5102037E - 120 - User ManualTX, TXS, TXR PDF

X-MET3000TX
Series handheld XRF analyzers

X-MET3000TX / TXS / TXR
User Manual
^~~
P.O. Box 85 (Nihtisillankuja 5)
FI-02631 ESPOO, Finland
Tel: 09 329 411
Fax: 09 3294 1300
Email: info@oxinst.fi
www.oxford-instruments.com
X-MET3000TX / TXS / TXR

User Manual
5102 037-4VE
Edition 1.20
March 2006
Safety Information
All users of this equipment must read and understand the Safety
Information (Section 6) before using the equipment.
The X-Met generates X-ray radiation when it is operating. In most

countries a license or registration is needed to use it.
Because of the radiation, the X-Met must only be used by persons who
have been trained to operate it safely.
CAUTION: This instrument produces X-rays when energised.

The X-MET3000TX generates X-ray radiation when it is operating. A red LED indicates that the X-rays
are on. The safety of the X-MET3000TX has been verified by radiation safety authorities. As long as
there is no physical damage to the instrument, there is no danger of exposure to radiation above
permissible levels when the instrument is used according to the instructions. It is important that the
distributor and user of the X-Met understand both the correct operation as well as the safety measures
that are engineered into the analyzer to prevent incorrect operation.
CAUTION: Corrosion of Beryllium

A beryllium window is used in the radiation detector inside the probe. Corrosion of beryllium may occur
if it is exposed to moisture, particularly when ions such as chlorine, sulphates, copper or iron are
present.
Corrosion may damage the detector component. In case of suspected corrosion, store the instrument
in a safe place and contact the nearest OIA representative for further instructions.
The instrument should not be used or stored in high humidity areas or in circumstances where
atmospheric condensation may occur.
CAUTION: Beryllium toxicity

Beryllium and its compounds are considered to be toxic. Overexposure is usually caused by inhalation
of a) airborne particulates resulting from grinding beryllium metal or its compounds, or b) welding
fumes containing beryllium.
Beryllium in its solid form, as it is used in the detector window, poses no health hazard.
Note: The beryllium window is very thin and thus mechanically weak. Do not grind or machine
beryllium window. Removal of corrosion products from this window should be done only by authorized
personnel.
Contents
SAFETY INFORMATION .......................................................................................................................... 3
DESCRIPTION OF THE X-MET3000TX..................................................................................................... 7
PRINCIPAL COMPONENTS OF THE X-MET 3000TX ............................................................................... 9
2.1. PRINCIPAL PARTS...........................................................................................................................................9
2.2. THE ANALYZER ...........................................................................................................................................11
2.3. THE PDA COMPUTER ..................................................................................................................................12
2.4. ENVIRONMENTAL OPERATING CONDITIONS FOR THE X-MET3000TX.........................................................13
2.5. POWER SUPPLY ............................................................................................................................................14
Battery power ................................................................................................................................................14
Line (A/C) power ...........................................................................................................................................14
Charger..........................................................................................................................................................14
2.6. HOT SURFACE ADAPTER .............................................................................................................................15
PRE-OPERATING INSTRUCTIONS.......................................................................................................... 17
3.1. PREPARING THE X-MET FOR USE ................................................................................................................17
3.2. SWITCHING BACKLIGHT ON/OFF................................................................................................................17
3.3. CALENDAR AND CLOCK ADJUSTMENT .........................................................................................................17
3.4. CHARGING THE BATTERIES ..........................................................................................................................18
3.4.1. Charging instrument batteries .............................................................................................................18
3.4.2 Charging the PDA internal battery.......................................................................................................18
3.5. BENCH TOP OPERATION ...............................................................................................................................18
3.6 TO TURN OFF THE INSTRUMENT ....................................................................................................................19
3.7. SAMPLE PREPARATION ................................................................................................................................19
ANALYSIS MEASUREMENTS................................................................................................................. 21
4.1. START UP .....................................................................................................................................................21
4.2. MAKING MEASUREMENTS ............................................................................................................................21
4.2.1. General ................................................................................................................................................21
4.2.2. Name Sample .......................................................................................................................................23
4.2.3. Select Method.......................................................................................................................................24
4.2.4. Display spectra ....................................................................................................................................26
4.2.5. Configuration Backup..........................................................................................................................27
INSTRUMENT SETTINGS........................................................................................................................ 29
5.1 GENERAL ......................................................................................................................................................29
5.2. FP METHOD SETTINGS .................................................................................................................................29
5.2.1. Set Measurement Time.........................................................................................................................29
5.2.2. Output Settings.....................................................................................................................................30
5.2.3 Test Measurement .................................................................................................................................30
5.2.4. Method Type Parameters.....................................................................................................................30
5.2.5. User Setup............................................................................................................................................35
5.2.6. Assay Screen Settings...........................................................................................................................35
5.2.7. Energy Calibration ..............................................................................................................................36
5.3. EMPIRICAL ASSAY METHOD SETTINGS .........................................................................................................37
5.3.2. Output Settings.....................................................................................................................................37
5.3.3. Test Measurement ................................................................................................................................37
5.3.5. User Setup, See Section 5.2.5...............................................................................................................39
5.3.6. Screen Settings, See Section 5.2.6........................................................................................................39
5.3.7. Method Parameters..............................................................................................................................40
5.4. IDENTIFICATION METHOD SETTINGS ............................................................................................................43
5.4.2. Output Settings.....................................................................................................................................43
5.4.3. Test Measurement ................................................................................................................................43
4
5.4.5. User Setup ........................................................................................................................................... 44

5.4.6. Screen Settings..................................................................................................................................... 44
5.4.7. Method Parameters ............................................................................................................................. 44
INSTRUMENT CALIBRATION ................................................................................................................ 47
6.1. GENERAL .................................................................................................................................................... 47
6.2. CALIBRATING WITH X-MET 3000 CALIBRATION SOFTWARE ..................................................................... 47
6.3. MSG AND FP CALIBRATION ........................................................................................................................ 47
6.4. ADDING A REFERENCE TO AN IDENTIFICATION METHOD ............................................................................. 47
6.4.1. Adding a reference sample to a predetermined identification method ................................................ 47
6.4.2. Setting screening conditions for a reference ....................................................................................... 48
6.4.3. Adding a sample to the identification library when sample type is not known.................................... 49
SAFETY INFORMATION ........................................................................................................................ 49
7.1. RADIATION SAFETY .................................................................................................................................... 49
7.1.1. Customer Responsibilities ................................................................................................................... 49
7.2. DESCRIPTION AND USE OF THE SAFETY INTERLOCKS ................................................................................... 51
7.2.1. Precautions to take when analysing Small samples ............................................................................ 52
7.2.2. Precautions to take when analyzing thin samples ............................................................................... 53
7.3. RADIATION PROTECTION DOS AND DONTS ............................................................................................... 53
7.4. RADIATION DOSE RATES ............................................................................................................................. 54
7.4.1. The intensity of the primary beam ....................................................................................................... 54
7.4.2. Scattered Radiation dose rates ............................................................................................................ 55
7.5. WHAT TO DO IN CASE OF EMERGENCIES ...................................................................................................... 57
7.5.1. Minor damage ..................................................................................................................................... 57
7.5.2. Major damage ..................................................................................................................................... 57
7.5.3. Loss or theft ......................................................................................................................................... 57
7.6. CUSTOMER MAINTENANCE ......................................................................................................................... 57
APPENDIX 1: TROUBLESHOOTING ...................................................................................................... 59
8.1. IF MEASUREMENT WILL NOT START ............................................................................................................. 59
8.2. IF THE X-MET PROGRAM LOCKS UP ........................................................................................................ 59
APPENDIX 2: X-MET3000TXS SOIL MEASUREMENTS ..................................................................... 61
9.1. DESCRIPTION OF THE X-MET3000TXS ...................................................................................................... 61
9.2 RADIATION SAFETY ...................................................................................................................................... 62
9.3 DETECTING HEAVY ELEMENTS IN SOIL ......................................................................................................... 63
9.3.1 Heavy elements..................................................................................................................................... 63
9.3.2 Typical soil remediation project........................................................................................................... 63
9.3.3 Sampling............................................................................................................................................... 64
9.4 SELECTING OPERATING MODE ...................................................................................................................... 65
9.5 MEASUREMENTS .......................................................................................................................................... 65
9.6 SAMPLE PREPARATION ................................................................................................................................. 65
9.6.1 Sample cups .......................................................................................................................................... 66
9.6.2 Sample Bags ......................................................................................................................................... 68
APPENDIX 3: X-MET3000TXR MEASUREMENT OF ELECTRONIC COMPONENTS .......................... 69
10.1 DESCRIPTION OF X-MET3000TXR............................................................................................................ 69
10.2 METHODS ................................................................................................................................................... 69
10.2.1 Auto Detect ......................................................................................................................................... 69
10.2.2 Alloy FP.............................................................................................................................................. 71
10.2.3 Plastic FP ........................................................................................................................................... 71
10.3 ANALYZING DIFFERENT MATERIALS ........................................................................................................... 71
10.3.1 Measuring time................................................................................................................................... 71
10.3.2 Non-homogeneous material................................................................................................................ 71
10.3.3 Metals ................................................................................................................................................. 72
10.3.4 Solders ............................................................................................................................................... 72
10.3.5 Plastics ............................................................................................................................................... 73
10.3.6 Printed circuit boards and semiconductor chips ................................................................................ 73
10.3.7 Powders, pellets, etc. .......................................................................................................................... 74
APPENDIX 4: ENERGIES OF K AND L LINES ........................................................................................ 75
5
Description of the X-MET3000TX

The X-MET3000TX series analyzers are portable elemental analyzers intended for various different
applications. The X-MET3000TX is primarily intended for metal alloy analysis, the X-MET3000TXS for
soil and mining analysis, and the X-MET3000TXR for electronic industry applications. The basic
configuration of all these models is the same and this manual covers operation instructions for all
these analyzers. Application specific information for use of the TXS and TXR model can be found in
the appendices.
The X-MET3000TX series analyzers are based on energy dispersive X-ray fluorescence technology
and use an X-ray tube as the source of excitation. The X-MET3000TX provides a method for chemical
analysis or sample identification (sorting) directly from samples in various forms. The instrument is a
fully portable analyzer with an integrated PDA (Personal Digital Assistant) computer. Within the XMET3000TX analysis program, the user may select analytical modes, view spectra and save data.
Figure 1.1.
Field portable configuration of X-MET3000TX
The analyzer is battery operated with A/C operation as an option. In some cases, it may be more
convenient to use the X-MET3000TX in a stationary bench top configuration. The picture below (Fig
1.2) shows the X-MET in the stand provided. There are grooves in the body and the handle which
slide into the stand. Note that for bench top operation, the instrument can be used with battery or A/C
(line voltage) power.
Figure 1.2.
Bench top installation of X-MET3000TX
Principal components of the X-MET 3000TX

