Manual M1

Manual M1 ORA / M1 MISTRAL
Bruker AXS Microanalysis

12489 Berlin, Schwarzschildstr. 12
Mail: [email protected]
Manual Karatmeter
CONTENT OF MANUAL
MANUAL M1 ORA / M1 MISTRAL 1
1. INTRODUCTION 4
1.1 About this manual 4
1.2 User Information 4
1.3 Intended Usage 5
1.4 Guarantee and liability 5
2. SAFETY INSTRUCTIONS 6
2.1 Basic safety requirements 6
2.2 Safety requirements on the place of installation 7
2.3 Radiation protection 7
2.4 Protection against electric current 8
2.5 Staff requirements 9
2.6 Safety equipment 9
2.7 Warning labels and name plates 11
3. INSTALLATION REQUIREMENTS 12
3.1 Electrical connection 12
3.2 Room planning 12
3.3 Environmental conditions 13
4. PRODUCT DESCRIPTION 14
4.1 Product versions 15
5. TECHNICAL DESCRIPTION 16
5.1 Technical parameters of the M1 ORA/Mistral 16
5.2 Main components 18
6. FUNCTIONAL DESCRIPTION 19
6.1 X-ray fluorescence 19
6.1 Detection of the X-ray quanta 20
6.1 Digitalization and channel allocation 21
6.1 Spectroscopic resolution 22
6.1 Composition of a Spectrum of the M1 ORA/Mistral 24
6.1 Evaluation of X-ray fluorescence spectra 25
7. SOFTWARE 28
7.1 Structure 28
7.2 Installation of the program 29
7.3 Start of the program 33
7.4 Configuration files in the program structure 35
8. START OF OPERATION 37
8.1 Installation of the instrument 37
8.2 Establishing the operating state 37
2 / 77 Bruker AXS Microanalysis GmbH

Manual Karatmeter
9. PROGRAM XSPECT 40
9.1 User Interface 40
9.2 Start of the program 41
9.3 Instrument Status line 42
9.4 Function panels 43
9.5 Service measurements 44
9.5.1 Reference measurement 44
9.5.2 Measurement of pure elements 45
9.5.3 Measurement of calibration samples in the service mode 47
9.6 Settings of the instrument 48
9.6.1 Setting of tube parameters 48
9.6.2 Setting for the measure spectrum 50
9.6.3 Video settings 50
9.7 Spectrum display and manipulation 51
9.8 Quantification models 54
9.9 Fundamental-Parameter quantification 55
9.9.1 Quantification with the preset application 55
9.9.2 Generation of a standardless application 56
9.10 Standard based quantification 57
9.10.1 Measurement with an application 59
9.10.2 Evaluation of a loaded spectrum 63
9.10.3 Generation of an application 64
9.10.4 Display and edit details of an application 68
9.10.5 Normalization of an application 69
9.10.6 Calibration of an application 70
10. THE SERVICE PROGRAM XSTOOLS 74

10.1 Managing standard samples 74
10.2. Process of reference data 76
10.3 Display of log-file data 77
10.4 Update measuring time 77

Manual Karatmeter
1. Introduction
1.1 About this manual
These operating instructions are intended to familiarize you with the operation of the
M1 ORA/Mistral X-ray analysis machine from Bruker Microanalysis GmbH. The
instructions allow you to get started quickly and include all information necessary to
operate the machine safety and competently.
These instructions cover functionality, configuration and operation of the M1
ORA/Mistral.
A solid understanding of these instructions is mandatory for the operation of the M1
ORA/Mistral X-ray analysis machine from Bruker AXS Microanalysis GmbH. Please
familiarize yourself with the contents and follow the safety instructions, particularly
those regarding the handling of the product. This way you can be sure of taking full
advantage of the capabilities of the product. We reserve the right to make product
changes which enhance technical advancement.
1.2 User Information

The manual is divided up into certain sections. On each page, you can find the
section heading in the header. The footer contains the manual’s document status
with the indication of the date of issue and the page number.
Various cross-references are included in the operating instructions to ease navigation
within the document and to change to external documentation. In these cases, cross-
references include the description of the external documentation to which they refer.
The following warning symbols and informational symbols and signal words are used
in these operating instructions:
DANGER
Warning of a potential danger to life and limb
DANGER
Warning of a potential danger to life and limb from electrical current
DANGER
Warning of a potential danger to life and limb from X-ray radiation
DANGER
Warning of a potential danger to life and limb from exposure to
poison
CAUTION
Warning of possible material damage or damage to machinery
NOTE
Tips on usage and useful information
NOTE
4 / 77 Information on protecting the environment
Bruker AXS Microanalysis GmbH
Manual Karatmeter
1.3 Intended Usage

The M1 ORA/Mistral X-ray analysis machine from Bruker AXS Microanalysis GmbH
may only be used for material analysis in particular for the determination of element
composition of materials or for analysis of coating systems.
The M1 ORA/Mistral may only be operated by trained and authorized personnel in
compliance with all safety instructions covered in these operating instructions. Safe,
accurate operation can not guaranteed unless the machine is used as intended as
defined by these operating instructions.
Any other use beyond that described is considered as non-intended usage. The
operator, not the manufacturer, assumes sole liability for all personal injury and
material damage arising from not-intended usage.
The following applications are explicitly excluded from the definition of intended
usage:
• Medical and biological applications of any sort

• Radiographic applications
• Online process analytical applications in industry and research
• Analysis of aggressive chemical or radioactive substances
1.4 Guarantee and liability

The general conditions of sale and supply as passed to the operator of the M1
ORA/Mistral X-ray analysis device by Bruker AXS Microanalysis GmbH strictly apply.
Guarantee and liability claims for personnel and material damage are excluded if
they are a result of one or more of the following:
• Non-intended usage of the M1 ORA/Mistral

• Improper start-up, installation, packaging or operation of the M1 ORA/Mistral
• Structural changes to the M1 ORA/Mistral
• Operation of the M1 ORA/Mistral whilst protective housing not completed
closed or safety equipment faulty or not properly attached.
• Non-compliance of the safety regulations and instructions within this document
• Improper connection and improper cabling of the M1 ORA/Mistral and its
safety equipment
• Use of control software other than the “XSpect” software included in the
delivery
• Use of computer technology other than recommended during delivery or the
measurement computer authorized by the manufacturer.

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2. Safety Instructions
X-ray energy levels (up to 50 keV) in the excitation beam as used in the M1
ORA/Mistral cause damage to tissue and bone as a result of high levels of radiation.
Poorly healing wounds and, in extreme cases, loss of individual limbs (e.g. fingers)
could result. In contrast to “accidental radiation“ with a high dose over a short period,
there is an increased risk of cancer from a lower radiation load over a longer period.
All information pertaining to safety in this document applies to current, valid, national
laws and the Ordinance of the European Union. In other countries, applicable laws
and national regulations must be complied with.
In addition to the safety instructions in this document, general, valid, regulations
regarding accident prevention and the protection of the environment must also be
observed and complied with. All information in these operating instructions must be
followed unreservedly at all times.
In order to safely operate X-ray machines such as the M1 ORA/Mistral X-ray analysis
machine, norms, directives and regulations are defined for safety and radiation
protection. These must be adhered to by both manufacturer and users alike.
2.1 Basic safety requirements

The following basic safety requirements must be observed at any times:
• The M1 ORA/Mistral may only be used as intended.

• All safety instructions in this document and in all other applicable documents
must be observed and fulfilled.
• The device may not be operated unless the complete safety equipment, such
as the protective housing, is present and fully functional.
• Each person who is authorized to set up, install, activate or operate the M1
ORA/Mistral must have read and understood the complete manual.
• The operating instructions must be available for the staff at any time.
• Smoking, eating and drinking near the machine is not allowed.
• Operation is not allowed in case of fatigue as well as under the influence of
alcohol or drugs. The operating staff must be in good physical and psychical
condition to avoid poor concentration of judgment capability either temporarily
or permanently.
• Authorized service staff only must perform maintenance work on the M1
ORA/Mistral. Excluded are maintenance works, which have explicitly been
allowed to the user.
• Powering-on of the high voltage supply and opening of the shutter are only
possible from the “XSpect“ control software supplied as part of the delivery

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2.2 Safety requirements on the place of installation
CAUTION
The M1 Ora has a weight of approximately 24 kg and the M1
MISTRAL of approx. 46 kg. Dropping the instrument can cause
injuries or results in a complete damage of the device.
The following safety measures must be observed when installing the instrument:
• The instrument and the control computer must be placed on a stable and fixed
support. A dolly is not suitable as a measuring site.
• The measurement site should not be exposed to intensive vibrations.
• The measurement site should not be close to strong magnetic fields such as
electric motors or generators.
• In the surrounding of the measurement site, there should not be any sources
for splash water such as showers or washing sites.
• The instrument should not be exposed to aggressive media at the
measurement site.
• The installation site of the instrument should only be accessible to authorized
staff or must be monitored.
Otherwise, the parameters defined in the technical specification respectively the

installation guide apply to the installation site.
2.3 Radiation protection

DANGER
Without the manufacturer’s radiation protection measures, the X-
ray source used inside the M1 ORA/MISTRAL would cause
possible health risks
For instance, a direct exposure of the excitation beam over a period of several
seconds could cause a deep damage of biological tissue. Contrary to such a
„radiation injury“ with a high dose over a short period a lower radiation exposure over
a long period could increase the risk of cancer.
Observing the safety rules can prevent a risk of X-ray radiation for the operator due
to the measures taken by the manufacturer and the technical installations.
According to the Röntgenverordnung (RöV) – the German X-ray Ordinance - the M1
ORA/Mistral complies with a full protection system regarding its radiation protection
data and the radiation exposure of the operating staff.

