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
D
RE
y
RA
erg
VIS
E
IBL
Central to PANalytical’s business
philosophy is a determination that its
products and services should increase
the efficiency of customer processes.
And this was a driving force behind the
introduction of the Epsilon 5.
HT
LIG
25
0.1
A
TR
UL LET
VIO
A
X-R
125
keV YS
A
γ -R
keV YS
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.
INF
Epsilon 5 Alternative Fuels
A dedicated, pre-calibrated system
for the analysis of solid alternative
fuels.
Leading the way
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
half a century of experience in this
dynamic field.
En
• 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
• 100% efficient Ge detector
ensuring high detection
efficiency across the periodic
table
• 15 polarization/secondary
targets allowing optimization of
the excitation source according
to the elements of interest
• X-Y sample changer
ensuring flexible, unattended
handling of up to 130 samples in
six trays.
The Epsilon 5
A fully integrated hardware and
software system, the Epsilon 5 has been
designed for optimal performance
across the periodic table. With the
incorporation of five patented
technologies, it sets the standard for
quality and performance in XRF analysis.
Characterized by highly precise,
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.
ICP - OES
XRF
γ-SPEC
Unlike many other analytical techniques
XRF spectroscopy does not involve sample
dissolution. By avoiding the potential for
inaccuracies caused by incomplete
dissolution, the complete analysis offered
by XRF helps ensure the accuracy and
reliability of results.
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.
Simple EDXRF
Simple EDXRF spectrometers employ a
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
spectrum, but also a large amount of
the scattered X-ray tube spectrum. This
contributes to relatively high
background levels and negatively
influences the detection limits
achievable.
Sample
Source
Detector
Polarising EDXRF
4
5
Energy (keV)
5
7
8
6
7
8
2-dimensional optics
The primary beam (yellow) from the
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
spectrum of the sample is recorded by a
detector placed along the third axis
(purple).
I(cps/ch)
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.
I(cps/ch)
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.
4
5
3-dimensional optics
Energy (keV)
Customer Benefits
K-Ka 1
Ca-K a 1
Fe-K a 1
Mn-Ka 1
I(cps/ch)
Cr-K b1
Ca-K b1
Ti-Kb1
V-Kb1
V-Ka 1
Ti-Ka 1
Cr-K a 1
La-L b1
La-L a 2
Pr-L a 2 Ce-L b1 Pr-L b1
Ce-L a 2
Nd-La 2
Ba-L a 2
Nd-Lb1
Ce-L a 1
Nd-La 1
Ba-L a 1
Sm-L a 2
Pr-L a 1
La-L a 1
Sm-L a 1
5
4
Sm-L b1
6
Energy (keV)
Ce-K a 1
I(cps/ch)
La-Ka1
Analytical flexibility
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.
Ce-K b1
Ce-K a 2
La-K a 2
Nd-Ka 1
Pr-K a 2 Ba-K b1
La-K b1
Pr-K a 1 Nd-Ka 2
Ba-K a 1
Ba-K a 2
30
32
34
36
Epsilon 5 is able to overcome these
problems and make K-line analysis of
heavy elements a reality. This, in turn,
results in superior spectral resolution
and lower detection limits.
Sm-K a 2
38
Energy (keV)
Improved low-level determination
of heavy elements
Traditionally in XRF heavy elements are
analyzed using their L-series spectral
lines. This is because of restrictions
imposed on the use of K-lines by
inadequate excitation voltages, suboptimal 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
Non-destructive analysis
The Epsilon 5’s combination of low
power (600 W) and three-dimensional
optics causes very low sample heating or
X-ray damage. Samples are therefore
unaffected by analysis, and even
delicate foils and filters can be
measured repeatedly over significant
periods of time.
Precision
The Epsilon 5 capitalizes on the inherent
precision of XRF. Because calibrations
can be maintained for many months,
the continual short-period recalibrations, associated with other
instrument techniques, are unnecessary.
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
I(cps/ch)
Sn
Sb
I
70kV
50kV
27
24
34
30
37
40
Energy (keV)
Targets (3)
Up to 15 targets (a combination of
polarizing and secondary fluorescence)
can be used. The basic system is
configured with nine targets to provide
comprehensive coverage of the periodic
table. The additional six target positions
can be configured when optimum
excitation conditions are required for
the lowest possible detection limits in
specific applications. A large choice of
additional target materials is available.