2.1. Principal parts
Analyzer
Instrument stand
for bench top use
Battery charger
Battery (*2)
AC adapter
PDA computer
Included accessories:
PDA AC adapter
PDA AC adapter plug
USB Synchronisation
cable
Standard shipping
case
Stylus
Remote extension
cable for PDA
PDA display shield

set
Safety shield for

small samples
Kapton window film

kit
Shoulder strap
Protection cover
User Manual
Optional accessories: (depending on analyzer type)
Sample bag holder
Background plate
Sample cup holder
Sample bags
Sample pressing
tool
Remote trigger
cable
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Sample cups
Sample cup film
Pistol holster
Rod adapter
Weld beam adapter
2.2. The Analyzer

The excitation source in the X-MET3000TX is an X-ray tube. The standard target material is
Silver. The analyzer contains a high resolution Si-PIN diode detector with Peltier cooling.
To turn on the instrument,
turn the X-MET3000TX
interlock key to the ON
position.
Figure 2.2.1
The second lock is for

removing the palmtop
computer from the
instrument.
Figure 2.2.2
There are two indicator lights
on the analyzer:
The yellow light is always on
when the power is on.
The red light is on when
X-rays are being generated.
Figure 2.2.3
There are two (round) connection ports on
the instrument.
The one on the front is for connection to the
PDA, using the remote PDA extension cable,
during bench top operations (see Figure 1.2).
(The second port, located on the handle is for
connecting the remote trigger cable.
Figure 2.2.4
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The infrared safety sensor on the

instrument nose operates by
detecting IR reflected from the
sample surface. It is designed to
prevent accidental X-ray activation
while no sample is in place in front of
the analyzer.
Figure 2.2.5
2.3. The PDA computer

The removable PDA computer in the X-MET includes the user interface for operating the
instrument. The computer is installed in the cradle of the instrument. The display is a 320240
pixel color touch screen, which can be operated either with a fingertip or the stylus provided.
For further information about the computer refer to the HP iPAQ Pocket PC instruction guide.
The guide can be found with the CD delivered with the instrument.
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2.4. Environmental operating conditions for the X-MET3000TX

Temperature
Analyzer
-10 to 50 C
Charger
-10 to 45 C, operating
-40 to 70 C, non-operating
Humidity
Continuous operation at 20 to 95 % RH, non condensing.
The charger is designed for indoor use only.
Shock resistance
In transport and operation the instrument must not be dropped or left in exceptional
conditions, which might damage its sensitive components.
During the measurement, small vibrations may lead to inaccuracies if the vibrations
influence the detector.
Line voltage
Analyzer 90 240 V, 50 60 Hz.
PDA 100 240 V, 50 60 Hz
Charger 85 - 265 V, 47 - 63 Hz
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2.5. Power supply

Battery power
The X-MET batteries are situated inside the handle. To remove the battery, push the switch
and pull to remove the battery. Each fully charged battery will operate the X-MET for
approximately 4 hours.
Line (A/C) power

Line operation of the X-MET is possible by connecting the AC adapter to the instrument. To
do this, remove the battery and connect the AC adapter to the plug in the bottom of the
handle.
Charger
The battery charger is provided for charging X-MET batteries. To charge a battery, remove it
from the X-MET and connect the battery to the charger. Charging the X-MET batteries can
take up to 2 hours if they are fully discharged.
Note: the PDA has internal batteries. Be sure to fully charge the PDA batteries using the
iPAQ AC adapter prior to using the instrument for the first time. The PDA draws power both
from the X-MET battery and its own internal battery, but will not charge from the X-MET
battery.
14
2.6. Hot Surface Adapter
The hot surface adapter is a standard feature of the X-MET3000TX. It is designed for
measurement at hot surfaces like hot tubes or plates. The adapter lowers the heat conduction
and radiation from the hot sample to the detector. This is necessary because the detector
crystal has to be cooled and stabilized to maintain its analytical performance. However, the
heat conduction can not be prevented completely, thus there are limitations on the
measurement times. Table 1 illustrates the limitations surface temperatures with
measurement and cooling times between measurements.
Table 1
Sample Temperature
Measurement time
Cooling time between

measurements
300oC
15 s
10 min
300oC
5s
5 min
15
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Pre-operating instructions
3.1. Preparing the X-MET for use

1. Insert a fully charged battery into instrument.
2. Remove stylus from the PDA computer.
3. Unlock the PDA computer lock with the key (Figure 2.2.2).
Slide the PDA computer snugly into the cradle on the instrument. Take care to seat the PDA
on the connector correctly
4. Lock PDA computer into place.

5. Turn the X-MET power key to ON position (Figure 2.2.1). The yellow power indicator is
switched on. Wait 1-2 minutes for the peltier cooler and X-ray tube to stabilize.
6. Push PDA power switch ON.
3.2. Switching backlight ON/OFF

From the Start menu on the PDA main screen, tap Settings, then System and then
Backlight. Set the parameters according to your need.
3.3. Calendar and clock adjustment

The setting of the date and time is done from the main screen of the PDA. To change the
settings, tap the date on the screen and perform the adjustments.
If the PDA battery power has been completely discharged or the PDA has been reset, it may
be necessary to adjust the date and time settings.
17
3.4. Charging the batteries

3.4.1. Charging instrument batteries
Turn the instrument off (Section 3.7).
Remove the battery from the instrument.
Connect the charger to the battery.
The Power light on the charger is green when it
is connected to the power supply.
The Status light on the charger is amber when
the battery is charging.
When charge is complete, the Status light is
green.
3.4.2 Charging the PDA internal battery
Turn the instrument off (Section 3.7.).

Remove the PDA from the instrument by unlocking
the PDA lock with the key.
Insert the PDA adapter plug into the charging port
on the bottom of the PDA. Plug one end of the
PDA AC adapter into an electrical outlet and plug
the other end into the PDA adapter plug in the
bottom of the PDA.
The amber charge light on PDA blinks while the
battery is recharging and turns solid amber (nonblinking) when the battery is fully charged.
It is recommended that the PDA battery be completely charged before use if instrument has
not been used for several days. Battery low warning messages will be displayed when the
PDA battery charge is low.
3.5. Bench top operation

To set the instrument for bench top operation, do the following:
Place the instrument in the instrument stand provided so that the grooves in the instrument
slide into the stand. (See Figure 1.2.).
Connect the PDA to the X-MET with the remote extension cable using the port on the front of
the X-MET.
18
Turn on the instrument.
WARNING: To measure small sized samples, which dont completely cover the measuring window and /or
the infrared sensor, use the safety shield provided.
3.6 To turn off the instrument

To turn off the X-MET, exit the analysis program, turn the PDA power off and turn the X-MET
3000TX power key to OFF position.
3.7. Sample preparation

The sample surface should be clean of dust, corrosion, oil etc. The analysis is done on the
surface of the sample, so the surface must be representative of the material.
If the sample is smooth and clean (no rust, oil, dirt etc.), no sample preparation is necessary.
If the sample surface is dirty it should be cleaned. Contamination on the sample surface will
have the greatest effect on light element analysis (Ti, V, Cr). Dirt and oil can be simply
cleaned from the surface with a cloth. Rust, paint and coatings should be removed by grinding
the sample surface.
19
20
Analysis Measurements
4.1. Start up
After powering ON the X-MET (see Section 3.1) the analysis program is started from Start
menu (Figure 4.1.). Tap X-MET to start the program.
Figure 4.1. Start menu

The X-MET3000 screen (Figure 4.2.) appears with Waiting for Connection message in the
lower left corner (this may take up to 30 sec.).
Figure 4.2. Getting connected
4.2. Making measurements

4.2.1. General
The X-MET is usually delivered to the user fully calibrated. Therefore, it can be used for daily
work without any preparation other than that described in Section 3.
After start up the X-MET will go to the measurement screen (Main menu) (Figure 4.3.).
21
Via this menu the user can:

1. Select the mode of operation.
2. Make a measurement.
3. Name the sample to be measured.
4. Display the spectrum of the latest measurement.
5. Access the settings to change, for example, the measurement time.
Measurements are made by putting the nose of the analyzer on the sample (or the sample on
the nose), and pressing the trigger on the analyzer. Be sure that the infrared sensor on the
nose of the instrument is covered or the measurement will not start.
The red light indicates that the X-ray tube is generating X-rays. Make sure that you keep the
analyzer on the sample during the entire measurement. If the sample does not cover the
infrared sensor no data will be acquired. In that case release the trigger immediately and
reposition the sample to cover the sensor. The total measurement time and the elapsed
measurement time will show at the bottom of the measurement screen (figure 4.4.)
After the measurement time has elapsed, release the trigger. The calculation takes a few
seconds, depending on the selected method, sample type and grade identification. When the
measurement is completed and results are shown (Figure 4.5) a new measurement can be
started.
To hide the menus in the measurement screen tap once in the white area above the menu
boxes. To unhide the menus tap the screen again.
Note: The instrument will take 1-2 minutes to stabilize after switching the instrument power
on. During this stabilization time it is not possible to perform measurements.
WARNING: When the X-MET3000TX is operating, ensure that the sample

completely covers the aperture and IR sensor or use the small parts shield.
This prevents stray radiation from exiting the instrument.
WARNING: Never point the instrument at yourself or another person even with
a sample in place.
22
Figure 4.3.
Measurement
screen, Main menu.
Figure 4.4. Measurement

in progress.
Figure 4.5.
Measurement results
screen.
4.2.2. Name Sample

The user can give a name to the sample to be measured. If the result is saved, the name will
be also saved. To name a measurement, tap Name Sample on the main menu. This brings
you to the screen where you are prompted to input the name using the keyboard (Figure 4.6.).
If the name consists of a continuous string, a space and a number (for instance PIPE 5), the
number is automatically increased after every measurement (PIPE 6, PIPE 7 etc.).
Note: You can only name a sample before it is measured. Entering a sample Name by
tapping on the name box in the results screen will name the next sample.
Figure 4.6. Name sample.
23
4.2.3. Select Method

To select the desired method tap Select Method from the main screen. This will activate a
screen where you will find all the methods stored in the instrument memory (Figure 4.7). The
method name and type are shown. To select a method, highlight the method and tap Select
Method.
Figure 4.7. Selecting a method.

