Leading the way in heavy metals analysis

EPSILON 5

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.

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

The Epsilon 5Spectrometer

Leading the wayA 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.

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.

The Epsilon 5A 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

Energy

0.125 keV 125 keV

INFRA

RED

X-RAY

Sγ-RAY

S

ULTRA

VIO

LET

VISIBLE LIG

HT

Epsilon 5 Alternative FuelsA 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.

About X-ray fluorescence spectroscopy

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.

• 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.

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

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.

An essential tool GeologyRecyclingRoHS WEEEEnvironmentalAlternative Fuels

Simple EDXRFSimple 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.

State of the art EDXRF

Sample

Source

Detector

Energy (keV)

I(cp

s/ch

)

4 5 5 7 8

Energy (keV)

I(cp

s/ch

)

4 5 6 7 8

2-dimensional optics

3-dimensional optics

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.

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).

About XRF spectrometersThe 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

Customer Benefits

Analytical flexibilityThe 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.

Improved low-level determinationof heavy elementsTraditionally 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, sub-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

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.

Non-destructive analysisThe 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.

PrecisionThe Epsilon 5 capitalizes on the inherent precision of XRF. Because calibrations can be maintained for many months, the continual short-period re-calibrations, associated with other instrument techniques, are unnecessary.

Sm-K 2a

Ce-K 1b

Ba-K 2a

Ba-K 1a

La-K 2a

La-Ka1

Ce-K 2a

Ce-K 1a

La-K 1bNd-K 1a

Nd-K 2aBa-K 1b

Pr-K 1aPr-K 2a

30 32 34

Energy (keV)

36 38

I(cp

s/ch

)

Ca-K 1b Ti-K 1b

Ba-L 2aLa-L 2a Pr-L 2a

Nd-L 2aNd-L 1a

Ce-L 1b

Sm-L 2aSm-L 1a

Pr-L 1b

Pr-L 1a

La-L 1b

Ce-L 2aCe-L 1aBa-L 1a

La-L 1a

K-K 1a Ca-K 1a

Ti-K 1a

Mn-K 1a

V-K 1a V-K 1bCr-K 1a

Nd-L 1b

Sm-L 1b

Cr-K 1b

Fe-K 1a

54 6

Energy (keV)

I(cp

s/ch

)

Customer Benefits

Safety firstThe 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 handlingAn 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 mobileThe 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

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.

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.

Sn Sb

I

Ba

La

CeNd

100kV

70kV

50kV

Energy (keV)

I(cp

s/ch

)

24 27 30 34 37 40

2575

2580

2585

2590

I(cp

s/m

A)

DAY 1 DAY 2 DAY 3 DAY 4

CSE = 0.045%RMS = 0.054%

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.

12

3

4

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.

The PAN-32 detector demonstrates superior spectral resolution at high energies compared to that obtained in WDXRF using dispersion crystals.

0 5 10 15 20 25 30 35 40 45 50Energy (keV)

Si-drift (0.3mm)

Si(Li) (3mm)

Ge (5mm)

0

0.2

0.4

0.6

0.8

1.0

1.2

Rel

ativ

e Ef

fici

ency

0 30 32 34 36

Cs

Ba

Inte

nsi

ty

Energy (keV)

LiF200 (Fine Collimator)

Ge Solid-State Detector

0 10 20 30 40

1.00

0.90

0.80

0.70

0.60

0.50

0.40

0.30

0.20

0.10

0.00

Full

Wid

th a

t H

alf

Max

imu

m (

keV

)

Energy (keV)

Ge solid-state detector

LiF200 (Fine collimator)

7

5

6

9

8Automatic 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.

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.

10

System Features

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 connectionsThe 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

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*.

*Spectrum evaluation uses non-linear least squares fitting, based on the AXIL algorithm developed at the University of Antwerp.

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.

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

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.

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.

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 re-standardizations are therefore unnecessary and the data produced is highly consistent over time.

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.

Unrivalled performance

RMS = 3.6352Correl. = 0.9994

0 200 400

Cchem. (Rb ppm)

Rco

rr. (

cps/

mA

)

RbRMS = 1.6683Correl. = 0.9982

0 20 40 60 80 100

Cchem. (Ce ppm)

Rco

rr. (

cps/

mA

)

Ce

Sr-K 2a

Zr-K 2a

Pd-K 2a

Ag-K 2a Sb-K 1b

Sr-K 1b

Br-K 1a

As-K 2aAs-K 1a

Cu-K 1aZn-K 1a

As-K 2bBr-K 2a

Rb-K 2a

Sr-K 1a

Zr-K 1aNb-K 2a

Y-K 1b

Zr-K 1b

Mo-K 2aMo-K 1a

Nb-K 1b

Mo-K 1b

Pd-K 1a

Ag-K 1aCd-K 2aCd-K 1a

Ag-K 1bCd-K 1b

Sn-K 2aSn-K 1a

Sb-K 2aSb-K 1a Sn-K 1b

Cs-K 2aCs-K 1a

Ba-K 1a

Ba-K 2a

La-K 2aLa-K 1a

Ce-K 2aCe-K 1a

Cs-K 1b

Ba-K 1b

La-K 1b

I(co

un

ts/c

h)

10 20 30

Energy (keV)

Zn-K 1b

Cu-K 1b

Rb-K 1b

Y-K 2aY-K 1a

Rb-K 1a

Br-K 1b Nb-K 1a

Pb-L 1a Pb-L 1b

Ap

plic

atio

n L

LD (

pp

m)

Cd

Epsilon 5

Sn Sb Te I Cs Ba La Ce Nd

WD-XRF

A comparison of application lower limits of detection with a typical WDXRF system shows the superior performance of the Epsilon 5

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)

Repeat measurements of a single sample over a period of 6 months demonstrate the system’s precision and long-term stability

360 5 10 15 20 25 30 35 40 45 50 55 60 65 70 75

37

38

39

40

Co

nc.

(p

pm

)

Sn

Permission kindly granted by the British Geological Survey

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

Dedicated customer supportPANalytical 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.

Quality to rely onQuality 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

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 tailor-made 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 AlmeloThe NetherlandsT +31 (0) 546 534 444F +31 (0) 546 534 598info@panalytical.comwww.panalytical.com

Regional sales offices

AmericasT +1 508 647 1100 F +1 508 647 1115

Europe, Middle East, AfricaT +31 (0) 546 834 444 F +31 (0) 546 834 969

Asia PacificT +65 6741 2868 F +65 6741 2166

Global and near

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