High-voltage Gd or Sc/W X-ray tube (1)
Operating at a maximum power of
600 W and voltages between 25 kV and 100 kV,
PANalytical’s patented X-ray tubes are unique
among EDXRF spectrometers. The characteristic
tube lines of the Gd-anode enhance the
fluorescence of elements in the range of rhodium
to barium, while the Sc tube lines of the Sc/W tube
enhance the fluorescence of lighter elements. The
tube’s 100 kV capability has advantages for the
excitation of heavy element K-lines.
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.
I(cps/mA)
2590
2585
2580
CSE = 0.045%
RMS = 0.054%
2575
DAY 1
DAY 2
DAY 3
DAY 4
Stability
The Epsilon 5 benefits from decades of
PANalytical experience in the
development of WDXRF spectrometers
– systems that are renowned for their
excellent stability. Its robust
construction, precisely made mechanics
and closely controlled cabinet
temperatures (35 ±1.0 ºC) provide
outstanding stability.
1
2
4
3
1.2
Ge (5mm)
Relative Efficiency
1.0
0.8
Si(Li) (3mm)
0.6
Si-drift (0.3mm)
0.4
0.2
0
0
5
10
15
20
25
30
Energy (keV)
35
40
45
50
X-ray detectors (4)
The PAN-32 liquid nitrogen-cooled
solid-state Ge detector is characterized
by a high degree of detection efficiency
across the periodic table. Unlike other
common solid-state detectors, it
maintains 100% efficiency for heavy
element K-lines – a perfect match for
the Epsilon 5’s high-voltage excitation
source.
LiF200 (Fine Collimator)
The PAN-32 detector demonstrates
superior spectral resolution at high
energies compared to that obtained in
WDXRF using dispersion crystals.
Ba
Intensity
Cs
Ge Solid-State Detector
0
30
32
Energy (keV)
34
36
Full Width at Half Maximum (keV)
1.00
0.90
0.80
LiF200 (Fine collimator)
0.70
0.60
0.50
0.40
Ge solid-state detector
0.30
0.20
0.10
0.00
0
10
20
Energy (keV)
30
40
7
Automatic current regulation (5)
Different sample types have variable
spectrum characteristics making it
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
from sample to sample.
8
5
6
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
10
X-Y sample changer (7)
The changer can accommodate up to six
sample trays. Different trays are
available for sample holders, steel rings
and unmounted samples with diameters
of 25, 32, 41 and 50 mm. Total capacity
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
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.
Loading time is reduced by direct
loading/unloading of the unmounted
samples to a cup in the measurement
position.
A priority loading position allows
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.
Mobility and accessibility (9)
Mounted on wheels, the Epsilon 5 is
easily manoeuvred in confined
laboratory spaces. Removable panels on
all sides of the instrument allow
unrestricted access for maintenance.
External connections
The Epsilon 5 is powered from a
standard wall socket (eg 230 V, 13 A)
and is connected to the PC via USB and
UTP ports. External cooling water is not
necessary.
Liquid nitrogen level sensing (10)
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)
Nickel127129
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.
Copper118 130
Zinc 220231
Arsenic145 156
Rubidium131
137
Strontium830
829
Zirconium310
314
Barium1500 1460
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*.
Plastic (BCR680)
Element
Certified
Auto Quantify
(ppm)
(ppm)
Chromium114.6
110
Arsenic30.9
25.5
Bromine808
821
Mercury25.3
27.6
Lead107.6
116
Cadmium140.8
140
Steel (SS65)
Element
Certified
Auto Quantify
(%)
(%)
Manganese0.94
0.88
Chromium18.45
18.5
Molybdenum0.03
0.03
Nickel9.479.53
Tungsten0.02
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.
0.01
Copper0.13 0.14
Iron69.670.0
*Spectrum evaluation uses non-linear least
squares fitting, based on the AXIL algorithm
developed at the University of Antwerp.
Unrivalled
performance
40
Sn
Conc. (ppm)
39
The unique combination of PANalytical’s
strict quality standards, innovative
design and pioneering technological
achievements guarantees the unrivalled
analytical performance of the Epsilon 5.