There are three method types available:
Empirical Assay.
Identification.
Fundamental Parameters.
4.2.3.1. Empirical Assay method type

Empirical Assay is an Assay & Grade method for measuring the elemental concentrations of
unknown samples. An empirical assay method is a set of calibration curves and other
parameters that calculate the concentration of a specific set of elements in an unknown
sample. It is the result of a calibration procedure. The calibration procedure assay method is
created using a set of standards which have assay values for the elements being analysed in
the unknown samples. The standards have concentrations that vary from one another and
span the range of concentrations expected in the unknown samples. Analysis of samples
outside the calibration range can result in erroneous results.
Figure 4.8. Result of an empirical assay method measurement
24
The X-MET software automatically checks to see if the analysis results are outside the
calibration range. If this occurs, the results are displayed with an arrow next to the number. If
the arrow is pointing to left, the result is below the calibration range. If it is pointing to the right,
the result exceeds the range. In either instance, the results should be reviewed before
accepting them. If the out of range indicator shows often for an analyte, it may be necessary
to recalibrate the method for the new range of concentrations.
4.2.3.2. Identification method type
Often it is not necessary to find out the actual assay values for an unknown sample, but only
necessary to identify or verify the sample grade, or proprietary alloy name. This is done by
comparing the X-ray spectrum of the unknown sample to the spectra of known samples,
which have been recorded in the memory during the calibration.
If a similar sample is stored in the reference library, the X-MET will simply give the name of
the sample as it is stored in the memory. The name can be the grade of the alloy e.g. SS 316,
or any other name under which that sample was stored. Where a positive identification is
made, the identified sample name is shown together with the note Good Match.
Figure 4.9. Result of positive identification of 2 Cr 1Mo

If the measured sample is slightly different from any reference in the memory then Possible
Match is displayed, together with the closest reference name(s). Where a Possible Match is
identified one or two reference names can be given by the instrument.
Note: The first given reference name is a closer match to the measured sample.
When the measured sample is not similar to any of the references stored in the memory, the
message No match is given.
Figure 4.10. Result of negative identification.
25
A test value called Difference shows the closeness of the measured sample to the reference
in the memory. The closer the value is to zero the more exact the measured sample and the
stored reference signatures are to each other. The threshold values between good, possible
and no match can be set during the calibration of the instrument.
4.2.3.3. Fundamental Parameters method type

Fundamental Parameters (FP) is an Assay & Grade method for measuring the elemental
concentrations of unknown samples. FP analysis provides assays based on fundamental
knowledge of X-ray physics, the detector response, and the basic spectra of a few standards.
There are three different FP methods available depending on instrument configuration.
Alloy FP provides chemical analysis of elements commonly found in alloys. The
concentration range for each element can vary from 0% up to 100%. The program normalises
the results to 100%.
Soil FP is for analysing heavy element concentrations in soil.
Plastic FP is for analysing heavy elements in plastic or other low density material.
Low concentrations of elements are not shown if their value is less than 2 standard deviations
(STD). The elements are shown in decreasing order of magnitude, thus making it easier to
read the results (Figure 4.5).
4.2.4. Display spectra

The user can view the spectrum of the latest measurement by tapping Display Spectra
(main menu). Figure 4.11 shows the screen used to plot spectral data. The data on the right
side of the spectrum shows information relating to the Cursor position in the spectrum.
Cursor Energy displays the energy value in keV. Channel is the cursors position in channels.
Count gives the number of counts at the cursors position.
Select Zoom In to view any part of the spectrum in more detail. Once an area has been
enlarged, a new area can be enlarged again. To restore to the previous scale select Zoom
Out. To restore to original settings select Fit to Window. To zoom on the Y-axis enable
Zoom on Y-Axis.
Figure 4.11. Spectral display.
26
Select XRF Line Display to place markers on the spectrum identifying the and lines for
the K and L series of the X-ray lines. To select an element, tap the element symbol (Figure
4.12.) and tap Ok to view. The markers for the selected elements will be shown as in
example Figure 4.13.
4.12. Selection of element for line identification
4.13. Spectral display XRF line markers
4.2.5. Configuration Backup

This feature backs up all files associated with calibrated methods. To start the backup
procedure, select Configuration Backup from the Main menu (Figure 4.3.) and then Store
Configuration in the menu shown in Figure 4.14.
27
4.14. Configuration Backup Settings
28
Instrument settings
5.1 General
A user can select different choices and options related to the instrument operation and data
output. To start these functions first tap Settings in the main menu. The content of the
Settings menu is different depending on the selected method type.
5.2. FP method Settings
Figure 5.1. Settings menu of a FP method

5.2.1. Set Measurement Time
The measurement time can be changed by selecting Set Measurement Time: on the
Settings menu. This brings you to the screen where you are prompted to set the time using
the keyboard (Figure 5.2). Tapping Del deletes the last character entry and tapping Clear
empties the edit field.
Figure 5.2. Measurement time setting.
If the measurement time is set to 0 (zero), the measurement time elapses until the trigger is
released. The result is updated in the screen at intervas of couples of seconds. the final result
is calculated after releasing the trigger.
29
5.2.2. Output Settings

Data produced during analysis can be stored to the PDA. To activate saving of data select
Output Settings on the Settings menu.
There are two different file formats for saving analysis results. The logfile stores the data
displayed in routine analysis in text format. The table file uses a worksheet format, and the
stored results can be processed further with Excel program.
To save results tap either Write logfile? or Write tablefile?, depending on the desired
format. The button changes to YES (results will be saved) if it was earlier NO and vice versa.
The selected value (YES/NO) is shown in bold font.
To specify the directory path and filename where the analysis results will be stored, select
Log filename: or Table filename: depending on what was selected as an output format.
Spectra of the analysis measurements can be saved by tapping the Write spectra? button.
The directory where the spectra will be stored can be changed by selecting Set spectra
directory:.
Figure 5.3. Output settings.
5.2.3 Test Measurement

The test measurement function provides a means to measure an arbitrary sample and display
the recorded X-ray spectrum on the screen. Select the desired current / voltage pair and
press the trigger to start the measurement. During the measurement the elapsed and total
measurement time is shown, as usual. After the measurement is finished the spectrum is
shown (see Section 4.2.4 Display Spectra).
5.2.4. Method Type Parameters
This screen allows the changing of various parameters related to the selected measurement
method.
30
Figure 5.4. Method type parameters of FP method.

5.2.4.1. STD Display
Standard deviation (STD) is the precision of the measurement based on the counting
statistics. To display the measurements statistical error for each analysed quantity select
STD Display ON.
5.2.4.2. Concentration
The measurement unit can be changed either to percent (%) or parts per million (ppm).
5.2.4.3. Invisible Element Correction
The X-MET3000 cannot measure the elements with a lower atomic number than Ti (22).
Those elements are called invisible elements. If their concentrations are significant, the
analysis will be distorted because of the normalization to 100%.
If the concentrations of invisible elements are known beforehand, the user can input the
values manually. If the invisible element correction is not needed, it can be switched off.
To enable invisible correction select Invisible Element Correction ON from the Method
Parameters screen (Figure 5.4).
5.2.4.4. Set Invisible Element
If the concentrations of invisible elements of the sample are known, select the Set Invisible
Elements button. The Invisible Element screen is shown, see Figure 5.5.
To choose an element select Add Element, this will open the screen shown in Figure 5.6.
Choose the element you want to add and select Ok.
To set the known concentration choose Change Element Value. Figure 5.8. shows the
added element list.
Figure 5.5. Manual input of invisible elements.
31
Figure 5.6. Adding elements.
Figure 5.7. Set concentration.
Figure 5.8. Added elements
Individually add all the elements you want to include as invisible elements. An element can be
removed by first highlighting the element and then selecting Delete Element.
When the user has manually input the concentration of invisible elements, they are used until
the input is changed.
5.2.4.5. Grade tables
On the result screen, the X-MET is able to show the grade name(s), or trade name(s) of the
measured sample. The instrument does this by comparing the assays of the measured
sample with those in a grade table. A grade table is a list of grade names with associated
upper and lower assay limits for the analytes.
Grades for the FP methods are automatically inserted in the system. The FP chooses the
appropriate grade table according to the matrix element. Matrix elements are the elements
which usually form the biggest part of the sample. For instance, low alloy steels contain
about 95% iron, the rest (5 %) being alloying elements. Thus Fe is the matrix element of low
alloy steels.
32
5.2.4.6. Grade Expansion Coefficient:

In this screen you may expand the grade identification limits. A value, which expands the
lower and upper limit of grades , is calculated from n*STD. N is a discrete value, 0,1,2,3 or 4,
and this can be changed by the user.
Figure 5.9. Grade expansion coefficient.

5.2.4.7. Grade Table Editor
To create or edit grade files in the X-MET use the built-in grade editor. To access the grade
editor, select Grade Table Editor from the Method Type Parameters screen (Figure 5.4.) and
the Select Matrix Element screen, shown in Figure 5.10, is displayed.
Figure 5.10. Select Matrix Element
An FP method chooses the right grade table according to the matrix element. Choose the
desired matrix element by tapping the element symbol. The Add/Edit/Remove Grade screen
will be displayed (Figure 5.11).
33
5.11. Grade editor, grade list screen.

