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The document discusses wavelength dispersive X-ray fluorescence (WDXRF) spectroscopy and its use for chemical analysis of solids and liquids. It introduces the ARL OPTIM'X instrument as a compact WDXRF system.

The document discusses the wavelength dispersive X-ray fluorescence (WDXRF) technique which can analyze elements from beryllium to uranium in a variety of samples. It also mentions other spectroscopic methods.

The ARL OPTIM'X instrument has features like unique WDXRF platform capabilities, element coverage from fluorine to uranium, closely coupled optics for increased intensity, multichromators for fast analysis, and configurations for speed and flexibility.

e l e m e n t a l

a n a l y s i s

ARL OPTIMX
X-Ray Fluorescence Spectrometer

Optimized Performance for Your Application

Analyze Detect Measure Control

ARL OPTIMX
Optimized Performance for Your Application

ARL OPTIMX
Optimized Performance for your Application.
The wavelength dispersive X-ray fluorescence
(WDXRF) technique is one of the most
versatile analytical methods for the chemical
analysis of solids and liquids. Elements from
beryllium to uranium can be analyzed in a
wide variety of samples with accuracy,
precision and reliability. The technique and
the analytical methods are mature enough to
establish clear qualitative and quantitative
characterization of diversified materials.
Modern technological developments have
helped to include WDXRF into reference
methods for analytical laboratories (ASTM
and ISO norms for example) by virtue of their
simplicity, flexibility, affordability and
reliability. The cost per analysis is clearly
advantageous over many traditional wet
chemical and other spectroscopic methods.

Optimum configuration for specific


applications with simplified operation
(ISO or ASTM standards compliance)
Stand alone and autonomous operation
without water cooling
No gas supply required (depending on the
configuration)
Direct and simple introduction of the
sample
Automatic analysis of batches with
sample changer
Small footprint.

Conguration for speed and


exibility
Up to 8 elements simultaneously using 4
Multichromators
Sequential analysis with the
SmartGonio
Sequential-simultaneous analysis:
SmartGonio and 2 elements
simultaneously on one Multichromator

A compact and independant


WDXRF instrument
Continuing its tradition of innovation and
leadership in WDXRF, Thermo Electron
Corporation presents a new compact
instrument, the ARL OPTIM'X, with the
following salient analytical features:
Unique WDXRF platform with sequential
and/or simultaneous capabilities
Element coverage from fluorine to
uranium, depending on configuration
Closely coupled optics for increased
intensity (210% higher than conventional
geometry)
Multichromators for fast analysis;
Unique compact SmartGonio for
sequential analysis
Sequential-simultaneous configuration
blending speed to analytical flexibility
High precision (short term and long term
repeatability) thanks to temperature
regulation of spectrometer and crystals
Superior spectral resolution from low Z
elements to heavy elements (~15 eV at
CaK)

Excellent resolution: Si and Al peaks are free from any interference


despite the presence of 55% of Mg in this magnesite sample

Cassettes for manual loading of solids

Cells for liquids and loose powder analysis

Configuration selected according to application needs

ARL OPTIMX with its sample changer

Fast qualitative analysis


When a SmartGonio is fitted, two forms
of digital scanning are available. Step
scanning provides precise definition of
peaks with a resolution of 0.001. For rapid
qualitative analysis, continuous digital
scanning allows fast acquisition of spectra
at speeds up to 320/min. Peaks
identification is automatic.

Quantitative analysis made easy


Analytical programs and calibrations are
defined with the help of the on-line
Analytical Assistant. Calibration curves are
built using the multi-variable regression
(MVR) program.
Correction models serve to minimize the
influence of interfering elements in
multicomponent matrices and to achieve
better accuracy of analysis. These models are:
Line overlap correction
Additive correction on intensities
Additive correction on concentrations
Lucas-Tooth: Multiplicative correction on
intensities
Lachance-Traill: Multiplicative correction
on concentrations
Lachance-Traill+/Lachance-Traill AC:
Multiplicative and additive corrections on
concentrations
Comprehensive Lachance (COLA) with 3
term alphas to be used with the optional
NBSGSC fundamental parameters
program, which can simulate analytical
calibrations for homogeneous materials.
Interelement correction factors
(theoretical alphas) are calculated and
used as known coefficients in the MVR.
This minimizes the number of standards
necessary to produce calibrations and
improves the accuracy of analysis.

