analyzed using EPA method
Mn 294.92
200.7 [2] for ICP-OES. Approximately 0.5 ± .01 g of each sediment Ni 221.648, 231.604
sample was measured and then digested with 10 ml of concen- Pb 220.350
trated nitric acid (Trace Metal Grade 99.9% purity Fisher Chemical Zn 206.200
Co.) in a CEM MARS5 microwave-accelerated reaction system. The These are based on [25]. In the cases where multiple wavelengths are given, there
digested samples were centrifuged and the eluent was diluted to was not a single best wavelength and the ICP-OES results for the given wavelengths
50 ml using deionized water to create a stock solution. Due to were averaged.

Table 1
Both ICP-OES and PIXE values from a typical single measurement of the NIST 2586 sediment sample together with reported LOD’s

Element NIST PIXE PIXE ICP ICP

Concentration (ppm) Measured values (ppm) LOD (ppm) Measured values (ppm) LOD (ppm)
K 9760 ± 180 9830 ± 200 130
Ca 22,180 ± 540 22,020 ± 270 160
Ti 6050 ± 660 6670 ± 110 66
V 160 250 ± 53 130
Cr 301 ± 45 303 ± 35 47 142.7 ± 0.1 0.1
Cu 81 66 ± 10 10 51.6 ± 0.6 0.6
Fe 51,610 ± 890 51,200 ± 2000 37 25,900 ± 1400 5
Mn 1000 ± 18 904 ± 59 57 636.3 ± 0.2 0.2
Ni 75 71 ± 33 27 39.01 ± 0.02 0.02
Pb 432 ± 17 375 ± 41 40 251.65 ± 0.01 0.01
Zn 352 ± 16 340 ± 20 7 244.07 ± 0.01 0.01
Sr 84 ± 8 102 ± 20 21