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Among others, the following safety measures were taken with the construction of the
M1 ORA/Mistral:
• The X-ray source is completely encapsulated by the safety housing during

the measurement.
• The local dose rate with closed shutter in a distance of 10 cm to the
touchable surface adds up to less than 7.5 µSv/h.
• All important safety relevant functions work independently from the control
computer.
• All important safety devices are double-constructed.
• All safety circuits are wired.
• Switching on the system voltage is just possible by means of a key switch.
• Switching on the high voltage is just possible using the controlling software
„XSpect“ included in delivery.
The following basic safety rules must be observed at any time:
• It is strictly prohibited to modify or uninstall parts of the system housing or

to open the instrument.
• It is prohibited to start operations with the instrument when parts of the
housing or other components of the instrument seem to be seriously
damaged (e.g. transport accident).
• The M1 ORA/Mistral must just be operated with the control software
„XSpect “ included in delivery. Only this software guarantees the
compliance of the X-ray source operation parameters as certified
according to anti-radiation precautions.
2.4 Protection against electric current

DANGER
The mains voltage supply of 100 to 240 V and the high tensions
supply of the X-ray tube of 50 kV are perilous when bodily
contacted.
Observing the safety rules can prevent a risk of X-ray radiation for the operator due
to the measures taken and the technical installations provided by the manufacturer.
The same basic safety rules (see section 2.1) are valid both for the prevention of
damages to persons by electric current and for the prevention of damages by X-ray
radiation.
The following safety rules have to be considered additionally:
The power supply of the instrument installation site must have a ground conductor
contact.
Only the power and signal cables included in delivery have to be used for the
operation of the instrument. They must be undamaged.
Especially upon transport, the instrument must not be taken into operation unless it is
acclimatized to room temperature and no condensed water on or inside the
instrument has emerged.

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It is prohibited to take the instrument into operation if the relative humidity in the
surrounding would result in the emergence of condensed water on parts of the
instrument.
It is prohibited to take the instrument into operation if accidentally water was poured
on or ingresses into the instrument.
2.5 Staff requirements

The following requirements are made relating to the operating staff of the M1
ORA/Mistral:
• In case of fatigue as well as under the influence of alcohol or drugs an operation
is not allowed. The operating staff must be in good physical and psychical
condition to avoid poor concentration or discernment either temporarily or
permanently.
• The manufacturer must have familiarized at least one person of the operating
staff with the technical and safe application of the M1 ORA/Mistral. This
accountability is non-transferable.
• Each person who is authorized to set up, install, activate or operate the M1
ORA/Mistral must have read and understood the complete manual.
• The staff must have profound knowledge of the following operational procedures,
regulations, behavior and components:
– Operational procedures such as taking into operation and switching off the M1
ORA/Mistral.
– Safety equipment of the M1 ORA/Mistral and its correct function.
– Operational procedures during the operation of the instrument.
– Behavior and taking action in hazardous situations.
2.6 Safety equipment
DANGER
The Karatmeter must just be operated with functional safety
equipment.
Concerning the M1 ORA/Mistral, X–ray radiation with a maximum energy of 50 keV is

generated with a maximum tube rating of 50 W (refer also to the datasheet of the X-
ray tube). All possible constructive measures have been implemented to avoid X-ray
radiation hazards for the personnel.

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The M1 ORA/Mistral is fitted with the following safety equipment:

Pos. No. Safety equipment Function
1 key switch implies an operation by authorized
persons only
2 warning light „Power“ indicates that the mains voltage is
green in the keypad switched on and the instrument can be
taken into operation
3 warning light „X-ray“ current controlled display, which
yellow in the keypad indicates that the X-ray tube is switched
on and radiation is produced,
in case of failure, the high voltage is
switched off or cannot be switched on
4 primary radiation protection of housing made of 5 mm brass with a 3
the X-ray tube mm hole for limiting the beam emission
5 Shutter software controlled shutter for opening
only in case of closed instrument doors
and start of measurement
6 instrument door with door door switches connected to the safety
switches circuitry that allows opening the door for
change of the sample only if the shutter
is closed. In all other cases the HV is
switched off
7 internal safety switches interlock circuit connected with the
housing parts inside the instrument;
opening the instrument for service
purposes will lead to an interruption of
HV or even the 24V power supply
Safety equipment on the front panel of the M1 ORA/Mistral

1: Green warning light “Power on”
2: Yellow warning light “shutter open on”
3: Warning light “HV switched on”
4: Button for switching on HV

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2.7 Warning labels and name plates

Warning labels and name plates on the electronic unit
Pos.-No.. Component Function

1 front panel product name
2 front panel company logo
3 rear panel name plate of the instrument
4 rear panel name plate of the X-ray source
5 rear panel warning label HV and X-ray
6 rear panel information label fan

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3. Installation requirements
3.1 Electrical connection
Electrical Dimensioning
connection
spectrometer 100…250 V
50…60 Hz
max. 150 W
control computer and Depending on the
periphery PC
3.2 Room planning

The installation must be performed on a sustainable and vibration-free support. For
an unhampered circulation of cooling air, a minimum distance of 20 cm to the wall is
necessary.

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3.3 Environmental conditions

Environmental conditions
Room / Instrument Requirements
Optimal room temperature 22 – 28 °C
The main components have a temperature
compensation that allows working in a wide
temperature range
Working temperature range 17 – 33 °C
Relative humidity 20 - 80 %, not condensed
Heat production The instrument and the connected components
produce a lost heat of about 150 W, which is
emitted to the surrounding.
Compartment air free of corrosive fumes, no intensive dust
exposure

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4. Product description
The M1 is an energy dispersive X-ray spectrometer that can be used for elemental
analysis of bulk materials but also for coating analysis (determination of thickness
and composition).
A very special analytical task for the M1 ORA/Mistral is the analysis of jeweler alloys.
That requires a high accuracy for the analysis.
The instrument is controlled by a PC. The PC is connected only via USB to the
instrument.
The most important benefits of the instrument are:
• High count rate capability for all used detector types

• Small analyzed area due to strong collimation of the excitation beam
• Exact sample positioning with help of a video system
• Quantification with standardless model and with standard quantification
(Lucas-Tooth-model)
• Suitable for variable sample types and applications
• Low cost operating costs
The M1 ORA/Mistral is, among others, applied in the following areas:
• Quality control
• Material sciences
• Alloy analysis, especially jeweler alloys
• Coating thickness analysis

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4.1 Product versions

The M1 ORA/Mistral is available in two basic versions, which vary according to the
type of detector and sample chamber.
The M1 ORA is equipped with a prop-counter and a small sample chamber. The
prop-counter has a limited energy resolution which requires the knowledge of the
qualitative composition. Further the sensitivity of the spectrometer is relatively small
due to the bad peak-to-background ratio of prop-counters. Limits of detection are in
the range of 0.1 Wt-%. The sample chamber of M1 ORA can be small, adapted to the
analytical task.
The M1 MISTRAL is equipped also with a high resolution detector (PIN-diode or

SDD). These detectors have a significant better peak-to-background ratio and
therefore also a higher sensitivity. Limits of detection are in the range of 50 ppm.
Further this instrument every time has a large sample chamber and is equipped
typically with an X-Y-Z-stage. This stage allows automatic sample positioning.
Both types of instruments are working in air. That means that only elements with
atomic number than 22 can be measured. Characteristic radiation of lighter elements
is absorbed in air.
Different quantification models are available in dependence of the version. The M1
ORA has models for quantification of bulk samples. A standardless model is
available and for more accurate quantification also a model with standards can be
used.

