EPSILON 5

Leading the way in heavy metals analysis

Analytical excellence
Advantages of XRF spectroscopy
• Non-destructive method
• Suitable for use with solid, liquid or powdered samples
• Simple, fast and safe sample preparation
• Highly accurate and reproducible measurements
• Wide dynamic concentration range
Elemental analysis by X-ray fluorescence
spectroscopy (XRF) is a well-proven
technique that is applied in diverse
industries. These include metal, cement,
oil, polymer, plastic, food, mining,
mineralogy, geology, environmental and
waste materials. Simple sample
preparation, non-destructive analysis,
accuracy, precision, a wide dynamic
range and good to excellent detection
limits across large parts of the periodic
table are the principal reasons behind its
widespread use in numerous research
and industrial applications. Modern
systems are also easy to operate, highly
reliable, safe and cost-effective.
As system characteristics continue to be
refined and analytical performance is
enhanced, it is not surprising that XRF is
becoming an indispensable analytical
tool.
 About X-ray
fluorescence
spectroscopy

Incorporating five patented

technologies, the Epsilon 5 out
performs its rivals in medium to
heavy metals analysis

The Epsilon 5
Spectrometer

Leading the way

• 3-dimensional polarizing optics
improving detection limits by
reducing spectral background
• 100 kV Gd or Sc/W-anode X-ray
tube enhancing the excitation of
heavy element K-lines
A culture of innovation and quality has
made PANalytical the world’s leading
supplier of analytical X-ray
instrumentation. Formerly Philips
Analytical, the company has more than
En
INF

erg
half a century of experience in this RA

• 100% efficient Ge detector y

RE

dynamic field.
D

ensuring high detection

VIS
IBL

efficiency across the periodic Central to PANalytical’s business

E
LIG

table
HT

philosophy is a determination that its

• 15 polarization/secondary products and services should increase
UL LET
VIO

0.1
TR

targets allowing optimization of the efficiency of customer processes.

A
25

the excitation source according

keV YS
X-R

And this was a driving force behind the

A

125

to the elements of interest introduction of the Epsilon 5.

keV YS
γ -R

• X-Y sample changer

A

ensuring flexible, unattended The Epsilon 5

handling of up to 130 samples in
six trays.
Epsilon 5 Alternative Fuels
A dedicated, pre-calibrated system
for the analysis of solid alternative
fuels.
The calibration is set up using a
series of certified reference
materials (CRM).
Accurate matrix correction allows
the calibration to be used for a
wide range of solid alternative fuel
materials.
A fully integrated hardware and ICP - OES XRF γ-SPEC
software system, the Epsilon 5 has been
designed for optimal performance
across the periodic table. With the
Unlike many other analytical techniques
incorporation of five patented
XRF spectroscopy does not involve sample
technologies, it sets the standard for dissolution. By avoiding the potential for
quality and performance in XRF analysis. inaccuracies caused by incomplete
dissolution, the complete analysis offered
by XRF helps ensure the accuracy and
Characterized by highly precise,
reliability of results.
sub-ppm determinations, the Epsilon 5
out performs its rivals in medium to
heavy metals analysis, targeting a wide
range of elements, many of
environmental significance.
An essential tool Geology
Recycling
RoHS WEEE
Environmental
Alternative Fuels
The Epsilon 5 combines all the benefits
of traditional XRF with greatly improved
performance for the analysis of medium
to heavy metals. As a result, it supports
a wide range of applications in areas
such as: geology, agriculture, use of
fossil and secondary fuels, industrial
emissions monitoring, recycling, catalyst
production, and the manufacture or
disposal of electronics and electrical
appliances in line with RoHS and WEEE
directives.

The measurement of low-levels of toxic

elements, notably heavy metals, is
particularly important in environmental
applications. Global concern over the
environment and the impact of industry
and consumerism continues to grow.
And meanwhile, legislation governing
the use, and the release into the
environment, of toxic heavy metals is
being significantly tightened. The legal
implications are widespread, requiring
the analysis of highly diverse material
types and widely varying concentrations
of elements.