Measurements are accurate and precise
and the instrument’s stability is such
that individual calibrations can be used
for months. Time-consuming restandardizations are therefore
unnecessary and the data produced is
highly consistent over time.
38
37
36
0
5
10
15
20
25
30
35
40
45
50
55
60
65
70
75
Repeat measurements of a single sample over a period of 6 months demonstrate
the system’s precision and long-term stability
Permission kindly granted by the
British Geological Survey
Application LLD (ppm)
Of greatest significance, however, is the
instrument’s improved low-level
determination of heavy metal elements.
Even in comparison with a typical
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.
Epsilon 5
WD-XRF
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
Ce
Rb
RMS = 1.6683
Correl. = 0.9982
R corr. (cps/mA)
R corr. (cps/mA)
RMS = 3.6352
Correl. = 0.9994
0
200
400
0
20
C chem. (Rb ppm)
40
60
80
100
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)
Ba-K a 1
Cu-K a 1
Zn-Ka 1
Cu-K b1
Zn-Kb1
I(counts/ch)
The Epsilon 5’s spectrum peak
search and match routine can be
performed on individual or sets of
spectra to provide an accurate
assessment of the elements present
even at ppm levels.
Ba-K a 2
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
Sn-K a 2
Zr-Ka 2
Pb-L a 1 Pb-L b1
Ag-Ka 2
Ce-K a 2
Sb-K b1
Sn-K a 1
Zr-Ka 1 Zr-Kb1
La-K b1
Ag-Ka 1
Ce-K a 1
Rb-K a 2
Cs-K a 2
Sb-K a 2
Nb-Ka 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
Y-Ka 2
Pd-K a 2 Cd-K a 1
Br-Ka 1
Mo-Ka 1
Br-Kb1 Y-Ka 1 Nb-Ka 1 Nb-Kb1 Pd-K a 1
10
30
20
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.
PANalytical
PANalytical is one of the world’s leading suppliers of analytical instrumentation
and software for X-ray diffraction (XRD) and X-ray fluorescence spectrometry
(XRF). The materials characterization equipment is used for scientific research and
development, for industrial process control applications and for semiconductor
metrology.
During the last decade PANalytical has added a variety of other analysis techniques
to their product portfolio. Optical emission spectrometry (OBLF GmbH, Germany),
pulsed fast thermal neutron activation (Sodern, France) and near-infrared (ASD
Inc.) capabilities together with XRD and XRF can provide customers with tailormade analytical solutions for the characterization of a wide range of products such
as cement, metals, nanomaterials, polymers and many more.
PANalytical’s headquarters are in Almelo, the Netherlands. Fully equipped
application laboratories are established in Japan, China, the USA, and the
Netherlands. PANalytical’s research activities are based in Almelo (NL) and on
the campus of the University of Sussex in Brighton (UK). Supply and competence
centers are located on two sites in the Netherlands: Almelo (development and
production of X-ray instruments) and Eindhoven (development and production of
X-ray tubes) and in Boulder, USA (development and production of near-infrared
instruments). A sales and service network in more than 60 countries ensures
unrivalled levels of customer support.
The company is certified in accordance with ISO 9001 and ISO 14001.
Visit our website at www.panalytical.com for more information about our
activities.
PANalytical is part of Spectris plc, the productivity-enhancing instrumentation and
controls company.
PANalytical B.V.
Lelyweg 1, 7602 EA Almelo
The Netherlands
T +31 (0) 546 534 444
F +31 (0) 546 534 598
[email protected]
www.panalytical.com
Regional sales offices
Americas
T +1 508 647 1100
F +1 508 647 1115
Europe, Middle East, Africa
T +31 (0) 546 834 444
F +31 (0) 546 834 969
Asia Pacific
T +65 6741 2868
F +65 6741 2166
Although diligent care has been used to ensure that the information herein is accurate, nothing contained herein can be construed to imply any
representation or warranty as to the accuracy, currency or completeness of this information. The content hereof is subject to change without
further notice. Please contact us for the latest version of this document or further information. © PANalytical B.V. 2009. 9498 707 27213 PN9646
Global and near