The Analytical Assistant helps definition of analytical programs,


calibrations and instrument use

Easy navigation and comfortable operation

In addition, ex-works calibrations can


be delivered for various materials such as
various oxides through the General Oxide
calibration, several metal matrices, ferroalloys and others for which analytical
specifications are available on request.

Quantitative analysis - Typical results presentation with flagged


values

Statistical Process Control - Typical screen

Sample 25ppm 100ppm

0.12
0.10
Intensity (Kcps)

Petrochemical industry analysis of S


(ISO 14596 or ASTM D2622), Pb (ASTM
D5059) or other elements in gasoline and
oils
The calibration curve for sulfur in oils and
gasoline can be easily obtained for
concentrations ranging from ppm levels
up to 5% (see Fig. 1). The excellent limit
of detection of 1.4 ppm in 100s (or 1 ppm
in 200s) is achieved. This good result is
proved by the reproducibility test shown
in Table 1. Separate Application Notes
XRF-701 and XRF-706 give additional
details
Major and minor oxides in raw materials
such as limestone, sand, feldspar,
bauxite, magnesite and other mining
applications as well as clinker and raw
meal. The ARL OPTIM'X shows excellent
repeatability of analysis for such types of
materials (see Table 2).
As the calibration curve (Fig. 2) proves,
the analysis of Na can be carried out
without problem either with the
SmartGonio or with a fixed channel.
Additional data can be found in separate
Application Notes XRF-702 and XRF-705
Major and minor oxides in products such
as sanitary ceramics, refractories, slags
and sinters (more details in separate
Application Notes XRF-703 and XRF-704)
Glass, paints, paper, ferro-alloys, silicon,
metal sheets and other products where a
few major and minor elements need to be
monitored
Food industry for major and minor
nutrients and other regulated elements.
Typical concentration ranges and the
excellent limits of detection in milk
powders are listed in Table 3 below

0.08
0.06
0.04
0.02
0.00
0.000

0.008
0.012
Concentration

0.004

0.016

0.020
(%)

Fig. 1: Calibration curve for S in oils and gasoline


(zoom on the low concentration level range)

Cell 1
Cell 2
Cell 3
Cell 4
Cell 5
Cell 6
Cell 7
Average
Std. Dev.

25.4
25.7
26.4
26
25
25.9
26.7
25.9
0.58

100.6
100.7
101.8
102.3
98.4
100.5
101.5
100.8
1.27

Table 1: Excellent
reproducibility obtained for
analysis of sulfur in oils (120s)

Run nr

Al2 O3

Ca0

Fe2O3

K2O

MgO

P2O5

SO3

SiO2

1
2
3
4
5
6
7
AVG
Sd.Dev.

0.329
0.328
0.328
0.324
0.326
0.327
0.327
0.327
0.0015

50.41
50.44
50.45
50.41
50.36
50.38
50.41
50.41
0.029

0.303
0.303
0.304
0.305
0.301
0.301
0.302
0.303
0.0014

0.116
0.117
0.116
0.117
0.117
0.116
0.116
0.116
0.0005

2.76
2.77
2.74
2.76
2.75
2.74
2.74
2.75
0.011

0.014
0.015
0.014
0.014
0.014
0.014
0.014
0.014
0.0003

0.036
0.036
0.036
0.036
0.036
0.035
0.036
0.036
0.0003

2.68
2.68
2.68
2.69
2.68
2.69
2.68
2.68
0.005

Table 2: Repeatability test for a limestone sample (pressed powder, 100 s counting time)

0.025

0.02

Intensity (kcps)

ARL OPTIMX
Optimized Performance for Your Application

Optimized for specic


applications

0.015

0.01

0.005
0

0.05

0.1

0.15

0.2

0.25

0.3

0.35

Concentration (%)

Fig. 2: Calibration curve for Na using fusion beads of oxides. Standard error of estimate is
0.011% in a range from 0.02% to 0.32%