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5. Technical description
5.1 Technical parameters of the M1 ORA/Mistral
The most important technical parameters of the M1 ORA/Mistral instrument versions
are given below.
REMARK
The technical parameters of the enclosed spec sheet always
apply to the respective customer instrument.
Technical parameters:
Parameter M1 ORA M1 MISTRAL

Instrument cabinet
L X W x H / mm 700 x 450 x 400 700 x 450 x 400
or only for jewellery
550 x 330 x 380
Weight 20 kg w/o PC 24 kg w/o PC

Connection values
Voltage 110 – 230 V AC 110 – 230 V AC
Frequency 50 – 60 Hz 50 – 60 Hz
Power max. 150 W max. 150 W
Connections 3 prong grounded plug P + N 3 prong grounded plug P + N

+PE +PE
according DIN 49441 according DIN 49441
Components
X-Ray tube
Manufacturer Toshiba, Petrick GmbH Toshiba, Petrick GmbH
Type Glass side window tube with Glass side window tube with
glass window glass window
Max. excitation 50 kV, 50 W 50 kV, 50 W
X-Ray optic Collimator ∅: 300 – 800 µm Collimator ∅: 300 – 800 µm

HV- power supply
Manufacturer Hitek Hitek
Type
Max. output 50 kV, 50 kV,
Input 24 V, 24 V,

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Detector
Manufacturer LND Inc Bruker axs MA
Type Prop-counter SDD
Sensitive area approx. 1000 mm² 30 mm²
Energy resolution approx. 800 eV for Mn-Ka approx. 135 eV for Mn-Ka
max. countrate 30 000 cps 100 000 cps

Signal and control electronics
Manufacturer Bruker AXS MA Bruker AXS MA
Type: Safety XGS XGS

circuitry
Type: Detector XCU XCU

control and PC
connection
Sample positioning
Stage manual Z-Stage motorized Z-Stage
Travel 120 mm 120 mm
Option motorized Z-Stage motorized X-Y-Z-stage

Travel 120 mm 150 x 150 x 80 mm
Sample view
Camera colored camera system colored camera system
Magnification approx. 20 x and 40 x approx. 20 x and 40 x
PC connection USB USB

Operation conditions
Temperature 22 – 32 °C 22 – 32 °C
Tel. humidity 20 – 80 %, not condensing 20 – 80 %, not condensing
Compartment air free of corrosive fumes free of corrosive fumes

no intensive dust exposure no intensive dust exposure

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5.2 Main components

The M1 ORA/Mistral consists of the following main components:
• Spectrometer
• Control PC
Key switch Keypad Stage switch
Connections at the spectrometer and controlling computer

At the spectrometer and the controlling computer of the M1 ORA/Mistral there are the
following connections:
Connection of the M1 ORA/Mistral
Pos Component Connection Function

1 spectrometer line connector line connection with
integrated cut out
2 control PC line connector line connection
3 spectrometer / USB instrument drive and
control PC data exchange

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6. Functional description
6.1 X-ray fluorescence
Basis of the X-ray fluorescence analysis is an excitation and relaxation process
within the atomic electron shell. In atomic physics, fluorescence is generally defined
as a two-stage process in which an atom passes into an excited status by an external
energy transfer and then passes back into the initial state on spontaneous emission
of a photon.
One characteristic of X-ray fluorescence in comparison to optical fluorescence is that
the excitation occurs with distinctly higher energies and that the emitted fluorescence
radiation lies within the X-ray range. An additionally important characteristic is that
this process is predominantly specific to elements and less specific to molecules.
X-ray fluorescence analysis is a method for the determination of the element content
in samples. Conclusions about the chemical bonds cannot be made directly this way.
X-ray fluorescence
1: ionization of an inner shell by an X-ray photon
2: refilling of the gap with an electron from a higher energy level
3: emission of an X-ray photon

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The schematic illustration in figure briefly explains the process once again.
Either a high-energetic electron, proton or X-ray photon ionizes an inner energy level,
e.g. the K-shell of an atom (see 1 in last figure).
After the ionization, a refilling of the gap (see 2 in last figure) occurs rapidly by an
electron from a higher energy level. The energy difference between the two states is
emitted as an X-ray photon (see 3 in last figure). This radiation is called X-ray
fluorescence radiation.
This instrument description just treats X-ray fluorescence, which was excited by
means of X-ray radiation. Important rules of X-ray fluorescence are:
• The possible excitation states and shell transitions are subject to the laws of
atomic physics and result in a line spectrum, which is characteristic for each
element.
• Depending on the ionized shell, the radiation is labeled K-, L- or M-radiation and,
depending on the refilling shell, an additional indication, e.g. Kα 1, 2, Kβ 1, Lα 1 etc.
describe the relative intensity of the lines and depends on the level where the
electrons are coming from.
• Fluorescence lines can just be excited with energy lines, which are higher than
the fluorescence line itself. Thus, e.g. the Au Lα -lines of about 9.5 to 13 keV can
only be excited with radiation of higher energies than the Au-L absorption edge.
Another component of radiation in case of excitation with electrons is the continuous

bremsstrahlung which is generated due to the stopping of high accelerated electrons.
Their energy than will be emitted in steps of different size as electro-magnetic
radiation i.e. a continuous radiation is emitted.
This continuous radiation is only emitted by the tube. The tube radiation, both
characteristic radiation of the tube material (for the M1 ORA/Mistral typically W) and
the bremsstrahlung excites the sample to emit only characteristic radiation.
This reduces the spectral background of the excited spectrum. Therefore tube
excited spectra have a better peak-to-background ratio and allows a better
sensitivity.
6.1 Detection of the X-ray quanta

The emitted radiation of the sample hits the detector. There it will be absorbed and
generates charges.
In the prop-counter the incident radiation ionized the Ar-atoms. Electrons and Ar-ions
are accelerated in the electrical field to the electrodes. The electrons get so many
energy that they can ionize other Ar-atoms, close to the anode wire a avalanche will
be generated and is responsible for the internal gas-magnification of this detector.
The signal is proportional to the incident energy.
In semiconductor detector also electrical charges are generated as holes and excited
electrons. These charges are collected by the electrical field. This charge than is
amplified and shaped. Because the energy for generation of a charge carrier pair is
significantly less as for Ar-atoms their number can be much higher and that gives a
better precision.

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6.1 Digitalization and channel allocation

In order to facilitate an element identification and quantification the amount of X-ray
quanta, measured by the detector must be converted into a digital spectrum (see
next figure). For this purpose, the measured energy range is divided into sections,
the so-called channels. Concerning a measured range of 20 keV and 4096 channels
one channel corresponds to an energy range of about 4.9 eV. For example, the
channel 1024 represents the energy range 5.0000 – 5.0049 keV.
Emergence of a digital X-ray spectrum
Analogue voltage pulses of

the signal electronics
Digitized values of pulse

heights
Channel allocation
Digital spectrum as
distribution of probabilities of
incident energies
calibration of the form

E = a*channel + b
e.g. a = 0.020 keV/ch

and b = -0.950 keV

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The allocation of the channel corresponding to the fitting energy range can be
executed by the software based on an energy/channel calibration.
First, the voltage pulses of the spectroscopic amplifier are digitalized in an
analogue/digital converter and then allocated to the according channels by means of
a multi-channel analyzer (MCA). As soon as a detected X-ray quantum is allocated to
a certain channel, the counter of this channel is incremented by one. The spectrum
displayed by the software, thus, shows the how many X-ray quanta were counted in
a certain energy range (channel). In the magnified section of last figure, the channel
structure of the spectrum can be recognized.
An examination of the signal processing reveals that the signal can just be processed
sequentially. But due to the fast process (a few 10 000 cps can be accumulated) it
seems that the spectrum is growing simultaneously.
X-ray quanta, which are virtually detected in parallel, are separated and excluded
from registration. The registration of an X-ray spectrum is a temporary accumulation
process, which is subject to statistical laws. It cannot be compared with a current
measurement of a voltage or a current as known from electrical engineering. Quality
of the spectrum and with it of the analytical results is strongly dependent from the
fluorescence intensity and time of measurement. Measurement times between 10
and 180 s are common.
An X-ray spectrum usually does not just contain the fluorescence lines of the sample
material but also excitation radiation, which was scattered by the sample material.
6.1 Spectroscopic resolution

The natural width of fluorescence lines is normally < 10 eV and varies insignificantly
with the type of line series (K, L, M) and the chemical bond type of the atom.
Due to different influences from the detector and signal electronics a distinct line
broadening of the fluorescence lines is visible. This effect is caused by a physically
determined error during the registration of the X-ray quanta. Mainly the thermal
detector noise and the subsequent amplification electronics, the determination of the
produced amount of space charges for each X-ray quantum is afflicted with an
additional statistical error, which automatically results in an error of the energy
determination of the X-ray quanta. Mono-energetic X-ray quanta are thus not
displayed as sharp lines in the digitalized spectrum but spread to a Gaussian-type
curve.
The most important parameter for the description of this essential detector feature is
the Full Width at Half Maximum (FWHM), which defines the peak width at the half
peak maximum. The FWHM value is mainly depending on the following parameters:
• design of the detector and the applied electronic components