The elements for which there is no information given for ICP-OES are elements measured by PIXE that were not included in the ICP-OES analysis protocol. Except for Fe the
uncertainty and LOD for the ICP-OES measurements are identical. More detail is given in the text. The error shown for ICP-OES measurements does not reflect variation due to
the acid digestion process, it only reflects the variation in the actual ICP-OES measurement of the eluent.
 J.M. Lunderberg et al. / Nuclear Instruments and Methods in Physics Research B 266 (2008) 4782–4787
3. Measurement results
3.1. Introduction
Below we detail the three phases of this study. First PIXE and
ICP-OES were compared for a NIST standard mud (Sections 3.2
and 3.3). PIXE gave measurements that were consistent with the
published values for all elements with a single normalization fac-
tor. ICP-OES gave measurements that were reproducible from
day-to-day but were smaller than the published NIST value of total
metal concentration for some elements. This is a result of incom-
plete elution where only a fraction of the total concentration of
the element was removed from the soil matrix during the micro-
wave-assisted acid digestion.
Second, the correlation between PIXE and ICP-OES results were
compared using a common sample taken from White Lake (Section
3.4). The concentration of two elements, manganese and chro-
mium varied greatly by depth within the White Lake cores. This
variance allowed us to check the correlation of the two techniques
for a typical lake sediment example.
Third, the concentration of elements in the digestate residue
remaining after ICP-OES digestion was measured by PIXE. The ori-
ginal ICP-OES values from the NIST standard were added to PIXE
values obtained from the residue (Section 3.5). The sum of these
two measurements were in good agreement with the published
NIST value for all elements.
In each case, one can see the tradeoffs between PIXE and ICP-
OES analysis. PIXE always measures higher levels of the metals in
agreement with standards or, in the case of the White Lake sam-
ples, closer to a total concentration value. However, PIXE generally
has larger error bars and higher LOD than ICP-OES.
3.2. PIXE measurements of NIST SRM 2568
Before each series of PIXE measurements of sediment samples,
at least one measurement of a NIST standard mud pellet (NIST SRM
2586) was done in order to check the general efficiency of the
detection system. This measurement was used for calibration but
during the course of multiple projects, a body of data on PIXE mea-
surements on the NIST samples was compiled and is shown in Fig.
2. A weighted average of 18 separate measurements on NIST SRM
2586 is shown along with the standard deviation of those mea-
800
x0.1
600
Concentration (ppm)
x0.01 x0.05 x0.5
400
x0.01
200
0
Fe Ca K Ti Mn Pb Zn Cr V Sr
Element
Fig. 2. NIST certified values and PIXE measurements of the concentration of various
elements in decreasing concentration in NIST SRM 2586. Fe, Ca, K, Ti, Mn have
relatively high concentrations and have been scaled by the noted factors for a better
comparison between elements. In each case, the PIXE values reproduce the certified
values well.
4785
surements. The standard deviation is given so the variability in
the measurements can be seen. This measurement on the NIST
standard was calibrated with a single normalization constant with
the highest concentration elements (Fe, Ca and K) dominating the
calibration. Concentrations of all elements aligned well over many
runs as seen in the figure even though the normalization was based
on iron, calcium and potassium.
3.3. ICP-OES measurements of NIST SRM 2568
For ICP-OES runs on the NIST standard, it was found that the
ICP-OES values for the concentrations of elements were a fraction
of the NIST published values for total metal concentration. The
fraction varied from 50% of the NIST value for chromium to
90% of the NIST value for zinc. The fraction of the NIST value
was consistent within elements over multiple runs as seen in Fig.
3. The concentration of metals in a sample that the ICP-OES gave
was based on the mass of soil digested as explained previously. It
is important to note that in this measurement, unlike in PIXE, there
was not a single correction factor as each element was measured
individually via an internal standard. The fraction of the NIST value
that the ICP measured varied widely between elements but the
measurements were consistent within each element. These varia-
tions are an effect of the soil matrix and the acid digestion process.
3.4. White Lake sediment
The White Lake samples had chromium concentrations that
varied by depth from 300 to 900 ppm and manganese concen-
trations that varied from 500 to 1800 ppm as measured by
ICP-OES. This variation in concentrations led to an excellent oppor-
tunity for a comparison between the PIXE and ICP-OES. The con-
centrations given by PIXE and ICP-OES at each depth for the
concentrations of Cr were plotted against each other and a linear
correlation was observed as seen in Fig. 4. The concentration of
Mn given by both methods were plotted in the same manner as
in Fig. 5. These regressions are not perfect, and the ICP has better
LOD’s but as this graph shows, PIXE is certainly able to accurately
quantify the concentrations of these elements in sediment. The
regression lines in both graphs had slopes of less than unity, which
is a result of incomplete elution of metals out of the sediment dur-
ing the acid digestion process. The two graphs had slightly differ-
ent slopes which indicates a different efficiency of the acid
digestion process for each element (Mn is more efficiently eluted
PIXE 800
NIST
ICP
600 NIST
Concentration (ppm)
x0.01 x0.5
400
200
Cu Ni
0
Fe Mn Pb Zn Cr Cu Ni
Element
Fig. 3. NIST certified values and ICP-OES measurements of the concentrations of
various elements in SRM 2586. Fe and Mn have relatively high concentrations and
have been scaled as in Fig. 2 for a better comparison.
4786 J.M. Lunderberg et al. / Nuclear Instruments and Methods in Physics Research B 266 (2008) 4782–4787

1400
1.5
ICP+PIXE on Residue

Fraction of Published NIST Value

1200
PIXE on Residue
Cr
ICP Concentration (ppm)

1000 ICP
1.0
800

600

0.5
400

200

0 0.0
0 200 400 600 800 1000 1200 1400 Fe Mn Pb Zn Cr Cu Ni

PIXE Concentration (ppm) Element

Fig. 4. The PIXE and ICP-OES values for the concentration of chromium in White Fig. 6. A comparison between the NIST SRM certified values (scaled to 1.0) and the
Lake sediment. Error bars for PIXE are those given by GUPIXWIN and the error bars sum of the ICP-OES values (on NIST sediment) and the PIXE values (on the NIST
for ICP-OES are one standard deviation about the mean of eighteen runs on NIST residue after acid digestion).
SRM 2586.