Table 3: Limits of detection (LoD) in milk


powders prepared as pressed pellets
(*cumulated counting time of SmartGonio
for Na and Mg)

Element

Analytical device

Typical ranges

LoD (ppm in 60s)

Na
Mg
P
K
Ca
Fe
Cu
Zn
Cl
Mn
Se

Fixed channel
Fixed channel
SmartGonio
SmartGonio
SmartGonio
SmartGonio
SmartGonio
SmartGonio
SmartGonio
SmartGonio
SmartGonio

0 0.03 %
0 0.12 %
0 1.1 %
01%
0 1.6 %
0 0.33 %
0 0.012 %
0 0.2 %
0 0.48 %
0 0.0023 %
0 3.4 ppm

20 ppm*
11 ppm*
4.4 ppm
2 ppm
10 ppm
2.1 ppm
0.6 ppm
2 ppm
10 ppm
1.2 ppm
0.24 ppm

LARGE VARIETY OF SAMPLES


Many different types of
samples can be analyzed on
the ARL OPTIM'X: conductive
or non-conductive solids,
liquids, loose powders,
pressed pellets, fusion beads,
pastes. However the
instrument configuration is
optimized for your specific
application.

Manual introduction
of a solid sample
placed in a cassette

ARL OPTIMX
Optimized Performance for Your Application

Data Handling: WinXRF


Designed for Windows XP Professional,
the comprehensive and user-friendly
WinXRF analytical software supports
spectrometer operation and data handling.

Some of its salient features are:


Graphical user interface featuring
navigation, operation and display through
HTML pages using Internet Explorer
Analytical Assistant helping the operator
in defining analytical programs,
calibrations and basic operations of the
instrument
Simple routine analysis mode through hot
key operation or software shortcuts
leading to analysis method templates
Unattended use through batch commands
and sequences
Correction for curved background
Variable counting time on peak and
background positions
Automatic choice of analytical program
according to the intensity or
concentration response
Type standardization to reach ultimate
analytical accuracy
User-defined result presentation with
abnormal values marked with flag and
color
Quality check & quality sort
Editing and validation of results with
audit trail protected by password
Recalculation of concentration results for
verification or update purpose, saves
analysis time
Fast and accurate calibration curve
determination through multi-variable
regression (MVR) facility
Post-processing functions performed
while the instrument is analyzing, e.g.
results storage and retrieval or statistics
and export (e.g. to Excel spreadsheet)
SPC-Basic: instrument control with online integrated SPC (Statistical Process
Control) package

Standardless analysis through OptiQuant

Audit trail of drift correction, type


standardization update and calibration
changes
Monitoring and logging of instrument
alarms and status with graphical display
tools
Password protection with up to 8
different access levels
Remote diagnostics through modem
connection.

Main software options


ARLnet: Package of results transmission
solutions via LAN Local Area Network to
up to 18 destinations. Includes among
others: TCP/IP computer task to
computer task transmission, Netfile
transmission of results to files on local or
network disks and printing on network
printers
Compac: transmission of results to up to
5 computers via serial lines
Remote: remote display of results to up to
8 remote printers or terminals via serial
lines
NBSGSC: program for theoretical alphas
generation
Charge correction: Calculation of furnace
charge additions
Metaverage: Average of sample analyses
according to pre-configured schemes
SPC-Full: integrated Statistical Process
Control software for instrument quality
assurance and production process control.
Fully on-line (bi-directional) with
automatic evaluation and SPC test result
feedback to the operator
Printing of reports of stored analytical
results according to a variety of Thermo
Electron or user defined formats
Remote Sample Definition: Reception of
sample identification and analysis
parameters from third party application
software (e.g. ARL ARMS or process
computer)
Sentry: allows a simplified sample
registration including bar code support
and powerful sample batch entry
capabilities

OEM Mode: connection to an external


process computer for automation
purposes
Translation of WinXRF texts into any
language supported by Windows XP
Professional
OptiQuant: Adaptation of the renowned
UniQuant package to the ARL OPTIMX
spectrometer. OptiQuant provides
"standardless" analysis for up to 73
elements when specific standards are not
available, or when samples can only be
obtained in small quantities or as
irregular shapes. Additionally OptiQuant
calculates the balance of unanalyzed
elements present in the sample, e.g.
organic and ultralight elements. The
OptiQuant optional package is fully
calibrated and pre-installed in the factory
using two fixed channels for Na and Mg
and the SmartGonio. Hence it is ready
to be used right after installation of the
instrument at the customer's site. Stable
samples for setting-up and maintenance
over time are included.