All the existing grade names for the selected matrix element will be listed. There may not be
any grade names if a grade table for the selected matrix element has not yet been created.
To add a new grade, tap Add. The user is prompted to give a name to the grade (see Figure
5.12). The name can have a maximum of 15 characters. Tapping Remove deletes the
highlighted grade. The deletion is confirmed before the actual operation.
5.12. Edit New Grade Name screen

To edit the grade, highlight the grade name and tap Edit (Figure 5.11). A screen (Figure
5.13.), with element list and with lowest and highest allowed concentrations, is shown. To add
a new element, tap New Element. To remove a highlighted element, tap Remove Element.
To edit lowest and / or highest allowed concentrations, tap the current value and a screen
(Figure 5.14.) is shown where new values can be entered.
34
5.13. Grade editor, editing grade
5.14. Editing concentration limits
5.2.5. User Setup

Access to the X-MET instrument functions is categorized by three levels. Access to a level
may be protected with a password. The user mode that is currently in use is highlighted.
Normal User Lowest level where functions related to making measurements and data
storing are available.
Supervisor Medium level which allows calibration of the instrument. This level is protected
by a password.
Service Highest level which is used only by service personnel. This level is protected by a
password.
In supervisor mode, the password of this level can be changed by tapping Change
password.
Figure 5.15. User setup.
5.2.6. Assay Screen Settings

To change the font size and the scrollbar size, go to Assay Screen Settings.
35
Figure 5.16. Screen settings.
5.2.7. Energy Calibration

In this screen the user can perform an energy calibration measurement. This is done by
measuring the DUPLEX 2205 sample supplied with the instrument. To do the energy
calibration measurement, place the sample in front of the analyzer and press the trigger. After
the measurement is finished, release the trigger. If you do not wish to perform this
measurement you may exit this screen by tapping Skip Measurement.
Figure 5.17. Energy calibration

Note: The instrument needs about a 2 minutes warming up period after switching the
instrument power on before it is ready for making measurements.
36
5.3. Empirical assay method Settings
Figure 5.18. Settings menu of empirical assay method

The measurement time can be changed by selecting Set Measurement Time: on the
released. The result is updated in the screen at approximately two (2) second intervals
(Figure 5.19). The final result is calculated after releasing the trigger.
Figure 5.19. Updating screen during measurement

See Section 5.2.2.
5.3.3. Test Measurement
See Section 5.2.3.
37

method.
Figure 5.20. Method type parameters of empirical assay method
5.3.4.1. Standard Deviation

See Section 5.2.4.1.
5.3.4.2. Distance Scaling

If distance scaling is enabled, the analysis is automatically corrected for irregular shape of the
sample and for distance changes between the sample and the analyzer.
The distance scaling works by identifying the sample and scaling the measured spectrum to a
similar spectrum in the memory. If the sample is not identified, a warning is shown (Figure
5.21).
Figure 5.21. Distance scaling failed

In this case, there is no matching reference in the spectrum library of the method. However,
the user can add typical samples to the identification library for distance scaling. The sample
to be used for scaling must be even and cover the whole measurement window of the
instrument. Adding samples to a method is described in the Section 6.4.
38
5.3.4.3. Edit Grades

On the result screen, the X-MET is able to show the grade name(s), or trade name(s) of the
measured sample. The instrument does this by comparing the assays of the measured
sample with those in a grade table. A grade table is a list of grade names with associated
upper and lower assay limits for the analytes.
Grades for empirical assay methods are always associated with predefined assay methods.
Thus the X-MET automatically uses a correct table to look for grades.
To create or edit grade files in the X-MET use the built-in grade editor. To access the grade
editor, select Edit Grades from the Method Type Parameters screen (Figure 5.20.) and a
screen, as shown in Figure 5.11, is displayed.
All the existing grade names for the selected matrix element will be listed. There may not be
any grade names if a grade table for the selected matrix element has not been yet created.
To add a new grade, tap Add. The user is prompted to give a name to the grade (Figure
5.12). The name can have a maximum of 15 characters.
Tapping Remove deletes the highlighted grade. The deletion is confirmed before the actual
operation.
To edit the grade, highlight the grade name and tap Edit (Figure 5.11). A screen (Figure
5.13) with element list and with lowest and highest allowed concentrations is shown. To add a
new element, tap New Element. To remove a highlighted element, tap Remove Element.
To edit lowest and / or highest allowed concentrations, tap the current value and a screen
(Figure 5.14.) is shown where new values can be entered.
5.3.4.4. Display spectral ID

To display the method and reference used in the distance scaling, change Display spectral ID
to YES.
Figure 5.22. Displaying method and reference used for distance scaling
5.3.5. User Setup, See Section 5.2.5.

5.3.6. Screen Settings, See Section 5.2.6.
39
5.3.7. Method Parameters
Figure 5.23. Method parameters menu of an empirical assay method

The Method parameters menu offers three functions for the maintenance of calibrated
empirical assay methods. These features help to insure accurate method analysis over time
while minimising the need for frequent recalibration. This chapter describes the features and
their use.
5.3.7.1. Single Point Recalibration

Single point recalibration is a method to correct the results for a selected material type only. It
is useful when the user has to make an accurate analysis within narrow concentration ranges.
Be careful when using this feature, because the correction is only valid for samples
close in concentrations to the specific (reference) sample.
To perform a single point recalibration, go to Single point recalibration. A screen similar to
that shown in Figure 5.24 will be displayed. Highlight the analyte you want to correct and
press Set concentration. Enter the concentration. Then place the reference sample against
the measurement window of the instrument and pull the trigger to start the measurement.
If the single point calibration is no longer needed, you can reset the single point recalibration
by pressing Reset.
Figure 5.24. Single Point Recalibration
40
5.3.7.2. Check Sample Measurement

The function of the check sample is to provide a reference point during calibration that can be
used later for updating calibration equations. This applies to empirical assay methods only.
During calibration, a sample is measured and stored as a check sample. This sample is
representative of the standards used in the calibration. When the sample is measured, the
assay values and standard deviations are stored along with the calibrated method. This sets a
reference point for the performance of the calibration equation.
At any time, the same sample can be measured using the Check sample option. This displays
the screen shown in Figure 5.25.
Figure 5.25. Measurement of check sample.

Place the check sample against the measurement window and pull the trigger to start the
measurement. After the measurement is completed the analysis results are displayed (Figure
5.25.). The first column shows the analyte. Original assay values from the analysis during
calibration are shown in the second column. The third column is the assay value from the
present analysis. Column four shows the difference between the two values.
Figure 5.26. Results of check sample analysis.

If the difference is less than three standard deviations, it is assumed that there is no statistical
difference between the measurements. Thus no update is recommended. In this instance, the
Cancel button should be pressed.
41
If the difference between the two measurements of an analyte is more than three standard
deviations, the deviating analyte is marked with yellow colour. In this instance, using the
check sample results to update the calibration curve is recommended. To update the
calibration simply press the Save button. The intercept of the calibration equation will be
adjusted so the new analysis will correspond with the original.
If the difference between the two values is more than ten standard deviations, the following
warning is displayed Check to see if sample is correct. Press the Cancel button and check
the following before updating the calibration:
1) Check that the sample currently being analysed is the sample used for the original check
sample measurement.
2) Make sure that the sample is stable over time and has not changed in composition since
the original analysis.
3) Insure that the sample has been properly placed against the measurement window.
If all these conditions have been met, then re-measure the sample and update the calibration
if necessary.
5.3.7.3. Analyte Correction

Correction of the calibration equation (of an empirical assay method) with the check sample
creates a coefficient that is applied to the calibrations curve intercept value. The Analyte
correction option shows the correction coefficient and allows for it to be manually changed.
Figure 5.27 shows the correction coefficients. To enter a manual correction coefficient,
highlight the element to be changed then press the Change Offset button. A dialogue box
opens and the new value can be entered. When the Ok button is pressed, the new value will
be used to update the calibration equation.
Figure 5.27. Analyte Correction
42
5.4. Identification method Settings
Figure 5.28.
The measurement time can be changed by activating Set Measurement Time on the
released. The result is updated in the screen at approximately 2 second intervals (see Figure
5.19.) The final result is calculated after releasing the trigger.

See Section 5.2.2.
5.4.3. Test Measurement

See Section 5.2.3.

method.
43
Figure 5.29. Method type parameters of an identification method

5.4.4.1. Difference Display
A test value called Difference shows the closeness of the measured sample to the reference
in the memory. The closer the value is to zero the more exact the measured sample and the
stored reference signatures are to each other. The threshold values between good, possible
and no match can be set during the calibration of the instrument.
To display the measurements difference value, change Difference Display to YES.
5.4.4.2. Confirm Possible Match / Confirm No Match
A user may be prompted to confirm a Possible Match or No Match by selecting Yes for the
corresponding option. A pop-up message box is displayed (see example Figure 5.30).
Figure 5.30. Confirmation box of No Match

5.4.4.3. Display Screening Path
Change the Display Screening Path to YES, to display the intermediate results of the
screening chain, not only the final result.
5.4.5. User Setup

See Section 5.2.5.
5.4.6. Screen Settings

See Section 5.2.6.
5.4.7. Method Parameters
44
Figure 5.31. Identification method parameters

The thresholds options define the limits for Good, Possible or No Match. If the difference
between the measured sample and the reference sample, that best matches the measured
sample, is below the fine threshold value, it is considered to be a good match. If the difference
is between the fine and coarse threshold values, it is a possible match. If the difference is
greater than the coarse threshold value, there is no match. To change the threshold value,
select the button and enter a new value.
If No Match is reported for a measurement, the result may be recalculated using a different
method. Select Recalculation Method and select the method you wish to use for
recalculation, from the list.
45
46
Instrument calibration
6.1. General
In order to give accurate results the X-MET needs to be carefully calibrated for all the sample
types to be measured. Although the instrument is often delivered fully calibrated, complete
software tools for user calibration are available.
6.2. Calibrating with X-MET 3000 Calibration Software
The empirical assay methods and the identification method are created with X-MET 3000
Calibration Software, which runs on an external PC. For further information about this
software refer to the X-MET 3000 Calibration Manual.
6.3. MSG and FP calibration

Both MSG (Metal Standard Generation) and FP calibration software can be accessed from
the Calibration button on the Main Menu (Figure 4.3). These calibrations are usually
provided when the instrument is delivered and in general the user does not need to create
these. For further information about this software refer to X-MET 3000 Calibration Manual.
6.4. Adding a reference to an Identification method

A user can perform the most commonly used operations for the identifications, directly in the
PDA program.
The user can add a new reference for an Identification method simply by making a sample
measurement, and instructing the X-MET to store the measured spectrum.
6.4.1. Adding a reference sample to a predetermined identification method
The user can add samples to any identification method calibrated into the X-MET by
proceeding as follows:
Select the method by tapping Select Method in the Main Menu (Figure 4.3). Choose the
identification method according to the sample type you are about to add. For example if you
have a Stainless steel sample, then highlight the SS ID method and tap Select Method.
Choose Settings in the Main Menu and then Method Parameters. Select Reference
Maintenance at the bottom of the screen (Figure 5.31). This will bring a new menu onto the
screen (Figure 6.1), with a list of all the references stored in the selected method. A date next
to the sample name indicates that the reference is measured and has a spectrum in the
identification library.
47
Figure 6.1. Adding a reference into memory