OES measurement is one standard deviation about the mean of

eighteen measurements on NIST 2586 and the uncertainity in the
2000 PIXE measurement is the uncertainty given by GUPIXWIN. As Fig.
6 shows, this technique of utilizing both PIXE and ICP-OES allows
Mn for an estimate of the elution factor for each element in the ICP-
ICP Concentration (ppm)

1500 OES method. It also validates the idea that an elution factor is
the root cause of the lowered ICP-OES measurements of elements
in the NIST standard. This reconstruction of the NIST value worked
1000 for all elements and was not dependent on the fraction of the NIST
concentration measured by ICP-OES.

500 4. Conclusion

PIXE has been shown to be a technique that can accurately

0 quantify the concentration of a range of elements of interest in sed-
0 500 1000 1500
PIXE Concentration (ppm)
Fig. 5. The PIXE and ICP-OES values for the concentration of manganese in White
Lake. Error bars for PIXE are those given by GUPIXWIN and the error bars for ICP-
OES are one standard deviation about the mean of eighteen runs on NIST SRM 2586.
than Cr for this sediment). Elements come out of the mud in differ-
ent proportions during the acid digestion process due to their dif-
ferent binding affinity to the soil matrix. This effect can also be
seen in Fig. 3 which shows that elements were measured by ICP-
OES at different fractions of the NIST value.
3.5. PIXE on ICP-OES residue
As seen above, the results of ICP-OES and PIXE correlated well
but did not give equivalent results because acid digestion does
not elute 100% of each metal in the sample. During the course of
the study, the acid digestate residues of multiple NIST SRM 2586
samples were retained. These samples were homogenized, pressed
into pellets and the metal concentrations were quantified by sub-
sequent PIXE analysis. The sum of the weighted averages of both
the ICP-OES results on the original NIST sample and the PIXE re-
sults on the ICP-OES digestate residue were compared to the pub-
lished NIST value for the concentration of each element in Fig. 6.
This figure gives the ICP-OES measurement on the NIST sample,
the PIXE measurement on the ICP-OES residue and the sum of
the two measurements as fractions of the published NIST value
for the concentration of the element. The uncertainty in the ICP-
2000 iment. It correlates well to standard ICP-OES measurements of the
same sediment and has the advantage of having both faster sample
preparation than ICP-OES and having a nondestructive sample
preparation. Disadvantages associated with the PIXE technique
are that it has a lower sensitivity for most metals and the range
of elements it can analyze is more limited. Of course, one must
realize that PIXE has higher LOD than ICP-OES and requires a par-
ticle accelerator that is a scarcer and more complicated device.
There are several situations where PIXE could play an important
role in trace element measurement of contaminated sediment. In
the event of large numbers of sediment samples needing rapid
quantification of metal concentrations, PIXE certainly could be
used in conjunction with ICP-OES. Even though PIXE has a lower
sensitivity, sample preparation consists merely of drying the sedi-
ment, homogenizing the mud and pressing it into a pellet. This has
the obvious advantages that the measurements and analysis could
be done faster and since the samples would not be destroyed, addi-
tional high precision testing could be done when needed. Similarly,
small or one-of-a-kind sediment samples would not be destroyed
and would be retained for additional testing.
In addition to being used as a preliminary scan measure, PIXE
can also be used as a complement to ICP-OES. PIXE could be used
on both a soil and its post-digestion residue in order to better
understand the elemental elution factors of a particular soil matrix.
The information on elemental elution factors in a given soil sample
could then be used to scale ICP-OES results to absolute values of
the concentrations of elements. This would allow for a better inter-
comparison of results from different soil matrices. Further studies
on this possibility are underway.
 J.M. Lunderberg et al. / Nuclear Instruments and Methods in Physics Research B 266 (2008) 4782–4787
Acknowledgements
The authors with to thank Dave Daugherty for his commitment
to successful operation of the accelerator. This work was funded
through support from the National Science Foundation under
Grants MRI-0319523, MRI-01166264 and RUI:PHY-0354920.
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