• temperature of the detector
• configuration of the spectroscopic amplifier (shaping time)
• input pulse rate
• energy of the X-ray quanta

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In order to cope with the fact that FWHM values increase with energy as well as to
compare X-ray detection systems, it was agreed to use the Mn-Kα as a reference line
of the FWHM. This line is used because the radioactive isotope Fe55 emits this
radiation.
The next figure shows the fluorescence spectrum of a Mn sample and the definition
of the FWHM for a SDD.
Definition of FWHM

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6.1 Composition of a Spectrum of the M1 ORA/Mistral

The spectrum of a jeweler-alloy is displayed in next figure.
Typical composition of a XRF spectrum (Prop-counter)
The spectrum shows the following features:
1. Abscissa in the measuring unit kilo electron volts (keV) or in channel presentation
after a shift in the software
2. Fluorescence peaks of the elements Cu, Zn, Au and Ag. These peaks are emitted
from the sample. Due to the measurement with a prop-counter the energy
resolution is limited and the single peaks are not separated.
3. Peak at zero energy. The zero energy peak is not originated in the sample or the
detector but synthetically created by the electronics. It is mainly used for the
control of the electronics and for service tasks, in particular for energy calibration
and live time calculation.
4. Ordinate in the measuring unit counts (pulses) or after switching into the
measuring unit counts/seconds (cps) in the software.

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6.1 Evaluation of X-ray fluorescence spectra

Within the scope of X-ray fluorescence analysis, mainly two partial tasks are solved.
Which elements are present in the sample and what is the concentration of them
within the complete sample amount? This is commonly called element identification
and element quantification. Often, the measurement task is just restricted on the
identification of the elements.
Upon completion of the measurement, the spectrum itself is just a data set and not
yet a result. It is an iterative process of spectra correction and evaluation that leads
to the solution of an analytical task. The different steps of a spectra evaluation will be
briefly described as follows:
Procedure Spectrum
1 Spectra correction
Correction of certain detector
artifacts such as shelf
background and escape peak.
Correction of sum peaks is not
possible by the program.
2 Element identification
The X-ray fluorescence lines of
the individual elements are stored
in an atomic data library. The
identification of the elements is
normally done by an interactive
comparison of the measured
spectral lines and the measured
spectrum from the periodical
system of elements.

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Procedure Spectrum
3 Background correction
A remaining spectral
background composed of the
detector shelf and the scattered
excitation radiation has to be
subtracted from the spectrum.
The scattered part depends on
the sample itself. For heavy
samples this background is very
small (as for jeweler samples)
but for light samples it can be
more significant.
4 Deconvolution
Especially for multi-element
samples, overlaps of the
individual fluorescence peaks in
the spectrum occur because of
the line diversity and the finite
detector resolution. To allocate
the correct intensities to the
individual elements, the
spectrum must be separated
into the individual element lines
by a complex mathematical
process (deconvolution or fitting
with pure element peaks).
The result is the peak area
(intensity) for each element of
the individual not overlapped
fluorescence peaks.
5 Statistical error Sigma
For each deconvoluted δ i = N i + 2N BG
fluorescence peak the absolute
standard deviation on the basis
δi = standard deviation for the peak area
of the statistical error of the
complete peak and the Ni = net peak area fort he element i
background is calculated. NBG = background area

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Procedure Spectrum
6 Fit quality (Chi)
The fit quality is a statistical
parameter, which allows
conclusions about the quality of
the deconvolution. For all
channels the standardized
square sum of the differences
between the measured and the
calculated, deconvoluted
intensities is calculated there.
The value for the fit quality
should preferably be smaller 10.
High values (>10) are an
indication for misidentified or
non-identified elements
respectively for an inaccurate 1 n2
1
gain correction.
2
χ =
n2 − n1
∑δ
i = n1
2
(y i − y (1))2
i
7 Result calculation and output

In the result of the spectra
evaluation, i.e. finally the net
peak areas are transferred to
the quantification model.
This model calculates the
concentration of the elements in
the sample. Finally these results
are displayed and prepared for
a measurement report.

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7. Software
The program XSpect controls the complete instrument including measurement and
quantification procedure. It allows
• setting of measurement parameters like HV, tube current, measuring time etc
• control of the measuring process and accumulation of spectra
• selection of quantification procedures
• qualitative and quantitative quantification and generation of analysis reports
• preparation of quantification by measurement of pure element standards and
reference samples
• preparation of applications, their normalization and calibration
The program is Windows-based and offers high convenient handling due to graphic
user interface and intuitive handling. It is concentrated to the main function of
analysis according the main target of the instrument for quality control but it offers
also possibility for analysis of unknown sample qualities especially in the version with
a high resolution detector.
7.1 Structure
The software has the following structure
Database - contains both the database for the program itself

(atomic data for XRF, data for organization of the measurement
procedures, reference data etc) and the report templates. The
data are in XML-structure.
Drivers - contains the drivers for the instrument (USB, camera

driver etc.)
XSpect - is the main directory for all application relevant files and
the INI-file for the program.
In Application - the different applications are saved
Languages - the information for the different languages of the
program are saved
SysSpectra - the different spectra necessary for the measuring
and their quantification are saved
Work - contains information for the measurement orders

and their results
System 32 - contains all system DLL’s

Tools - contains special programs for checking the
instrument (for service and instrument setting)

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7.2 Installation of the program

Installation and up-date of the program can be done with the prepared Setup-
program Setup_XSpect.exe. This has to be started. The installation procedure then
runs automatically and all necessary files are installed.
During installation the following steps are necessary:
Start Setup.exe. The first question is for the language of the setup-wizard. The type
of installation has to be selected now (picture). The following choices are possible:
• full installation – for complete program installation

• program update – for updating the program without changing the data
As next the path of the program has to be defined:
And the icons that should be installed can be selected

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Then the installation is running automatically
After installation the PC is asking for the installation of the video-driver with the
following screen
The viewer has to be installed only for the first installation, any update don’t need the
installation of drivers.

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With <Install viewer> the installation runs automatically, after installation the wizard
can closed with <Exit>.
The complete setup procedure of the wizard has to be finished.
After finishing the installation procedure runs to load and actualize the database for
standard samples, applications, measured spectra etc. This can need a few minutes.
In case of a first installation of XSpect the installation wizards opens the programs
SVE_CHECK for setting the instrument configuration with the following screen.
Here the instrument configuration can be defined and saved to the configuration file
with <SAVE>. SVE_CHECK can be closed with the door.
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Now the program XSpect should available.
For the correct program run that the following regional settings have to be used in the
PC:

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7.3 Start of the program

The instrument can be connected via USB to any PC. The USB-controller in the
instrument has a code that requires the installation of the USB-drivers in case of
connecting the PC first time with the instrument. The PC comes up with the following
message:
Because the drivers

are on the PC it is
not necessary make
a connection to
Windows update, i.e.
use the last choice
For the installation it is necessary to define the path of the drivers. This will be asked
in the next screen
They are saved in Bruker_axs\Drivers\USB. The next question is if the installation

should be started

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With “continue installation” the installation can be started and runs automatically.
If the PC is used first time along with an instrument another drivers has to be
installed which is requested in the same way. The second driver is saved in
Bruker_axs\Drivers\USB\I386.
The PC than gives the information that the new hardware is installed and can be
used. The program is ready to start now.
If the program is started the instrument controller controls the last switch on of the
instrument. If this is longer than allowed for the tube a warm-up procedure starts
automatically i.e. tube voltage and current are enhanced slowly. In dependence of
the time out of the tube this procedure can need in between 10 and 30 min. In this
time the tube voltage reaches not the given value and the display in the status line is
red.
After the first program start it is necessary to prepare the energy calibration of the
program. For that purpose a reference measurement has to be performed. For
reference measurement the instrument has to be warmed up and needs high
temperature stability.
The first reference in the live of the instrument is used as a reference for all later
measurements. The measured spectra are saved and compared with later
measurements. Both energy calibration and intensity are compared.
The procedure of reference measurement is described in the corresponding chapter.