Tap the Add Sample button and type in the desired sample name for the sample to be
added (Figure 6.2) Tap the OK button. Make sure that the new sample name is highlighted
on the sample list. Place the sample on the analyzer and pull the trigger to start the
measurement. Keep the analyzer on the sample during the entire measurement time. After
the measurement is complete the sample name and its spectrum are stored in the memory.
Figure 6.2. Defining standard name

Note: When storing references you should use a measurement time long enough to
collect a well-defined spectrum (60 120 seconds).
The sample is now added to the selected X-MET identification library.
6.4.2. Setting screening conditions for a reference

Screening means instruction to the X-MET to use another method to re-calculate the result, if
the reference in question has been identified. The reason for this may be that more accurate
identification or concentration analysis is needed.
Note: Screening happens only if the result from the identification is Good match.
To define the screening method for a reference, press the Set Screening Method in the
Reference Maintenance menu (Figure 6.1.). This will bring a menu on the screen, which
shows all the calibrations in the X-MET memory. Scroll to move the cursor to the method you
wish to use. Tap the Select button to select the method.
48
6.4.3. Adding a sample to the identification library when sample type is not known
If the exact type of a sample is not known, it is not possible to allocate it to a predetermined
identification method. However, the user may allow the X-MET to deduce the general sample
type and target method.
First select the general identification calibration from the Select Method menu. Then make a
measurement as usual. The X-MET will now first try to identify the sample type and will switch
directly into the most likely calibration method. Select this as the target method on the Select
Method screen, and add the reference into the target method as described in Section 6.4.1.
Safety Information
You MUST:
Read and understand this entire safety section.
Contact the appropriate regulatory authority to determine what is needed (see
Customer Responsibilities 7.1.1)
Have received training in the safe operation of the X-Met (see Customer
Responsibilities 7.1.1).
Complete a risk assessment for the safe operation of the X-Met (Refer to 7.4 for dose
rates).
Maintain a list of authorized users.

Check correct functioning of analyzer once a month. See Customer Responsibilities
7.1.1 and Customer Maintenance 7.6).
7.1. Radiation Safety
The X-Met3000TX series must only be used by persons who have been
trained to operate the probe safely.
Do not point the instrument at any person when it is in operation.
Users must not try to gain access to the radiation enclosure.
Servicing must only be carried out by engineers trained by Oxford Instruments.
7.1.1. Customer Responsibilities
Contact the appropriate regulatory authority to determine if registration or licensing

requirements apply: For example, in the United Kingdom, equipment of this type is
defined as a radiation generator, and its use is governed by the Ionising Radiation
Regulations 1999 (IRR99); the Health and Safety at Work etc. Act 1974 (HSAW);
the Management of Health and Safety at work Regulations 1999 and the Provision
and Use of Work Equipment Regulations 1998. Users must notify the Health and
Safety Executive (HSE) of their intention to work with ionising radiation. (Notification
is only done once, or when an employer makes a material change to their work that
would affect the particulars of the original notification. If the employer has already
notified the HSE, further notification following the purchase of a 3000TX is not
required).
Help and advice is available from the HSE infoline on telephone number 0845 345
0055. The HSE require 28 days notice. There is a requirement to appoint a Radiation
Protection Advisor (RPA). The RPA will help specify work procedures to be followed
including training requirements for the correct use of the equipment.
49
Test the device for correct operation of the ON/OFF mechanism every six months and keep a
record of the test results. If the instrument fails the test, contact an OIA representative
immediately for instructions and return the instrument for repair.
Maintain a record of the instrument use and any service to shielding and/or containment
mechanisms for two years or until the ownership of the instrument is transferred or the
instrument is decommissioned.
Report to appropriate authority any possible damage to shielding and any loss or theft of the
instrument.
Transfer or loan the instrument only to persons specifically authorized to receive it, and report
any transfer to the appropriate regulatory authority, normally 15 to 30 days following the
purchase, if required.
Report the transfer of the instrument to an appropriate OIA representative.
Comply with all instructions and labels provided with the instrument and do not remove labels.
Removal of labels will void the warranty.
Do not abandon the instrument.
50
7.2. Description and use of the safety interlocks

The X-MET3000TX has been designed with a failsafe safety circuit to prevent inadvertent
exposure of the operator to the X-ray beam. The safety system for the instrument consists of
three failsafe lights, a key lock, a trigger to activate X-rays, and an infrared sensor. The
function of each safety feature is described below:
Primary power safety keylock
A key lock is employed to control power

to all components. The key lock must be
turned on before any actions can be
initiated.
NOTE: Remove the key from the
analyzer when not in operation to
prevent unauthorised use.
Yellow, High voltage on, failsafe warning light
When the key lock is turned on, the

yellow light will be activated to
indicate there is voltage to the power
supply. If the bulb has failed or has
been removed, the safety circuit will
not permit application voltage.
Operator trigger interlock When the trigger is pulled, X-rays are generated if the following
conditions are met:
Infrared beam safety sensor
The infrared beam safety

sensor, located at the
nose of the instrument, will
not permit X-rays to be
generated unless a solid
object covers the infrared
beam.
51
Dual red X-ray on failsafe warning light
When the trigger is pulled and

the infrared sensor is engaged,
the red lights will be activated
indicating the generation of Xrays. If one or both of the red
LEDs are burned out, X-rays will
not be generated.
Do not point the instrument at any person when the probe is

activated. Note that the form of the primary beam is a narrow cone that points obliquely to
the left, not directly forwards. The radiation intensity is high in the primary beam and therefore
no part of the body should be exposed to that radiation. While measuring, make sure that the
instrument is in contact with the sample and that the whole measurement window and infrared
sensor are covered by the sample. In cases where the sample doesnt cover the whole
measurement window use the safety shield for small samples. Thin samples may allow higher
exposure; see 7.2.1.
7.2.1. Precautions to take when analysing Small samples

Small samples that do not cover the measurement window entirely are quite obviously
potentially risky to measure because part of the primary radiation may go through the sample
un-attenuated. To eliminate the risk the protective safety shield for small samples is provided
to cover the sample entirely.
Protective safety
shield for small
sample
measurement.
52
7.2.2. Precautions to take when analyzing thin samples

A less obvious risk to radiation exposure is caused by the measurement of thin samples. Part
of the radiation coming from the X-ray tube is so high energy that it penetrates thin samples,
especially if they are of low atomic number material. The following table gives the relative
intensities after the radiation has gone through aluminum / iron sheets of various thicknesses.
(The tube is run at 40 kV, 2A).
Aluminium sheet
Relative intensity
Iron sheet
Relative intensity
0 mm
1 mm
2 mm
3 mm
4 mm
5 mm
10 mm
100
55
36
26
19
15
5
0.0 mm
0.1 mm
0.2 mm
0.3 mm
0.4 mm
0.5 mm
1.0 mm
100
31
15
8
5
3
0,4
NOTE: If the sample is unable to stop the primary radiation the dose rate may be high behind
the sample. An aluminum sample must be quite thick before it absorbs most of the radiation
whereas iron provides much better shielding. In practice the difference is important and
means that it is wise to measure aluminum samples at arms length.
7.3. Radiation Protection DOs and DONTs

DO
Read and understand the safety information
(Section 7)
DONT
Override the safety features
Follow any instructions given

Store the key away from the analyzer when
not in operation to prevent unauthorized use.
Point the analyzer at any person or animal

Leave the key with the analyzer when not in
use
Store the analyzer in a safe location when not

in use.
Keep control over who is authorized to use
the device.
Leave the analyzer unattended if not safely

stored away.
Allow people into the beam path and train
users in managing this risk.
53
7.4. Radiation Dose Rates

7.4.1. The intensity of the primary beam
The following table reveals the intensity of the primary beam when the infrared sensor is
intentionally bypassed and no sample is placed in front of the probe. It gives the time that
hands may be kept in the beam at different distances from the probe window without
exceeding the limit given by the law. The limit for a radiation worker is 500 mSv per year and
if we assume that the person works for a 50 weeks a year the weekly dose is 10 mSv /a. The
distance is calculated from the window, but the tube is actually about 3 cm from the window.
Reduce exposure by maintaining the maximum possible distance from the radiation source to
the operator or member of the public. Exposure rate is reduced as the distance from the
source is increased. The greater the distance, the less amount of radiation received. Doubling
the distance from a point source reduces the dose rate (intensity) to 1/4 of the original.
Tripling the distance reduces the dose rate to 1/9 of its original value.
Distance (cm)
Time per year
Time per week
100
50
25
10
5
0
1300 h
344 h
96 h
20 h
7h
1h
26 h
6 h 53 min
1 h 55 min
25 min
9 min
1 min
Although occasional accidental bypassing remains within permissible levels careless

handling of the instrument may cause overdoses. Looking at the distances the doses in this
case are most likely obtained by the user himself.
54
Primary beam direction if the safety logic circuit is bypassed
7.4.2. Scattered Radiation dose rates

Measurements taken at 10cm from analyzer with analyzer pressed against a sample.
Operating current 3.1A. (1Sv = 100rem).
55
Position
Sv/hr
Position
Sv/hr
0.07
0.07
0.07
0.06
0.04
10
0.05
0.05
11
0.05
0.05
12
0.06
0.06
13
0.05
0.07
56
7.5. What to do In case of emergencies

The X-ray emission from the instrument could be harmful to a person if they operate the
analyzer without the appropriate training. If the instrument is lost or stolen, notify the local
and/or state regulatory agency as soon as possible.
The first action to take in the event of an accident with instrument is to

turn off the device and remove the battery pack.
7.5.1. Minor damage

If any hardware item appears to be damaged, even if the system remains operable, contact
your nearest OIA representative immediately. Use of a damaged analyzer may lead to
unnecessary radiation exposure and/or inaccurate measurements.
7.5.2. Major damage
If the analyzer is severely damaged, contact an OIA representative immediately and the
appropriate regulatory agency in your state or country. Care must be taken to ensure that
personnel near the device are not exposed to unshielded X-rays that may be generated.
Removal of battery pack will stop all X-ray production.
7.5.3. Loss or theft
Notify the appropriate regulatory agency in the country or state in which the device is being
utilized. In addition, contact your nearest OIA representative immediately in case of a stolen
device.
Take the following precautions to minimize the chance of loss or theft:
Never leave the analyzer unattended when in use.
When not in use, always keep the device in its shipping container and store it in a locked
vehicle or in a secured area.
Keep the key separate from the analyzer.
Maintain records to keep track of all instruments, and the operators assigned to use them and
where they were used.
7.6. Customer Maintenance

Establish a routine for checking the correct functioning of the infrared beam safety sensor,
located at the nose of the analyzer: Measure a sample in the normal way but pull away from
the sample during the measurement. The measurement will immediately cease as the safety
beam is uncovered. Do this once a month to check that x-ray emission does indeed cease
unless a solid object covers the infrared beam.
Similar rules apply in other countries. Users should contact their local Oxford Instruments
representative for specific advice.
57
58
Appendix 1: Troubleshooting
8.1. If measurement will not start

A1. If the X-MET program is started before the instrument power is turned on the program
cannot communicate with the instrument.
1. Exit the X-MET program and turn off the instrument power.
2. Take the PDA out of the instrument and press the reset button at the back of the PDA.
3. Remount the PDA onto the instrument.
4. Make sure the instrument power is switched ON before starting the X-MET program.
A2. If the infrared sensor is not covered the measurement will not start.
Make sure that the infrared sensor is covered completely.
A3. The sample surface may be too darkly coloured to reflect light to activate the infrared
sensor.
Insert a piece of white paper between the sample and the infrared sensor.
A4. The battery is discharged and yellow light is not on or yellow light is blinking.
Is the yellow light on? If it isnt or it is blinking change the battery or connect the
instrument to the AC adaptor.
Note! Yellow light will become dim when battery is low.
A5. There is no communication between the PDA and the instrument.