MVR calibration curve: real concentrations vs. intensities

Collimator

Exclusive SmartGonio

Sample

Optical encoder
2 theta drive

Quantitative analysis of any element from F to


Fe or Al to Zn (with one detector fitted)
Quantitative analysis of any element from Al to U
(with two detectors fitted)
Angular positioning to ensure / 2
relationship between crystal and detector is
achieved through Moir fringe optical encoders:
- no friction
- no wear with time!
Temperature regulation of crystals for best
analytical stability
Closest coupling with X-ray tube provides
optimized sensitivity

Detector
Crystal
Optical encoder

X-ray tube
1 theta drive

SmartGonio
principle of
operation

Specications for the ARL OPTIMX


Element range
Spectrometer environment
Spectrometer design
Spectrometer arrangement
Spectrometer capacity

X-ray excitation

Multichromator

SmartGonio

Counting electronics

Sample loading
Sample holders

Dimensions and weight


Laboratory information
Power requirements:
Safety standards:

Fluorine (Z=9) to uranium(Z=92)


Vacuum or air for solids, helium for liquids and loose powders
Analysis devices contained in a vacuum chamber made of grey cast iron and temperature
controlled
X-ray tube inclined at 66 under sample
Simultaneous configuration: Four Multichromators
Sim-seq configuration: One SmartGonio + one Multichromator
Each Multichromator is composed of two fixed channels
Air cooled Rh anode end window tube with thin Be window (0.075 mm). 50 W power
providing excitation similar to 200 W thanks to ultra close coupling and large solid angle
irradiation. Other anodes available on request. Solid-state high frequency generator of
maximum voltage 50 kV and maximum current 2 mA (combinations chosen to be less than
50W). Max. line voltage variation: 230V -15% to +10%. Stability: 0.0002% per 1% variation
Fixed channel using multiple curved crystal optics. Sealed detectors available for all
elements from sodium (Z=11). Flow proportional or scintillation detectors also available
depending on element. Dual pulse height integration to discriminate and correct for 2nd
order peaks. A Multichromator is composed of two fixed channels, but some elements can
only be fitted as single channel monochromator
Fully automatic, gearless, microprocessor controlled compact goniometer using optical
encoders. Total angle range: 0-150 2 (Flow proportional counter: 17-150, Scintillation
counter: 0-90). Continuous digital scans: from 0.25/min to 320/min
Multi-channel analyzer to discriminate peaks of higher energies. Digital Automatic Gain
Control (AGC) for pulse shrinking correction. Automatic dead time correction ensures linearity
of response up to 2 Mcps on flow proportional counter and 1.5 Mcps on scintillation counter
Basic: 1 position for cassette or liquid cell. Optional: 13 position autosampler
Sample cassettes with maximum size of sample: height 26 mm, diameter 52 mm. Liquid cell:
height 22 mm, external diameter 40 mm. Exposed opening: 29 mm diameter (basic). Rotation
of sample holder in analysis position: 6 to 60 rpm
H 126 cm, W 88 cm, D 82 cm with basic sample changer. System weight: approximately 250 kg
Optional phone service support through modem connection
1.5 kVA single phase
Electrical and protection: IEC 1010-1, IEC 950
Radiation (fully protected system): ORaP (CH) 414.501 and BGB1.I. norms
Electro-magnetic immunity: CENELEC EN 50081-2 + EN 50082-2 (industrial)

Thermo Electron Corporation reserves the right to vary these specifications without prior notice

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2003 Thermo Electron Corporation. All rights reserved.


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BR41062_E 11/03C

XRF-02-1062-1103-CH-e

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