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7.4 Configuration files in the program structure

XSpect has several files that contain information about the configuration or the
applications. The main configuration file is:
C:\Bruker_AXS\KaratX\A1Basic.ini
It has the following structure:
Parameter in A1Basic.ini Description

(not mentioned parameters are not of
interest or their meaning is clear)
[MeasureUnit]
UnitDescription=Ora M0 Description of the unit
UnitType=0 UnitType = 0: Ora; = 1: Mistral
This is used to select the instrument
image from the same path
[Hardware]
Video=1 Flag = 0: not available; = 1: available
[Detector]
Type=2 Type = 0: PC; = 1: PIN; = 2: SDD
(setting from SVE-CHECK, see
installation)
Window_0_AtomicNumber=0 Description of absorption layers of the
Window_0_Thick=100 tube (window
[Tube]
Anode=42 Atomic number of target material
Window=14 Atomic number of window material (SiO2)
[HV]
NumbHVSettings=3 Number of fixed HV settings
HVValues=25,33,40 Values of these setting in keV
DefaultHV=2 Actual setting
DefaultCurrent=800 Setting for tube current
[Collimators]
NumbCollimators=1
Collimator0=C,300,300, 0.300 mm o
UsedCollimator=0
[Reference]
PTC= 0.0, 0.0, 0.0, Primary total counts for the 1st, 2nd 3rd HV
setting
RefROI=6.000000,28.000000 ROI for determination of PTC
EnergyCalibration=-0.96156,0.019904 Offset and gain for the instrument
Gain=1.000,1.000,1.000,1.000 Corrections of Gain, offset and intensity
Offset=0.000,0.000,0.000 for the actual HVB-setting from Reference
MeasTimeCorrection=1.00,1.00,1.00 measurement
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[XRayTube]
HighVoltage_Max=50000 Max voltage of the tube
[Report] Information about the report settings

Orientation=0
Margin Top=25, Margin_Left=25, Position of the margin
Margin_Right=25, Margin_Bottom=25
NumbLogos=2 Number of available logos
Logo_0=none,5,5,200,50 Name and position of the Logo,
Logo_1=Bruker_AXS,25,0,107,90 the logo has to be saved as *.bmp with the
ActiveLogo=1 same name as mentioned in this file in
C:\Bruker_AXS\Database\ReportTemplates
\Logos
[SpecialData]
ArchiveDirectory=C:\Bruker_AXS\Karat Directory of the archive file
X\ARCHIVE

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8. Start of operation
8.1 Installation of the instrument
For setting up and operating the instrument the directives described in section 2.2
and 3 must be observed.
8.2 Establishing the operating state

In the following, all necessary preparations, which must be performed prior to a
measurement start, will be described. In doing so, the described order must be
observed.
REMARK
Before switching on the instrument it must be assured by means
of a visual inspection that the spectrometer and the control
computer are properly connected to the mains supply and
interconnected via the data lines
CAUTION
Damage of the instrument upon condensate accumulation.
Upon transport or storage in cold environments, the instrument
must be warmed up at room temperature before switching on.
The start of operation of the instrument requires that the operator is familiar with the
measurement and evaluation software. For a detailed description of the particular
functionalities, please, refer to the following software description.
During the operation of the instrument, error messages can occur resulting from
operating errors or technical problems.
The following steps must be observed when starting the instrument:
Procedure Figure
1 Sight check of the mains supply and the
data lines of the spectrometer and the
control computer.
2 Switching on the spectrometer using the

key switch on the front panel.
The light up of the green POWER lamp on
Key switch
the keypad indicates the correct connection
with the mains supply.
Keypad with green light

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Procedure Figure
3 Switching on the control computer
using the provided key (refer to the
operating manual of the control
computer) and starting of the operating
system.
Additional local security checks of the
user or passwords of the operating
system or network are subject to the
responsibility of the user or the
corresponding administrator and will not
be executed or installed by Bruker AXS
Microanalysis GmbH.
4 Start of the measurement software.

Start with the corresponding Icon on the
desktop or via
Start >> Programs >> XSpect.
Depending on the software version and
the local installation, the access to the
measurement software can be
authorized by enquiring the user’s name
and the password.
Start >> Programs >> XSpect
5 Switch in the High voltage on the
keypad after question from the program
6 Perform a reference measurement

The reference measurement should be
done once a day after warm up of the
instrument (approx. 20 min).
Reference measurement can be started
from the start screen and has to be
performed according the displayed
comments with samples of pure Cu and
Ag.
7 Position the sample into the
instrument
The positioning is supported by the
camera image of the sample and the
cross hair in the image that displays
exactly the position and size of the spot.

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Procedure Figure
8 Selection of the application
For an analysis the correct prepared
application has to be selected from the
application list. Than the measurement can
be started with the corresponding button.
During measurement the program moves to
the spectrum display
After finish the measurement the result is
shown automatically.

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9. Program XSpect
9.1 User Interface
The program can be started with the corresponding icon from the desktop of
with Start >> Programs >> XSpect. The program starts than with the following
screen:
The main regions in the screen are as follows:

• Hardware status line: shows information about the status of the instrument
• Panels with functional buttons: change with the function in the program and
are used for the different functions in every status of the program
• Main information screen for the actual function: here all information about the
measurement are displayed (sample images, spectra, results, calibration
curves etc.)
• Software status line: for display of the measurement status
The program requires the switch on of the HV. If the HV is switched on the stability of
the instrument is improved.
The actual high voltage and tube current value are displayed in the Software status
line. The values are colored in red as long as the set value is not reached. If the set
value is reached the values are colored in light blue.

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ATTENTION
If the tube was not running for a long time the program starts
automatically a warm up procedure and enhanced HV and tube
current slowly. This can require 10 – 30 min in dependence of the
shut off time of the tube.
9.2 Start of the program

The program starts with the following screen:
The program requires for switch on the HV with the icon in the screen and with a red
lightening of the corresponding button on the keypad. The HV has to be switched on
the keypad. If HV is switched on the button on the start screen disappears and the
corresponding buttons on the instrument status line as well as that on the keypad
display this situation.
ATTENTION
The HV can be switched on only if the sample chamber door is
closed.

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9.3 Instrument Status line

The instrument status line gives an overview for the status of the instrument. The
following buttons are available:
These buttons display if the external warning bulb for

radiation is working correctly.
If the bulb is defect the Icon is grey and the tube can not
switched on. In case of no external bulb the sign shows the
correct working status.
If there is no external warning bulb the status is like a working
bulb.
These both buttons show if the sample chamber door is

opened or closed. The status is checked by the program and
the button will be changed accordingly.
The button only displays the situation but cannot open / close
the door.
These buttons display if tube high voltage is switched on or

off. The tube voltage will be switched on with the starting
procedure of the program (see last chapter).
For special reasons it can be necessary to switch the HV also

from the program directly than also these buttons can be
used.
These buttons display the status of the shutter (closed /

open). The shutter will be controlled by the program itself.
When a measurement should be started the shutter will be
opened before and if the measurement is finished the shutter
will be closed that a sample change is possible without
danger.
For special reasons it is possible to open / close the shutter
also with these buttons.

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9.4 Function panels

The function panel of the first screen offers the main functions of the program. Every
function can be opened with one of the following buttons:
Quantification by standard models (modified Lucas-Tooth) for

analysis of samples with known qualitative composition with high
accuracy
Quantification by standardless model on base of Fundamental-
Parameters with limited accuracy used mainly for unknown
samples
Service measurement of pure elements and for reference samples
for energy calibration and intensity monitoring
Setting of measurement conditions (measurement time)
Program exit
These functions are described in the following chapters.

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9.5 Service measurements

There are two different service measurements available. The selection can be done
via the following pull down menu that can be opened with the button.
9.5.1 Reference measurement

With the reference measurement the energy calibration is controlled (gain, offset)
and an intensity monitoring can be performed. This will be done with two sequential
measurements of air (O2) for 1 s and Ag for 150 s.
The reference measurement has to be performed in this sequence and starts with the
following screen.
At first a short measurement against air is required (no sample, no sample stage).
The measurement can be started with .
Than a pure Ag sample is required. If the sample is correctly positioned which can be
controlled by the sample image the measurement can be started.

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If both reference measurements are done the message box shows the following
information:
This message contains the following information:

• Gain: change of the gain in comparison to the first measurement of
reference samples (in the example 0.24 %)
• Offset: change of the offset in comparison to the first measurement of
reference samples (in the example by -0.097 channels)
• Int.corr: change of the intensity in comparison to the first measurement of
reference samples (in the example by 0.85 %)
The values of these parameters should be close to 1 (gain, intensity)
and zero (offset).
• Res (MnKa, O2Ka, AgKa): energy resolution of the mentioned elements
The value from MnKa is given because this element is used as
standard,
the value from O2 corresponds to the electronic contribution to noise,
the value from Ag is the directly measured contribution of the detector
and electronic to noise.
9.5.2 Measurement of pure elements

The spectra of pure elements are necessary for the following reasons:
• Pure elements spectra are used for the fitting the spectra of unknown sample
• The pure element intensities are used for normalization of unknown samples
For the measurement the following screen is opened:

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With the button for the PSE a periodical system can be opened and the element
of interest can be selected.
If the sample is correctly positioned the measurement can be started. The program
switches to the spectrum display. Measurement time is 300 s. At the end of the
measurement the selected element is added to the list of measured pure elements.
If the pure element spectrum is already measured with the same conditions it is
possible to load the spectrum in the Tab <Spectrum> (see chapter 9.6).
If the spectrum is loaded it is necessary to go back to the Tab <pure elements>.
Now the pure element has to be selected with help of the periodical system. With a
double click into the display for the element spectra the loaded spectrum will be
defined as the pure element spectrum.