PDA not seated properly. Exit the analysis program, remove the PDA and re-seat it on the
connector assuring that it is firmly seated. Restart the program and try again.
8.2. If the X-MET program locks up

If other programs are running the X-MET program may lock up. Closing other
programs frees system memory for other tasks.
1. Go to the Start menu and tap Settings.
2. Tap the System tab.
3. Tap the Memory icon and tap Running Programs and then tap Stop All.
59
60
Appendix 2: X-MET3000TXS Soil measurements

9.1. Description of the X-MET3000TXS
The X-MET3000TXS is a portable, elemental analyzer with an integrated PDA (Personal
Digital Assistant) computer. It is based on energy dispersive X-ray fluorescence technology. It
uses an X-ray tube as the source of excitation and a Peltier cooled Si-PIN detector.
The X-MET3000TXS provides a method for the chemical analysis of soil. Besides heavy
elements measurements in soil X-MET3000TXS can also be used for mining applications
where applicable.
Field portable x-ray fluorescence is an exemplary field method offering rapid, cost-effective
screening of heavy metals in soil. Measurements can be done either in the field (direct
measurements from the soil or bagged soil measurements) or in the laboratory (prepared
samples in the sample cups). Even in instances where laboratory analysis is required, field
XRF can be used to rapidly pre-screen samples to obtain the optimum efficiency from the
laboratory sampling effort. Since XRF analysis does not destroy the sample, any sample
collected and measured in the field can be retained for verification by a laboratory.
The instrument is delivered to the customer with a Fundamental Parameter analysis program
for soils. An Empirical soil calibration, with a factory soil sample set, is available as an option.
By aid of a special calibration program, customized empirical calibration models can be
created for an analyzer.
The analyzer is battery operated with A/C operation as an option. In some instances, it may
be more convenient to use the X-MET3000TXS in a stationary bench top configuration. The
picture below shows the X-MET in the stand provided. There are grooves in the body and the
handle, which slide into the stand. Note that for bench top operation, the instrument can be
used with battery or A/C (line voltage) power.
Figure 9.1
Bench top installation of
X-MET3000TXS with safety
shield for sample bag
measurements.
61
9.2 Radiation safety

Please read thoroughly the radiation safety section in the XMET3000TX Users Manual. In
addition, the following safety measures should be taken into consideration when analyzing
soil type samples:
Note: When measuring light matrix samples (for example, soil or sediment) they must not be
held on the analyzer measurement nose by hand.
A Radiation safety shield, either for plastic bag measurements (see Figure 9.2) or for sample
cup measurements (see Figure 9.3) or the background plate (see Figure 9.4) should always
be used, not only to avoid radiation health risks but also to make a measurement background
constant.
9.2 Safety shield

for sample bag
measurements
9.3 Safety shield for

sample cup
measurements (option)
9.4 Background plate
It should be noted also that the analyzer must be kept at right angles against the sample to
minimize the scattering radiation (see Figures 9.5 and 9.6).
9.5 Correct analyzer position
62
9.6 Incorrect analyzer position
9.3 Detecting heavy elements in soil

9.3.1 Heavy elements
Heavy elements are normally considered as an element with density 4 5 g/cm3 and higher.
Based on this definition all elements heavier than titanium (Ti) are heavy elements. However,
normally only poisonous heavy elements are considered: arsenic (As), cadmium (Cd),
chromium (Cr), copper (Cu), mercury (Hg), vanadinium (V), nickel (Ni), lead (Pb) and zinc
(Zn). Some of the metals like Cu and Zn are poisonous only in high concentrations and they
exist in normal, not contaminated soil as well.
Most often the heavy elements originate from industry, for instance from waste burning plants
(Cd, Hg), shooting tracks (Pb), mining (Cd, Cu, Ni, Zn), traffic (Pb) and fertilizers (Pc, Cd, Hg).
Heavy elements cause harm both to human health and to the environment. Humans can be
exposed to heavy elements by food plants, water and air. In the human body they concentrate
into the liver and kidneys. In nature, heavy elements may cause harm to soil microbes and
bacteria and they also can damage the vegetation.
In different countries there are determined accepted concentration levels (reference value,
target value, guideline value, soil quality criteria) for heavy elements. Levels are determined
based on use of the land. Typical classification is for example: 1) play grounds, 2) residential
areas, 3) parks, 4) industrial areas. Concentration levels and their classification may vary
significantly from one country to another.
9.3.2 Typical soil remediation project
Depending on the goals of a remediation project an exact research plan needs to be done by
the project management. At the very beginning of the project polluting elements need to be
identified so that the actions of the project can be defined. Also, as soon as possible, a
pollution degree needs to be defined on the contaminated area.
It is very expensive to move contaminated soil from one place to another. Because of that
sometimes soil removing can be avoided by more profitable but slower actions: for example,
trees can be planted on a contaminated area to take care of remediation they can absorb
the polluting elements from the soil through their roots.
A Research plan includes as a minimum the following issues:
-
all participants involved
the target of the research plan: are we doing preliminary study just to check if the site is
probably polluted or probably clean or are we finding hot spots of the area or are we
checking the border outlines for polluted area?
background information of an area i.e. all available history information
estimation for occupational health risks
63
what is the geochemistry of the site and what kind of soil properties will be examined
analysis requirements: what kind of analysis methods are used at the site and how much
analysis work need to be done in the laboratories
what kind of analysis is done: qualitative, quantitative, maximum concentrations, average

concentrations, concentration ranges
sampling method
sampling tools and sample preparation techniques
sampling plan
documentation
conclusion
actions based on the project
After the project research plan has been made it is very important that it will be followed
during the project so that all the reseach results can be interpreted.
X-MET3000TXS can be used for example for profiling the polluted site in order to determine a
sampling plan. Heavy element hot spots can be found quickly. Also remediation processes
(excavations, load of trucks) can be controlled as well as the soil cleaning processes by the
XMEt3000TXS analyzer.
9.3.3 Sampling
Like in all XRF analysis sample itself plays an important role in the quality of analysis.
Especially in soil analysis due to nature of soil itself the sampling and sample preparation are
major important. Typically soil mixture to be analyzed with FPXRF (Field Portable X-Ray
Fluorescense analyzer) is collected from five different points in the area of size 10m x 10m.
There are various subjects related to sampling at the contaminated soil site. At least following
questions need to be answered:
-
Are we doing random or systematic sampling?
Do we have only horizontal coordinates in our sampling map or are we taking samples
also vertically?
What is the sample amount? What is the sample bag material?
How do we name the samples? How do we store the samples and how do we transfer
them? Are we taking single samples, collection samples or do we do parallel sampling?
How many samples are taken and how many of them will be analyzed at site?
What kind of sampling diary is kept?
An example:
Person who takes care of the sampling has enormous responsibility in the successful
research and therefore he should have both experience and education. If the examined soil
amount is 20 000kg and from that 10 kg collection sample of is taken and 1kg of collection
samples is given to the laboratory where analysis is done from amount of 0.5g. In this
instance the laboratory analysis is done from 0.025ppm sample amount of original soil
amount and of course that 0.025 ppm should represent the whole 20 000kg.
Quite often soil contains particles with vast range: Particle size may vary from fine clay
powder (<0.004mm) to sand (0.062mm). Also soil type varies from one location to another.
Normally natural soil is a mixture of different particle types and sizes. Usually samples taken
from soil are not homogenous and may also have varying moisture content.
64
The most important thing is that all remediation project participants knows how the sampling
has been proceeded and what kind of sample preparation has been used so that the
measurement results can be interpreted.
9.4 Selecting operating mode

The X-MET3000TXS has two modes of operation, Empirical and Fundamental Parameter
(FP). Mode of operation is the way the instrument calculates the concentrations of elements
in an unknown sample.
X-MET3000TXS analyzer is calibrated by fundamental parameters (FP) method. FP is an
universal calculation method which takes into account the physical interactions in the sample,
for example primary and secondary fluorescenses, spectral overlap, background ect. It is
versatile calibration which can be used in all different soil types, without need for site specific
calibration adjustments. By using FP calibration all heavy elements can be measured in the
wide concentration range. FP provides chemical analysis of 21 elements commonly found in
soil. The 21 elements that can be analysed are: Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, As, Se, Sr,
Zn, Ag, Cd, Sn, Sb, W, Au, Hg, Pb.
If there is a need for more accurate results then empirical calibration can be made with factory
soil sample set or with customers own sample set. It gives good results when the unknown
samples have same matrix type compared to the calibration samples and when the analyte
and matrix element concentrations are in the calibration sample concentration ranges. By
using check samples intercepts of empirical calibration curves can be adjusted afterwards.
9.5 Measurements
Measurement itself is easy - just point the analyzer at the sample (field measurement) or
place the sample bag in the holder (field lab measurements), pull the trigger and read the
result. Measurement time is 15 300s depending on required accuracy and the interesting
analytes. Normally three different measurements from different sides of the samples is made
when working in the field.
Error due to counting statistics can be seen in the analyser display. It represents the main
source of instrumental error in analyses, STD can be decreased into its half by using four
times longer measurement time. It is recommended that 5% of the field portable XRF analysis
should be confirmed by an independent laboratory total digestion method.
9.6 Sample preparation

Purpose of appropriate sample preparation is to ensure that the sample meets the
requirements of the used analysis method and accuracy requirements. XRF analysis is done
on the surface of the sample, so the surface must represent the material.
In the field, direct measurement from ground can be done without any preparation for the
quickest possible screening result. However, minimal sample preparation is often
recommended to improve measurement accuracy. First of all the field operator should remove
any debris, such as leaves, grass and stones from the measurement surface. If there is lot of
debris in soil, the operator can screen the loose soil with a 2 mm mesh to bigger objects. After
that, the operator should loosen the soil to a depth of few centimeters and stir the loosened
soil for some homogenization. To reduce the effect of soil moisture the loosened soil may be
allowed to dry for a few hours or dried with absorbent paper before the measurement. Just
before the measurement, the operator can mix the loose soil and pack it down gently to
plastic bag for analysis.
65
If no sample preparation is performed at all less accurate analysis should be accepted.