This diversity of sample type and

measurement range is accommodated
easily by the Epsilon 5. Solid pieces,
pressed powders, loose powders and
granules, liquids, thin-films or filters can
all be placed directly into the
instrument. Calibrations cover wide
concentration ranges (sub-ppm to
100%) and the software’s Auto Quantify
routine enables the handling of many
different sample types and physical
forms with a single calibration. Prior
knowledge of the sample chemistry is
therefore not required.
 State of the art EDXRF
About XRF spectrometers
The basic configuration for all
spectrometers is a source, a sample and
a detection system. The production of
useful information depends on
separation or dispersion of the spectrum
of radiation coming from the sample so
that the characteristic X-rays can be
identified and counted. This is done in
two different ways:
• wavelength dispersive XRF (WDXRF)
employs a crystal to disperse the
spectrum
• energy dispersive XRF (EDXRF) directly
determines the energies of different
X-rays in the spectrum.
Polarising EDXRF
With a three-dimensional, or Cartesian,
geometry the X-ray tube spectrum is
eliminated by polarization. The
resultant reduction in spectral
background makes it possible for much
lower detection limits to be achieved.
The use of different polarizing targets,
placed along the first axis of the optical
path employing a three-dimensional
geometry, offers further analytical
advantages. Whereas some target
materials merely scatter the X-ray tube
irradiation onto the sample, other
materials fluoresce, yielding intense,
almost monochromatic X-rays that
irradiate the sample. By using targets of
different materials it is possible to
optimize the excitation source
specifically for elements of interest.
Simple EDXRF
Simple EDXRF spectrometers employ a Sample
two-dimensional, or direct excitation,
geometry where the X-ray tube
irradiating the sample and the detector
recording the spectrum, lie in the same
plane. While this offers very efficient
excitation of the sample, the recorded
spectrum not only contains the sample Source
spectrum, but also a large amount of
the scattered X-ray tube spectrum. This
contributes to relatively high
background levels and negatively Detector
influences the detection limits
achievable.
I(cps/ch)
4 5 5 7 8
Energy (keV)
2-dimensional optics
The primary beam (yellow) from the
I(cps/ch)
X-ray tube irradiates a polarizing target
placed along the first axis. After
scattering at 90° the X-rays travel along
the second axis (blue) to the sample. The 4 5
Energy (keV)
6 7 8
spectrum of the sample is recorded by a 3-dimensional optics
detector placed along the third axis
(purple).
 Customer Benefits

K-Ka 1 Ca-K a 1
Mn-Ka 1
Fe-K a 1
Epsilon 5 is able to overcome these
problems and make K-line analysis of
Cr-K b1
heavy elements a reality. This, in turn,
I(cps/ch)

Ca-K b1 Ti-Kb1
results in superior spectral resolution
and lower detection limits.
V-Ka 1 V-Kb1
Ti-Ka 1
La-L b1 Cr-K a 1
La-L a 2 Pr-L a 2 Ce-L b1 Pr-L b1
Ba-L a 2 Ce-L a 2 Nd-La 2 Nd-Lb1
Ba-L a 1 Ce-L a 1 Nd-La 1 Sm-L a 2
Pr-L a 1 Sm-L b1
La-L a 1 Sm-L a 1

4 5 6
Non-destructive analysis
Energy (keV)
The Epsilon 5’s combination of low
Ce-K a 1
power (600 W) and three-dimensional
La-Ka1
optics causes very low sample heating or
X-ray damage. Samples are therefore
I(cps/ch)

Ce-K b1
Ce-K a 2

Ba-K a 1
La-K a 2

Pr-K a 2 Ba-K b1 Nd-Ka 1

La-K b1
Sm-K a 2
unaffected by analysis, and even
Pr-K a 1 Nd-Ka 2

Analytical flexibility Ba-K a 2

The Epsilon 5 can be ‘tuned’ using a set
of programmable polarizing and
secondary targets to get the lowest
detection limits for a large number of
elements. Such ‘tuning’ makes X-ray
tube changes for optimum performance
a thing of the past.
delicate foils and filters can be
30 32 34 36 38
measured repeatedly over significant
Energy (keV) periods of time.
Improved low-level determination Precision
of heavy elements The Epsilon 5 capitalizes on the inherent
Traditionally in XRF heavy elements are precision of XRF. Because calibrations
analyzed using their L-series spectral can be maintained for many months,
lines. This is because of restrictions the continual short-period re-
imposed on the use of K-lines by calibrations, associated with other
inadequate excitation voltages, sub- instrument techniques, are unnecessary.
optimal detector efficiency and, in the
case of WDXRF, poor dispersion. The
main problem with the use of L-lines is
their position in crowded parts of the
spectrum, commonly overlapped by the
lines of major elements. They also have
relatively low sensitivities – again
resulting in higher detection limits. By
combining high excitation voltages with
a superior solid-state detector, the
 Customer Benefits

Safety first
The Epsilon 5 surpasses the most
stringent X-ray radiation safety
requirements. The heavily shielded
analysis chamber is machined from a
solid block of brass weighing almost
40 kg. Combined with double safety
interlocks, it ensures safe operation at
all times and avoids the need for
external X-ray monitoring.