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The excitation spectrum is required for the standardless quantification. This spectrum
can be approached by the scatter spectrum that is measured on a light matrix (for
example PMMA). This measurement can be performed also in the screen for pure
elements.
For that purpose the corresponding button has to be used. After positioning the
sample the measurement can be started. During the measurement the spectrum can
be observed after finishing the spectrum is saved automatically.
If the scatter spectrum is already measured with the same conditions it is possible to
load the spectrum in the Tab <Spectrum> (see chapter 9.6).
If the spectrum is loaded it is necessary to go back to the Tab <pure elements>.
With a click to the button the loaded spectrum will be saved as scatter
spectrum.
9.5.3 Measurement of calibration samples in the service mode

The measurement of the calibration samples can be performed with help of the
following screen:
The screen display

several information:
• list of calibration
samples
• sample image
• sample number, name,

type and source
• sample measured (spc)

- Y/N
• measurement
conditions of the
selected spectrum
All prepared standards of the database are listed in this table. For given excitation
conditions (HV, tube current) it is displayed if the sample is measured (spc: Y in
green) or not (spc: N in red).
If the sample is not yet measured it can be done immediately if the sample is
positioned in measuring position. The measurement can be started with the button

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If the sample was already measured and saved it can be loaded in the Tab
<Spectrum> (see chapter 9.6).
If the spectrum is loaded it is necessary to go back to the Tab
<CalibrationStandardSamples>. Now the Calibration sample has to be highlighted
on the table. With the button <use loaded spectrum> it can be transferred into the
table of calibration samples.
A further possibility to measure the spectrum of a calibration sample is given in the

calibration itself (see chapter 9.10.6 Calibration of an application).
9.6 Settings of the instrument

In every screen the settings for measurement and for the instrument can be changed
by using the tool box.
The tool box can be opened with the following button: The following pop menu
will be opened which allows the selection of the type of settings:
Here it is possible to select one type of settings directly – for the tube, the camera
and the measuring time. If one of the settings screen is opened the others are
available by tabs.
9.6.1 Setting of tube parameters

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Here settings of tube parameters can be set. These parameters can be changed only
for special situations. In all other situations the parameters are displayed but
deactivated.

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9.6.2 Setting for the measure spectrum
This Tab allows changes of the measuring time and the selection of the type of time
(Life and real time).
9.6.3 Video settings
Here settings for the image display are possible.

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9.7 Spectrum display and manipulation

The spectrum display is in all different functions the same and available with the tab
<Spectrum>. The spectrum display looks as follows and has the following functions:
Spectrum
load/save
PSE
Spectrum
display options
The spectrum display shows the spectrum. The abscissa can be scaled in channels
or in energy if energy calibration is available. A change is possible by a right hand
mouse click into the description of the axis of abscissa.
The status line shows

• the tube parameters
• the input and net counts of the complete spectrum
• the real and live time of the measurement
• the cursor position in channels and energy and the content of the cursor
channel

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The buttons on the right hand side have the following functionality:
Opens the following pull down menu:
The displayed functions are clear described

The spectrum can be saved ands loaded in
the *.spx-format.
In case of graphic the spectrum picture can be
saved and copy into the clipboard in several
picture-formats.
Opens the periodical system for selection of elements for peak

identification or measurement of pure elements
Opens the the following pull down menu:
Display of all spectra in logarithmic scale
Display a spectra table (see later)

Display a spectra manipulation box
Display as dots or bars
Display a grid in the spectrum screen
Display as bars or with smoothed lines
Display a legend of spectra
Display an X/Y cursor
With <Save> these settings can be

saved for the next program start

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The spectra table gives information to all displayed spectra in the following table:
The table contains the following information:

Spectra name, color of the spectrum in the display, identified elements.
The highlighted spectrum can be saved or deleted from the display.
With a click into the color box it is possible to define the properties of the spectrum
display.
Spectrum manipulation can be performed in different ways. A direct manipulation

with the keyboard:
• Energy zoom with <+> and <-> around the cursor position
• Movement of the complete spectrum on the energy scale with the left hand
mouse button on the energy scale
• Changing of the intensity scale with the left hand mouse button on the
⇑> and <⇓
intensity scale or the cursor buttons <⇑ ⇓> or with <PgUp> and
<PgDown>.
• Positioning of the cursor by clicking with the left hand mouse button in the
spectrum field or with the cursor buttons <⇒⇒> and <⇐>.
Another possibility is the use of the chart control box with the described meanings:
- scroll the spectrum in small steps

- stretch/zoom the spectrum around the cursor position
- scroll the spectrum in large steps
- go into standard presentation

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9.8 Quantification models

For quantification different models are prepared that can be selected with help of the
function buttons in the start screen.
An application summarizes all procedures that are necessary for

• preparation of an application (selection of the elements for the application,
setting of measurement conditions, measurement of standards for calibration,
normalization etc.)
• calculation of the calibration
• manipulation of applications
• selection of the application of interest
• measurement of the unknown sample and their quantification
• print of results
The following models are available:
Fundamental-Parameter model for standardless quantification which

allows the analysis of every sample, but with limited accuracy
Standard based quantification model that requires a set of standards

and which is valid for a limited sample quality but allows a high
accuracy
Analysis of coatings based on a Fundamental-Parameter model but

with improvement by standards
All models need different procedures for their application and especially for their
preparation and calibration.
The special requirements and procedures for these applications are described in the
next chapters.

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9.9 Fundamental-Parameter quantification

9.9.1 Quantification with the preset application
The standardless quantification can be selected with the following button:

The following screen will be opened that has the following functions
Quantification with standardless models delivers results with less accuracy than for
standard based models but can be used for every sample composition.
Function keys for

often used
applications
List of
applications for
selection
Function keys for

generation,
normalization,
calibration of
applications
The first application will be prepared automatically for all available pure element
spectra (measured or calculated) that are in the list of pure elements in case of first
opening this screen or after changing in the available elements.
This method also can be used for qualitative analysis because the fitting procedure
will try to fit every element to the measured spectrum. All elements with an intensity
higher than a given intensity level (deconvolution threshold) will be accepted and
identified. This deconvolution threshold can be set during preparation of an
application.

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9.9.2 Generation of a standardless application

Also for a standardless quantification it can be useful both for calculation time and
peak fitting to define the elements before the spectra evaluation.
For preparation of an application it is necessary to define
- the elements
- the excitation conditions and
- the measurement time
Definition of the
elements from PSE
(the available
elements are slightly
coloured)
Definition of excitation
parameters
Definition of the
measuring time
Definition of the
deconvolution
threshold

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9.10 Standard based quantification
The standard based quantification can be selected with the following button:
The following screen will be opened that has the following functions
Function keys for

often used
applications
List of
applications for
selection
Function keys for

generation,
normalization,
calibration of
applications
The application list contains information about

• the application (the name),
• measurement conditions (tube HV and collimator size) and
• information about the considered elements (elements of the application and
forbidden or critical elements) and about
• the status: green “A” for available, red “C” prepared for calibration and red “N”
not yet normalized
Function keys can be used for a fast selection of often used application. Up to four
functions keys (F 5 to F8) are available. The configuration of the function keys can be
Manual Karatmeter
done after highlighting an application in the list one empty function key by clicked
with the left hand mouse button. This application will be copied to the function key.
The application than can be opened also by the function key. In that case the color of
the function key and of the number of the application is colored in the same way.
An application can be deleted from a function key by using the right hand mouse
button on the function key.
The tool box for application shows the following function buttons that opens a new
screen.
Generation of an application
An application has to be prepared. For that purpose the elements
for the calibration, their concentration range and also the
measurement conditions for the application has to be defined.
Display and edit details of an application

The characteristic parameters (calibrated elements, measurement
parameters (tube, measuring time), concentration range) of an
application are displayed
Opens a window for selection between
• Normalization of an application
Ii is necessary to normalize all measured intensities of a
sample to the intensity of an infinite thick and pure element
sample. This reduces the influence of measuring conditions,
geometry etc.
• Calibration of an application
With this function an application can be calibrated i.e. a
procedure for the measurements of standards and the
calculation of calibration coefficients is offered.
Delete an application
Allows delete an application if it is not more used.
Select an application
If an application is highlighted in the list of prepared applications it
can be selected with a double click or with this button. Than the
application data are loaded and the measurement for analysis can
be started.