According to the research target representative sample may be defined in different way in
each project. Anyway, it should always be characteristic, descriptive and typical.
Example:
Measurement procedure for determing proper sample preparation:
1. Collect sub samples from from 10 m x 10 m area five different points from the desired soil
depth.
2. Dry the sample if it is wet.
Note that moisture of the sample should not be higher than 10-20%. If the moisture is higher
for example absorbent papers can be used for drying the sample or the sample should be
dried in the heated oven maximum + 150C.
3. Without any sample preparation measure sample in the sample cup. Standardize the mass
of the sample. Measure it from three different points by a measurement time of 180s and
check the average result.
4. Remove particles with diameter > 2 mm. Again, measure the sample from 3 different points
by a measuremet time of 180 s.
If the average result of this sample differ less than 20% with the average results of original
sample containing all particles with diameter > 2 mm it means that the measured sample from
sampling points is reasonably homogeneous and can be interpret as semi-quantitave results.
If the results between non-sieved sample and sample sieved with > 2mm sieve differ more
than 20% it indicates that the soil is not homogeneous and particle size is affecting to the
results. If so, then sample should be sieved by using 250 m sieve.
If results from this sample sieved with 250 m sieve differ less than 20% from the previous (>
2mm) then it indicates that minimum 2 mm sieving should to be done before measurements.
If the results differs more than 20% from the sample sieved through 2 mm then particle size is
still affecting the result. In this instance 125 m sieve should be used to aduquate to assure
the quantitative data quality level. Etc.
9.6.1 Sample cups
XMET3000TXS measurements can be done either through
the plastic bag or in the sample cups. Always better
repeatability and accuracy is obtained when careful sample
preparation, sample cups and safety shield for the sample
cups are used. This is not only because of the sample
homogenity but also because of the constant measurement
geometry.
Inconsistent positioning of samples in front of the analyzer window is a potential source of

error because the X-Ray signal decreases as the distance from the X-Ray tube increases.
Maintaining a consistent distance between the window and the sample minimizes the
problem. For the best results, the window of the analyzer should be in direct contact with the
sample.
66
When preparing the sample the penetration depth of the radiation should be taken account.
When measuring soil for example Cr analysis is done from about 100 m sample layer and
Cd analysis is done from about 6 mm sample layer. For example in Cd case if the sample
layer is thinner than 6mm then mass of the sample must be standardized i.e. sample cup
weight should be equal from one sample to another although the sample volume would be
different.
For good results, soil samples should be dried and then ground fine enough to be essentially
homogeneous. For Cu and Fe analysis this means grain size about 50 - 80 m. For lighter
elements the grain size should be even smaller, about 20 m. However, acceptable results
may be obtained in practice with coarser materials. Dry and ground soil sample should fullfill
the sample cup. Sample should be pressed by a sample pressing tool to get air out of the
sample material.
The sample cup consist of a plastic cell and a

snap-on ring with a piece of plastic foil
clamped between them. Pressing tool is used
to remove an extra air from the sample.
67
9.6.2 Sample Bags

When making the analysis through the plastic bags, a flat, smooth and clean powder surface
should be made for measurements. Before using any commercial sample bags it should be
checked that the plastic does not contain any elements (for example such as Zn or Ti) which
may disturb XRF analysis. It is recommended that sample bags provided by OIA Oy are used
for the measurements.
At least particles with diameter > 2 mm should be removed from the sample. In some
instances also the fine part with diameter > 0.5 mm of the sample is sieved out of the sample
to avoid the classification in a sample cup or in the plastic bag.
If the sample amount in the sample bag is too small i.e. the thickness of the sample under the
analyzer is less than about 1cm then background plate should be used not only for the
radiation safety issues but also to keep the measurement background constant.
68
Appendix 3: X-MET3000TXR Measurement of

electronic components
10.1 Description of X-MET3000TXR
X-MET3000TXR is a handheld EDXRF analyzer designed for quality control and RoHS
compliance screening of plastics, metals and electronic components. X-MET provides quick
quantitative analysis of all restricted elements; Pb, Cd, Hg, Cr and Br. Various different
materials can be measured with the instrument; cables, PCBs, components, plastic housings,
solder material, fasteners etc.
In addition to RoHS screening application X-MET3000TXR can be used also for many
different sorting and quality assurance applications like measuring solder composition (Sn,
Ag, Cu, Bi, Pb etc) and plastics (Cl, Ti, Fe, Sb, Sr, Ca, Zn etc). Basic configuration of TXR
model is same as TX and all general information applies also to TXR model. PDA user
interface is also similar than in TX model.
10.2 Methods
Standard methods in X-MET3000TXR are Alloy FP and Plastic FP. Both are standardless
fundamental parameter calibrations. Depending on instrument set-up it is possible also that
there is empirical assay and/or ID models in method list for instance for solder alloys.
Generally, ID method detects measured material based on spectral fingerprint and goes
automatically to proper method, which can be either empirical or FP assay method or
additional ID method.
Figure 10.1. Selecting a method.

10.2.1 Auto Detect
Auto detect mode is Empirical Identification method which is used to detect material type.
Depending on detected material type system will automatically use proper calibration method.
Typical calibration methods in X-MET3000TXR analyzer are Alloy FP for metals and Plastic
69
FP for low-density materials. Operation of Auto Detect method can be fine-tuned by adding
own reference samples to the database in following way:
Figure 10.2. Reference maintenance
When Auto Detect mode is active press Reference Maintenance button in bottom of Main
Screen.
From Reference maintenance menu choose Add Sample and give name to the reference
Measure sample by using at least 60s measuring time.
Set screening Method, which method should be used with this type of the sample, for
instance with plastic sample this would be Plastic FP.
Notice: When measuring first time after addition of new reference result, result update will
take long time as database is re-built.
Analysis
method
Sample name
Screening
method
Measurement
time
Results
Standard
deviation
Detected
grade
Add Reference
to modify auto
detect ID
Figure 10.3. Typical result screen, Auto Detect mode
70
10.2.2 Alloy FP
Alloy FP is general calibration for all metals types and allows measurement of wide
concentration range (0-100%) of all typical metals. It is possible to measure wide range of
alloys used in electronic industry including, Nickel, Iron, Cobalt, Copper, Lead, Titanium, Zinc,
Silver, Gold alloys etc. Important feature of Alloy FP calibration is that result is always
normalized to 100%. This means that if material contains light elements, which wont be
detected by X-MET3000TXR Alloy FP (e.g. C, H, O, Si, Na, Mg, Al, P, Cl, S, Ca) analyzer
reports higher concentration than true value as result of detected elements is normalized to
100%. All materials, which contains these elements should be measured with Plastic FP
which takes into account amount of light elements in calculation.
Following 29 elements are measured with alloy FP: Ag , As, Au, Bi, Cd, Co, Cr, Cu, Fe, Hg, Ir,
Mn, Nb, Ni, Pb, Pt, Sb, Se, Sn, Sr, Ta, Ti, V, W, Cd, Zn, Zr, Br, Re
10.2.3 Plastic FP
Plastic FP is general calibration for all light matrix material, even that it is specifically
optimized for plastics. Plastic FP is recommended method for all materials, which contains
light elements such as : C, H, O, Si, Na, Mg, Al, P, Cl, S, Ca etc. Typical light matrix materials
include: Plastic, rubber, soil, ceramics, wood, paper, cardboard, soil, fiberglass, liquids, fabric,
paint etc. Plastic FP, takes into account amount of light elements and gives correct result
even that some of these elements cant be detected by X-MET3000TXR. However, pure
metals cant be measured (excluding Al & Mg alloys) with Plastic FP as it is optimized for light
matrix materials. Following 22 elements are measured with Plastic FP: Cl, Br, Sn, Sb, Ti, Cr,
Mn, Fe, Ni, Cu, Zn, As, Pb, Bi, Se, Cd, Hg, Sr, Ag, Au, Mo, Ta. Plastic FP is designed to work
in light matrix materials, thus maximum concentration of heavy element it can measure is
about 20%.
10.3 Analyzing different materials

10.3.1 Measuring time
Recommended measuring time for RoHS screening is dependent on target precision that is
required for results by user. Generally recommended measuring time for measuring trace
amount of heavy metals in homogeneous material is 120s, which enables detection of all
RoHS elements which exceeds restricted limit (Cd 100ppm, Pb 1000ppm, Hg 1000ppm, Cr
1000ppm, Br 300ppm) in most materials. However if target is just to sort SnPb solder from
lead-free solder or detect if Br fire retardant is used in plastic, required measuring time can be
less than 10s.
When measuring time is extended detection limit will be lower and repeatability of
measurement result improves. As an example, when measuring time is doubled, detection
limit lowers about 40%.
10.3.2 Non-homogeneous material
When analyzing material, which is not uniform, i.e. it includes many different material like
printed circuit board or semiconductor chip, measuring result will be average of measuring
spot area. Measuring spot size is about 5 x 6 mm in X-MET3000TXR analyzer. When
measuring small components weld beam adapter (p/n4103407P) can be used to restrict
measurement area.
71
Figure 10.4. weld beam adapter