No compromise on sample handling

An easily accessible, fully integrated X-Y
sample changer ensures flexible,
unattended sample handling. Solids,
liquids or filters can be loaded and/or
measured in any order.

Compact and mobile

The Epsilon 5 has few laboratory
support requirements. It can be
powered from a standard wall outlet
and does not require the external
chilling devices common to other
high-power XRF instruments. Complete
with robust wheels for mobility, the
Epsilon 5’s compact design requires little
laboratory floor space (84 x 75 cm).
 System Features

Ba
Ce
Nd
100kV
La
Sn Sb
I(cps/ch)

I
70kV

50kV

24 27 30 34 37 40
Energy (keV)

High-voltage Gd or Sc/W X-ray tube (1) Targets (3)

Operating at a maximum power of Up to 15 targets (a combination of
600 W and voltages between 25 kV and 100 kV, polarizing and secondary fluorescence)
PANalytical’s patented X-ray tubes are unique can be used. The basic system is
among EDXRF spectrometers. The characteristic configured with nine targets to provide
tube lines of the Gd-anode enhance the comprehensive coverage of the periodic
fluorescence of elements in the range of rhodium table. The additional six target positions
to barium, while the Sc tube lines of the Sc/W tube can be configured when optimum
enhance the fluorescence of lighter elements. The excitation conditions are required for
tube’s 100 kV capability has advantages for the the lowest possible detection limits in
excitation of heavy element K-lines. specific applications. A large choice of
additional target materials is available.

Optical path (2)

Three-dimensional geometry, with proprietary
anti-scatter technology, ensures a high degree of
polarization, such that even the very intense
spectral lines used to excite the sample are
removed completely from the measured spectrum.

Stability
The Epsilon 5 benefits from decades of
PANalytical experience in the
2590 development of WDXRF spectrometers
– systems that are renowned for their
excellent stability. Its robust
2585
construction, precisely made mechanics
I(cps/mA)

and closely controlled cabinet

2580 temperatures (35 ±1.0 ºC) provide
CSE = 0.045% outstanding stability.
RMS = 0.054%

2575
DAY 1 DAY 2 DAY 3 DAY 4
 1
2

1.2
X-ray detectors (4)
Ge (5mm)
The PAN-32 liquid nitrogen-cooled
1.0
solid-state Ge detector is characterized
0.8 Si(Li) (3mm) by a high degree of detection efficiency
Relative Efficiency

0.6 across the periodic table. Unlike other

Si-drift (0.3mm) common solid-state detectors, it
0.4
maintains 100% efficiency for heavy
0.2
element K-lines – a perfect match for
0
0 5 10 15 20 25 30 35 40 45 50
the Epsilon 5’s high-voltage excitation
Energy (keV)
source.
LiF200 (Fine Collimator)

The PAN-32 detector demonstrates

Ba
superior spectral resolution at high
Cs
energies compared to that obtained in
WDXRF using dispersion crystals.
Intensity

Ge Solid-State Detector

0 30 32 34 36
Energy (keV)

1.00

0.90
Full Width at Half Maximum (keV)

0.80
LiF200 (Fine collimator)
0.70

0.60

0.50

0.40

0.30 Ge solid-state detector

0.20

0.10

0.00
0 10 20 30 40
Energy (keV)
 7

Automatic current regulation (5)

Different sample types have variable
8
spectrum characteristics making it 5
difficult to predict optimum power
settings. The linearity of the Epsilon 5
generator helps maintain optimum
sample throughput by allowing
regulation of the X-ray tube current 6
from sample to sample.

Counting electronics (6)

High channel resolution across the 100
keV spectrum range is achieved with
state-of-the-art counting electronics
consisting of a multi-channel analyzer
(MCA), with digital signal processing,
capable of handling more than 16,000
channels.