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9.10.1 Measurement with an application

If an application is prepared (generated, normalized and calibrated – see the
corresponding chapters) it can be used for the measurement. For that purpose the
application has to be selected from the list of applications by double click or using the
select button.
A new screen is opened that has two tabs – one for the analysis and one for the
display of the spectrum.
The screen for the analysis is displayed below. It has the following functions:
Display of the
name of the
application
Start / Stop of the

measurement
Print the report
Calculate result
Next order
Report settings
Leave the box
Settings for the

print out
Display of the actual Display of the list Sample view

measurement result of results of actual job
START of the measurement if the sample is correctly positioned
STOP during the measurement before the set measuring time is

finished
These functions are also available via the function key <F4>
The measuring conditions (excitation parameters, measuring time) are defined by the
application itself. But it is possible to reduce the measuring time by a manual stop of
the measurement.

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The result of this measurement will be displayed if the measurement is finished.

In case of Au-alloys the concentration of Au will not only displayed in Wt-% but also
in karat (1 karat = 4.17 %). The statistical error will be displayed also. This display
can be deleted with a double click into the result window.
The result of the actual job is displayed in the list of results. Here not only the results
of every measurement are displayed but also their date and time.
If there are more than two measurements also the average value and standard
deviation are displayed.
It is possible to select results of the list that should be used for average calculation
with the check box.
In case of results with a forbidden or critical element on the following message box
appears:
In that case the box can be closed and the result can be used but this can be wrong.
In case of printing a comment will be generated with information about the presence
of forbidden or critical elements.

Manual Karatmeter
The next measuring job can be opened with the next button if the actual job is
finished. This function is also available by the function key <F2>. If the next order is
started the average result of the last order is saved and can be prepared for print out.
This preparation includes the setting of the customer name, the sample name and if
necessary also of some comments in the corresponding boxes. The results of this
order are saved during the complete next order i.e. till the <Next> button will be used
again.
Setting for the print out of results is possible with the following screen that can be
opened with the tool-button .
Selection of printer
and paper format
Settings of margins
for the header
Position and size of

the logo
Selection of the logo
Title of the print out
Check box for

printing with image
The following settings are possible:

• Selection of the printer and the paper format – via windows functionality.
These settings are valid for the standard printer of the instrument. If the standards
settings are different it is possible to use special settings in the program but these
are valid only for the time of running of the program. After a new program start
these settings than has to be repeated.
• Settings of the margins for the header

The print out can handle paper with a header or print the header itself. For that
purpose three settings are necessary. The first is the setting for the margin which
reserves the size for a printed header on the paper.
Manual Karatmeter
• Position and size of a Logo

The log can be placed and adapted to the correct size of the paper
• Selection of the logo

Different logos can be prepared. The switch between the logos can be done with
the corresponding check boxes.
The logos have to be prepared in the A1Basic.ini-File as displayed in the following
structure:
[Report]
Orientation=0 Settings for the paper
Margin_Left=20 orientation, the margin
Margin_Top=20
Margin_Right=20
Margin_Bottom=40
NumbLogos=3 Number of logos
ActiveLogo=2 Number of the active logo
;; name, left, top, width, height (starts with 0,1 ..)
Logo_0=None,5,5,200,50
Logo_1=Quantum,0,0,160,50 Name of the bmp-file of
Logo_2=Bruker,0,0,160,50
Title=Certificate the logo with settings for
WithVideoImage=0 position and size
The logos have to be prepared as bmp-file with the same name as mentioned in the
INI-File and saved into the following path:
C:\Bruker_AXS\Database\ReportTemplates\Logos.
• Title of the print out

Here a title of the print out can be defined. This title is printed between logo and
result table
• Check box for image printing

With this check box it is possible to print out also the image of the measured
sample
All these settings are valid for print out till they will be changed. They are used for
print out automatically if the print out is started with the print button.

Manual Karatmeter
9.10.2 Evaluation of a loaded spectrum

It is possible to quantify also a saved spectrum. For that purpose this spectrum has
to be loaded in the spectrum display with help of the button .

If the spectrum is loaded it can be quantified in the analysis screen with the following
button . The result will be displayed in the same way like for an actual measured
spectrum.
This quantification is possible only for the given prepared quantification model i.e. for
the selected elements.
During spectra evaluation the program looks if also other elements (critical, forbidden
elements) can e found in the sample. In that case the standard quantification is not
possible and the program gives a message about the additional elements and their
approx. concentration.
In this case a standardless quantification could be helpful. This quantification can be
done with the button.

Standardless quantification is possible only once. Mean value calculation is not
performed.
The result will be shown in the box for the actual results. If there are too many
elements the result table can be scrolled.
A report can be printed for this single measurement. In this case automatically the
comment “FP result” will be implemented into the report.

Manual Karatmeter
9.10.3 Generation of an application

The generation of an application depends on the type of application. It has to be
started in any case with the button.

For bulk analysis at first the elements that should be included in the application has
to be defined. This can be done in the following screen that will be opened with the
mentioned button:
Selection of
• Name of the
application
• element type
• elements of the
application
• excitation
conditions
• measuring time
for unknown
and calibration
sample
• lower limit for
display of the
concentration
In this screen the definition of the following parameters is necessary:

• Definition of the type of the element. The different types have the following
meaning:
o Normal: elements of the application
o Forbidden: elements that are not allowed for this application, they will be
displayed separately in the result
o Critical: elements that can be available in the application but are not
considered in the calibration
• All these elements for an application can be selected from the PSE. The
sequence is displayed in the status line of the message field.
ATTENTION
The sequence of the selection is also the sequence for the application
i.e. the main element should be selected first
Selected elements are colored, the first (main) element light blue all others light
green.
The type of application and the selected elements are displayed in the sequence
of selection in the line above the software status line. This sequence is also used
for the display of the quantification result.
Manual Karatmeter
• In the top line the name of the calibration can be defined. This is possible also in
the next screens
• Excitation conditions - high voltage and current for the tube
• Measurement time for the unknown sample and for the calibration sample
• Min. concentration of other elements – if a concentration of a forbidden or critical

element in a calibration sample is less than this limit it will not displayed in the
table of calibration samples
With the tab <X-Ray data of element> it is possible to define the X-ray line that
should be used and energy ranges for the intensity integration.
As the next step the calibration standards have to be selected. This can be done with
the corresponding Tab <Select standards>.
By using this tab all standards that fulfill the requirement of this application in regards
to selected elements are loaded and displayed:

Manual Karatmeter
Display of the
available
standards
Criteria for
sorting
Help display
The standards can be listed according their number, their name or their concentration
of the main element.
The standards are displayed in green color if they are already measured, in red color
if they are not yet measured.
The concentrations are displayed for the main element in the first column, the
concentration of the other elements of the application and of additional elements if
their concentration is higher than the given limit of the first screen
The standards for the application can be selected with a double click on the standard
in the list. Than the line of the standard will be colored (light green) and transferred to
the list of <selected standards> (next tab).
This table displays the selected standards sorted for the concentration of the main
element from low to high concentrations.
If the calibration should be divided into several concentration ranges it is possible to
define the standard that should be used as concentration switch between two
concentration ranges by a double click in this table. This line of this standard will be
displayed in light green (see next picture).
If a sample is selected as a switch a table will be displayed on the right side that
shows the concentration range for the main element and the number of standards for
every concentration range.

Manual Karatmeter
After all these steps the application is prepared and can be saved with when a
name for the application is defined in the corresponding field.

Manual Karatmeter
9.10.4 Display and edit details of an application

When an application is already prepared is can be necessary to look for the
measurement conditions or even change them. For that purpose the button
can be used. This button opens the same screen as for the generation of a
application.
In that case the following parameters can be edited:

• tube current
• measuring time for unknown samples (measuring time for standards can not be
changed, because the standards are already measured for a prepared
application)
• min. concentrations for other elements
In a second screen which is the same as in the generation of the application also the
parameters of the selected elements are displayed. But they cannot be changed.
After editing the application it is possible to save these changes with the same name
of the application.

Manual Karatmeter
9.10.5 Normalization of an application

The normalization is necessary to normalize the measured intensities to the infinite
thick pure element sample.
The corresponding screen can be opened with help of the following button . It is
shown in the following picture and offers the described functions.
Display of the
pure elements
of the selected
application
Display of the
image of the
sample
Function button
for selecting
the spectrum
from the pool
Exit of the
normation
For the normalization the elements that are required for the selected application are
displayed in the table.
• It is possible to use the pure element spectrum from the pool of already measured
pure element spectra. In that case the color of the letters is changing from blue to
green. If there is no spectrum available for the element or for the measuring
conditions the letters are red.
• Another possibility is to measure the spectrum from this tab. In that case the pure
element sample has to be positioned and than the measurement can be started
with the corresponding button or with <F4>.
The box right down contain information about the requested activities.
If all pure elements and also all reference samples for the application are measured it
is possible to perform the calibration.

Manual Karatmeter
9.10.6 Calibration of an application

The calibration is necessary to make a correlation between the measured intensities
of standard samples to their known concentrations with help of the quantification
model. The calibration calculates calibration coefficients that can be used later for the
quantification of unknown samples.
The quantification will be performed with help of the following screen that has the
described areas:
Display of the
calibration curve
(analyzed against
given
concentrations)
List of elements to
calibrate
List of standard
samples
Selection of the type

of normalization of
results
Selection of the
concentration range
Button line for

calibration
Calibration of the application entails reading all the spectra from the standard
samples listed in the application, calculating the net intensities of the elements
specified in the calibration, and the performing of a regression analysis between the
concentration of the element and the net intensities of the standard spectra for each
element.
Not yet measured standards of the application are coloured in blue, all measured
standard samples are coloured in green. These not yet measured standard samples
can be measured directly from this screen. For that purpose the sample has to be
• highlighted in the list of calibration samples and positioned in the instrument
• measurement can be started with the <Start> button or <F4>
The spectrum of this sample will be saved in the database and is available now for all
other applications with this measurement condition.
If a sample could not be measured it can be deleted from the list with the right hand
mouse button. This sample than will be displayed in bold red and crossed out (see
next figure).

Manual Karatmeter
If all samples have been measured, or if the minimum required number of samples
has been measured, calibration can be performed.
This can be done with
• the calculate button for the element that is selected in the list of elements
• the Auto Calc button for all elements of the application
The result of the calibration is displayed in the calibration curve on the right hand side
and in the list of standards on the left hand side.

Manual Karatmeter
The red line in the middle of the diagram shows the expected relation between given
and analysed concentration. The points in the diagram represent the standard
samples for the selected element. Their calculated concentrations are also shown for
each sample in the table. The concentration range is only given for the main element.
If a sample does not fit the calibration i.e. one of the points is far away from the red
line in the diagram this sample can be disabled for calibration by clicking with the
right mouse button on the sample name in the table. The disabled samples will be
shown than in red colour. These samples will not used for a new calculation of the
calibration curve, just as if they had not been measured. The new calculation runs
automatically after deleting the standard.
If too many samples are taken off the calibration by this way, an error message will
appear and the Auto mode button will be disabled. In this case the calibration is not
possible.
The sigma value gives a quantification of the quality of the calibration curve. The
smaller this value the better the calibration.
The sample marked in the left hand table will be highlighted in light blue in the
diagram. You can also click on a specific point in the diagram to see which sample it
represents.
In the middle the elements of the application are listed. Clicking on one of the
element symbols shows the calibration curve for that element.
To check the calibration, all concentration ranges and all elements should be
checked carefully.

Manual Karatmeter
The complete result of the calibration can be displayed with help of the following
button .
This opens the following window that displays

• the name of the application
• the element of calibration
• the type of normalization
• the concentration range
• the calibration coefficients and
• the list of given and calculated concentrations and their difference
By changing the selected element the diagram and the result table also will change
and display the results for the selected element.
With the button it is possible to save the calibration result in the clipboard.
The result of the calibration can be saved with . This saving will be done
automatically in case of leaving the calibration screen with .

Manual Karatmeter
10. The Service program XSTools

The program XSTools is prepared for supporting the handling of
• standard samples
• applications
• backup and restore of data etc.
The program is saved in the path C:\Bruker_AXS\Tools\XSTools\XSTools.exe and

can be started from there or via Start > programs > bruker_axs > XSTools.
It starts with the following screen:
List of available functions
10.1 Managing standard samples

The instrument typically is delivered with a several applications that use standard
samples. A large set of standards is already implemented in the database. But for a
special customer it can be necessary to manage the standard samples i.E. add some
new samples or delete samples. This can be done with XSTools.
With the corresponding button in the list af available functions the following screen
can be opened:

Manual Karatmeter
List of standards
contained in the
database
Concentration of the
highlighted standard
Name, type and

deliverer of this
standard
Buttons for manage

the standard
database
With the button the highlighted standard can be deleted from the database.
With the button the next screen can be opened for setting a new standard. This
screen looks as follows:
List of the
expected elements
for this standard
type
Typing of
concentrations is
possible
Sum of
concentrations
Name, type and

deliverer of
standards
After selecting the type of the standard the expected elements are displayed. Here it
is necessary to type the concentratio0ns of every element. This is supported by the
arrow buttons and the display of the sum of all concentrations. If this sum is in the
range of 99.0 to 101.0 % the sum is green, in all other cases the sum is red.

Manual Karatmeter
After setting the name of the standard it is possible to save the standard into the
database with the button. This button is available only in case that the
concentration range is in between 99.0 and 101.0 % and the standard has a name.
After saving the database will be actualized immediately which take a few seconds.
The same procedure is running when the screen is left with the button.
10.2. Process of reference data

The data of reference measurements are saved into the log file. They give an
overview of the instrument stability. With the button it is possible to open this
function in the following screen.
Table with all

reference data
Diagram of data
Selection of the
presented
parameter set
Selection of the
number of data
sets to display
This function offers the possibility to display the results of reference measurements
and therefore also to control the condition and stability of the instrument.
All reference data are displayed in the right hand table. The number of data displayed
in the diagram can be selected in the bottom part together with the measuring
conditions (HV).
The diagram displays the distribution of the selected data set and the selected
parameter.

Manual Karatmeter
10.3 Display of log-file data

Different functions of the program XSpect are saved into a logfile. This logfile data
can be displayed with this function that is opened with the following button .
In the right hand table it is possible to select the data set(s) that should be presented
and in the left hand part these data are displayed.
10.4 Update measuring time

The saving of measurement time was changed during the development of XSpect.
That also old data can be correctly handled with new versions this function is
available. It is opened with .
After selection of the

data set of spectrum
files with the
measurement time can
be updated with the
corresponding button.

Manual M1

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What are the main components of the M1 ORA/Mistral?

What are the main components of the M1 ORA/Mistral?

What are the main functions of the XSpect software?

What are the main functions of the XSpect software?

Manual M1 ORA / M1 MISTRAL

Bruker AXS Microanalysis

MANUAL M1 ORA / M1 MISTRAL 1

2 / 77 Bruker AXS Microanalysis GmbH

10. THE SERVICE PROGRAM XSTOOLS 74

3 / 77 Bruker AXS Microanalysis GmbH

1.2 User Information

1.3 Intended Usage

• Medical and biological applications of any sort

1.4 Guarantee and liability

• Non-intended usage of the M1 ORA/Mistral

5 / 77 Bruker AXS Microanalysis GmbH

2.1 Basic safety requirements

• The M1 ORA/Mistral may only be used as intended.

6 / 77 Bruker AXS Microanalysis GmbH

2.2 Safety requirements on the place of installation

Otherwise, the parameters defined in the technical specification respectively the

2.3 Radiation protection

7 / 77 Bruker AXS Microanalysis GmbH

• The X-ray source is completely encapsulated by the safety housing during

The following basic safety rules must be observed at any time:

• It is strictly prohibited to modify or uninstall parts of the system housing or

2.4 Protection against electric current

8 / 77 Bruker AXS Microanalysis GmbH

2.5 Staff requirements

2.6 Safety equipment

Concerning the M1 ORA/Mistral, X–ray radiation with a maximum energy of 50 keV is

9 / 77 Bruker AXS Microanalysis GmbH

The M1 ORA/Mistral is fitted with the following safety equipment:

Safety equipment on the front panel of the M1 ORA/Mistral

10 / 77 Bruker AXS Microanalysis GmbH

2.7 Warning labels and name plates

Pos.-No.. Component Function

11 / 77 Bruker AXS Microanalysis GmbH

3.2 Room planning

12 / 77 Bruker AXS Microanalysis GmbH

3.3 Environmental conditions

13 / 77 Bruker AXS Microanalysis GmbH

• High count rate capability for all used detector types

The M1 ORA/Mistral is, among others, applied in the following areas:

14 / 77 Bruker AXS Microanalysis GmbH

4.1 Product versions

The M1 MISTRAL is equipped also with a high resolution detector (PIN-diode or

15 / 77 Bruker AXS Microanalysis GmbH

Parameter M1 ORA M1 MISTRAL

Weight 20 kg w/o PC 24 kg w/o PC

Connections 3 prong grounded plug P + N 3 prong grounded plug P + N

Max. excitation 50 kV, 50 W 50 kV, 50 W

X-Ray optic Collimator ∅: 300 – 800 µm Collimator ∅: 300 – 800 µm

Max. output 50 kV, 50 kV,

16 / 77 Bruker AXS Microanalysis GmbH

Type Prop-counter SDD

Sensitive area approx. 1000 mm² 30 mm²

max. countrate 30 000 cps 100 000 cps

Type: Safety XGS XGS

Type: Detector XCU XCU