9
 System Features

X-Y sample changer (7) Mobility and accessibility (9)

The changer can accommodate up to six Mounted on wheels, the Epsilon 5 is
sample trays. Different trays are easily manoeuvred in confined
available for sample holders, steel rings laboratory spaces. Removable panels on
and unmounted samples with diameters all sides of the instrument allow
of 25, 32, 41 and 50 mm. Total capacity unrestricted access for maintenance.
depends on sample size: trays for sample
holders or steel rings can hold eight
samples; trays for 25 mm diameter
unmounted samples can hold 21. There
is no restriction on the mix of the type
10 of samples present on the changer. The
changer recognizes the difference
between solid and liquid holders,
thereby protecting the instrument
against accidental loading of liquids
when under vacuum. Smart loading
automatically sorts liquid and solid
application measurements, enhancing
stability by minimizing the number of
changes of the analysis medium. External connections
The Epsilon 5 is powered from a
Loading time is reduced by direct standard wall socket (eg 230 V, 13 A)
loading/unloading of the unmounted and is connected to the PC via USB and
samples to a cup in the measurement UTP ports. External cooling water is not
position. necessary.

A priority loading position allows Liquid nitrogen level sensing (10)

immediate loading and analysis of
urgent samples in preference to routine
sample handling.
Gas purge system (8)
An optional helium or nitrogen gas
purge can be used for the analysis of
liquids and fine, loose powders.
Changeover of the analysis medium can
be carried out in under three minutes.
Level sensors monitor the liquid
nitrogen supply necessary for the
PAN-32 detector. An indication to refill
the nitrogen dewar is given four days in
advance, providing ample notification
even in the event of long weekends!
Fail-safe circuits prevent any damage to
the instrument should liquid nitrogen
be unavailable.
 Fully integrated
software
State-of-the-art
A comparison of calculated versus certified
concentrations for different reference materials
(eg. coal, plastic and steel) demonstrates the
analyzing power of the Auto Quantify routine.
Fly-Ash (NBS1633a)
Element Certified Auto Quantify
(ppm) (ppm)
Nickel 127 129
Copper 118 130
Zinc 220 231
Arsenic 145 156
Rubidium 131 137
Strontium 830 829
Zirconium 310 314
Barium 1500 1460
Plastic (BCR680)
Element Certified Auto Quantify
(ppm) (ppm)
Chromium 114.6 110
Arsenic 30.9 25.5
Bromine 808 821
Mercury 25.3 27.6
Lead 107.6 116
Cadmium 140.8 140
Steel (SS65)
Element Certified Auto Quantify
(%) (%)
Manganese 0.94 0.88
Chromium 18.45 18.5
Molybdenum 0.03 0.03
Nickel 9.47 9.53
Tungsten 0.02 0.01
Copper 0.13 0.14
Iron 69.6 70.0
The Epsilon 5’s powerful software is fully
integrated – combining instrument
control, sample handling and analysis
functions in a single program. A useful
wizard feature guides users step-by-step
through the analysis procedure and
simplifies control of the calibration
process. It also provides the functionality
and traceability necessary for laboratory
and method accreditation. The flexibility
to refine default parameters is readily
available for more experienced users.
An Auto Quantify routine (based on
Fundamental Parameter calibrations)
handles the analysis of unknown
samples, while a spectrum peak search
and match routine facilitates qualitative
analysis.
Four different levels of user
functionality (that can be password
protected) are available to safeguard
the instrument and ensure data security.
Different System User and Maintenance
User logons clearly separate customer
procedures from instrument service
access.
Behind the Epsilon 5’s simple operation
lie advanced algorithms for instrument
set-up, spectrum analysis and
calibration. The complexities of a sample
spectrum, for example, are revealed
using a powerful new deconvolution
algorithm developed in collaboration
with leading experts in the field of
applied mathematics*.
Laboratory and method
accreditation
The traceability of results (to prove
the relationship of calibrations to
certified values) is an important
aspect of modern analytical practice
and mandatory for laboratory
accreditation. The Epsilon 5
software gives users full control of
the calibration process and allows
easy demonstration of method
traceability.
*Spectrum evaluation uses non-linear least
squares fitting, based on the AXIL algorithm
developed at the University of Antwerp.
 Unrivalled 40
Sn

performance 39

Conc. (ppm)
38

The unique combination of PANalytical’s

strict quality standards, innovative
37
design and pioneering technological
achievements guarantees the unrivalled
analytical performance of the Epsilon 5.
36
Measurements are accurate and precise 0 5 10 15 20 25 30 35 40 45 50 55 60 65 70 75
and the instrument’s stability is such
that individual calibrations can be used
for months. Time-consuming re- Repeat measurements of a single sample over a period of 6 months demonstrate
standardizations are therefore the system’s precision and long-term stability
Permission kindly granted by the
unnecessary and the data produced is British Geological Survey

highly consistent over time.

Of greatest significance, however, is the

instrument’s improved low-level
Application LLD (ppm)

determination of heavy metal elements. Epsilon 5

Even in comparison with a typical WD-XRF
WDXRF system, the Epsilon 5 shows
superior performance for elements
ranging from molybdenum to the rare
earth elements, whilst maintaining good
performance for many others.

Cd Sn Sb Te I Cs Ba La Ce Nd
A comparison of application lower limits of detection with a typical WDXRF system
shows the superior performance of the Epsilon 5

Rb Ce
RMS = 3.6352 RMS = 1.6683
Correl. = 0.9994 Correl. = 0.9982
R corr. (cps/mA)
R corr. (cps/mA)

0 200 400 0 20 40 60 80 100

C chem. (Rb ppm) C chem. (Ce ppm)

Calibration plots for rubidium (Rb) and cerium (Ce) give a graphic illustration of the accuracy achievable with the Epsilon 5 (based
on 200 s live time measurements)

The Epsilon 5’s spectrum peak

search and match routine can be Cu-K a 1 Ba-K a 1
Zn-Ka 1
performed on individual or sets of Cu-K b1

spectra to provide an accurate Zn-Kb1

assessment of the elements present Ba-K a 2

I(counts/ch)

even at ppm levels. Sr-K a 2

As-K a 2 Ba-K b1
Sr-K a 1
As-K a 1
Sr-K b1 Ag-Kb1
As-K b2 La-K a 2 Cs-K b1
Rb-K b1 Y-Kb1 Cd-K b1
Br-Ka 2 La-K a 1
Zr-Ka 2 Sn-K a 2
Pb-L a 1 Pb-L b1 Ag-Ka 2 Sb-K b1 Ce-K a 2
Zr-Ka 1 Zr-Kb1 Sn-K a 1
Rb-K a 2 Ag-Ka 1 Ce-K a 1 La-K b1
Nb-Ka 2 Sb-K a 2 Cs-K a 2
Cd-K a 2
Rb-K a 1 Mo-Ka 2 Mo-Kb1 Sb-K a 1 Sn-K b1 Cs-K a 1
Br-Ka 1 Y-Ka 2 Mo-Ka 1 Pd-K a 2 Cd-K a 1
Br-Kb1 Y-Ka 1 Nb-Ka 1 Nb-Kb1 Pd-K a 1

10 20 30
Energy (keV)
PANalytical - Champion in XRF

A deeper understanding
PANalytical’s reputation for innovation and quality owes much to the
active exchange of information and ideas between customers,
researchers, academics and the company’s own experts. This
collaboration is highly valued and provides a sound understanding of
customer needs. It also helps make PANalytical systems the most
technically advanced, versatile and cost-effective solutions available.

Formerly Philips Analytical, the company has offered X-ray instruments

for materials characterization for more than 50 years, starting with the
introduction of the pioneering “Norelco Geiger Counter Diffractometer”
in 1948. During the 1970s and ‘80s the PW1400 series XRF spectrometers
became legendary, indeed some are still in service today, over 25 years
after the series was first introduced. More recently, the PW2400/MagiX
series spectrometers have the largest installed base of any WDXRF
instrument and it’s successor, the Axios, is undoubtedly the finest
wavelength dispersive spectrometer available.

The Epsilon 5 continues this tradition by combining the advantages of

3-dimensional EDXRF with the famous long-term stability and reliability
of PANalytical spectrometers.
 Quality Drive

Quality to rely on
Quality is a fundamental driving force at PANalytical. The
Epsilon 5 has been designed, built and tested according to
strict PANalytical quality management in the company’s ISO
9001:2000 certified factory.

Customer Service

Dedicated customer support

PANalytical places great emphasis on customer support.
Working from a wide network of service centres, its teams of
application specialists support more customers and cover
more countries than any other manufacturer of analytical
X-ray equipment.
 Global and near

PANalytical

Although diligent care has been used to ensure that the information herein is accurate, nothing contained herein can be construed to imply any

further notice. Please contact us for the latest version of this document or further information. © PANalytical B.V. 2009. 9498 707 27213 PN9646
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representation or warranty as to the accuracy, currency or completeness of this information. The content hereof is subject to change without
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metrology. F +31 (0) 546 534 598
info@panalytical.com
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to their product portfolio. Optical emission spectrometry (OBLF GmbH, Germany),
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Inc.) capabilities together with XRD and XRF can provide customers with tailor-
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