ED-XRF is generally surface measurement method and most of the signal is received from
surface of the sample. This applies particularly to metal alloys. However, when measuring
light metal alloys like aluminum and magnesium alloys or other low density materials like
paper, ceramic or plastic measuring depth can be several millimetres. As an example when
measuring semiconductor chip, not only plastic cover is analyzed, but also some of the
internal layers, thus measurement result will represent about average within penetration
depth. If accurate results are required it is advisable to separate all the different materials
from each other and measure them separately.
10.3.3 Metals
Metals generally are homogeneous in nature and analysis result will represent real metal
composition. However, if there is coating in metal its good idea to scrape the coating off and
measure separately coating material and base metal to ensure correct results. Alloy FP is
correct method for metals and metallic coatings and Plastic FP for paints etc.
10.3.4 Solders
In order to comply with the various directives, i.e. ensure electronic components are Pb-free
and conform to the RoHS requirements, electronic manufactures have in many cases
eliminated the traditional tin-lead solder and replaced it with non-lead containing solders. The
most common replacement for tin-lead (Sn-Pb) solder is tin-silver-copper (Sn/Ag/Cu or SAC)
solder. One of the most important characteristics of this solder is that the Pb level is less than
1000 ppm. In addition also total solder composition is very important to maintain
characteristics of the solder and prevent defects like tin whiskering.
To be able to get correct measurement result, only solder material should be in measuring
spot area. If for instance solder is measured directly from PCB, result will be average of whole
area, which means that solder composition result is not correct. All correct elements will be
reported but their concentration is much lower than real solder composition itself. Best
method for measuring solder composition from homogeneous material like PCB is alloy FP. It
is important to notice, that empirical calibrations like solder empirical works only for similar
materials that calibration set (pure solder) for other type of materials result will be completely
wrong.
72
10.3.5 Plastics
Many metals such as titanium, lead, cadmium, zinc, iron, bromine have been used for years
in the manufacture of plastic products. Content of metals in plastic material can be measured
using X-MET3000TXR with plastic FP method. Plastic FP can be used also to separate PVC
(poly vinylchloride) plastic from other plastic types based on Chlorine (Cl) content. Plastics as
such can be treated as uniform material, if they are not coated or painted. If plastic part is
coated or if it contains many different materials, these materials should be measured
separately if accurate quantitative results are required. Plastic thickness should be minimum
1mm to ensure accurate results.
Figure 10.5. Analysis of plastic material

When measuring plastics, it should be taken into account that penetration depth to plastic
material is maximum 10mm, which means that when measuring for instance cable insulation
or monitor housing analyzer sees matrial also under the plastic material. In this instance
analysis result represents average of measuring depth not only plastic material. Also, when
measuring thin plastic materials (<10mm thick) on the table, background plate should be used
to make a measurement background constant
Figure 10.6. Background plate
10.3.6 Printed circuit boards and semiconductor chips

PCB analysis is very complex as it is non-homoeneous multi-layer structure, containing
metals, epoxy, fiberglass, fire retardant etc. which means that measurement result is average
composition of metals in measured area. Penetration depth is dependent on material layers,
which means that measuring result is difficult interpret.
73
Figure 10.7. Direct measurement from populated PCB
When Auto Detect ID mode is used normally Plastic FP is used as PCB contains lot
of fiberglass. However, generally alloy FP works best if user want to know
composition of metal coatings, solder materials or metals in general and Polymer FP
if user wants to know real average composition of the PCB.
10.3.7 Powders, pellets, etc.
When measuring small semiconductor chips or raw material like liquids, powders or
pellets It is most effective to measure these through plastic bag or by using sample
cups for measurement.
When making the analysis through the plastic bags they can be measured on table
using background plate or by using optional sample bag adapter in bench top mode
(Figure 10.6). Before using any commercial sample bags it should be checked that
the plastic does not contain any elements (for example such as Zn, Pb or Ti) which
may disturb sample results. It is recommended that sample bags provided by OIA Oy
are used for the measurements.
Figure 10.8.
Bench top installation of
X-MET3000TXS with safety shield
for sample bag measurements
When measuring liquids, it is best to make analysis in bench top mode using disposable
sample cups and standard safety shield or optional sample cup or sample bag adapter for the
analysis. Before analysis, make sure that sample cup window does not contain any elements
which may disturb the results and it can withstand chemically the liquid material.
74
Appendix 4: Energies of K and L lines

Atomic
number
Symbol
Element
Intensity Ratios
K
7:
12
13
14
15
16
17
18
19
20
21
22
23
24
25
26
27
28
29
30
31
32
33
34
35
36
37
38
39
40
41
42
43
44
45
46
47
48
49
50
51
52
53
54
55
56
57
Mg
Al
Si
P
S
Cl
Ar
K
Ca
Sc
Ti
V
Cr
Mn
Fe
Co
Ni
Cu
Zn
Ga
Ge
As
Se
Br
Kr
Rb
Sr
Y
Zr
Nb
Mo
Tc
Ru
Rh
Pd
Ag
Cd
In
Sn
Sb
Te
I
Xe
Cs
Ba
La
Magnesium
Aluminum
Silicon
Phosphorus
Sulfur
Chlorine
Argon
Potassium
Calcium
Scandium
Titanium
Vanadium
Chromium
Manganese
Iron
Cobalt
Nickel
Copper
Zinc
Gallium
Germanium
Arsenic
Selenium
Bromine
Krypton
Rubidium
Strontium
Yttrium
Zirconium
Niobium
Molybdenum
Technetium
Ruthenium
Rhodium
Palladium
Silver
Cadmium
Indium
Tin
Antimony
Tellurium
Iodine
Xenon
Cesium
Barium
Lanthanum
1.2
1.4
1.74
2.0
2.3
2.6
2.9
3.3
3.6
4.0
4.5
4.9
5.4
5.8
6.4
6.9
7.4
8.04
8.6
9.24
9.8
10.5
11.2
11.9
12.6
13.4
14.1
14.9
15.7
16.6
17.4
18.4
19.2
20.1
21.1
22.1
23.1
24.1
25.2
26.2
27.3
28.5
29.6
30.8
32.0
33.2
75
L
9:
1.3
1.5
1.8
2.14
2.4
2.8
3.1
3.5
4.0
4.4
4.9
5.4
5.9
6.4
7.0
7.6
8.3
8.94
9.6
10.3
11.0
11.8
12.6
13.4
14.2
15.1
16.0
16.9
17.8
18.7
19.8
20.8
21.9
23.0
24.1
25.2
26.4
27.6
28.8
30.1
31.3
32.7
34.0
35.4
36.8
38.3
1.3
1.4
1.5
1.6
1.8
1.9
2.04
2.1
2.2
2.4
2.5
2.7
2.84
2.9
3.1
3.2
3.44
3.6
3.7
3.94
4.1
4.2
4.4
4.6
L
6:
1.4
1.5
1.64
1.7
1.8
2.0
2.1
2.3
2.4
2.6
2.7
2.94
3.1
3.2
3.4
3.64
3.8
4.0
4.2
4.4
4.6
4.8
5.04
5.2
2.3
2.4
2.6
2.7
2.9
3.14
3.3
3.5
3.7
3.9
4.1
4.3
4.5
4.8
5.04
5.2
5.5
5.7
Atomic
number
58
59
60
61
62
63
64
65
66
67
68
69
70
71
72
73
74
75
76
77
78
79
80
81
82
83
84
85
86
87
88
89
90
91
92
Symbol
Ce
Pr
Nd
Pm
Sm
Eu
Gd
Tb
Dy
Ho
Er
Tm
Y
Lu
Hf
Ta
W
Re
Os
Ir
Pt
Au
Hg
Tl
Pb
Bi
Po
At
Rn
Fr
Ra
Ac
Th
Pa
U
Element
Intensity Ratios
K
7:
Cerium
Praseodymium
Neodymium
Promethium
Samarium
Europium
Gadolinium
Terbium
Dysprosium
Holmium
Erbium
Thulium
Ytterbium
Lutetium
Hafnium
Tantalum
Tungsten
Rhenium
Osmium
Iridium
Platinum
Gold
Mercury
Thallium
Lead
Bismuth
Polonium
Astatine
Radon
Francium
Radium
Actinium
Thorium
Protactinium
Uranium
34.5
35.8
37.1
38.4
39.8
41.2
42.6
76
39.7
41.3
42.8
44.5
46.0
47.6
49.3
L
9:
4.84
5.0
5.2
5.4
5.6
5.84
6.0
6.2
6.4
6.7
6.94
7.1
7.4
7.6
7.8
8.14
8.3
8.64
8.9
9.1
9.4
9.7
9.9
10.3
10.5
10.8
11.1
11.4
11.7
12.0
12.3
12.6
13.0
13.3
13.6
L
6:
5.4
5.7
5.9
6.2
6.4
6.7
6.9
7.24
7.5
7.7
8.0
8.3
8.64
8.9
9.24
9.54
9.8
10.2
10.5
10.9
11.2
11.5
11.9
12.3
12.6
13.0
13.4
13.8
14.2
14.6
15.0
15.4
15.8
16.3
16.7
6.0
6.3
6.6
6.8
7.1
7.4
7.7
8.1
8.4
8.7
9.0
9.4
9.7
10.1
10.5
10.9
11.3
11.7
12.1
12.5
12.9
13.4
13.8
14.3
14.8
15.2
15.7
16.3
16.8
17.3
17.8
18.4
19.0
19.6
20.2

5102037E - 120 - User ManualTX, TXS, TXR PDF

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5102037E - 120 - User ManualTX, TXS, TXR PDF

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X-MET3000TX

Series handheld XRF analyzers

X-MET3000TX / TXS / TXR

The X-Met generates X-ray radiation when it is operating. In most

CAUTION: This instrument produces X-rays when energised.

CAUTION: Corrosion of Beryllium

CAUTION: Beryllium toxicity

5.4.5. User Setup ........................................................................................................................................... 44

Description of the X-MET3000TX

Principal components of the X-MET 3000TX

PDA AC adapter plug

PDA display shield

Safety shield for

Kapton window film

Optional accessories: (depending on analyzer type)

Sample bag holder

Sample cup holder

Sample cup film

Weld beam adapter

2.2. The Analyzer

The second lock is for

The infrared safety sensor on the

2.3. The PDA computer

2.4. Environmental operating conditions for the X-MET3000TX

2.5. Power supply

Line (A/C) power

2.6. Hot Surface Adapter

Cooling time between

3.1. Preparing the X-MET for use

4. Lock PDA computer into place.

3.2. Switching backlight ON/OFF

3.3. Calendar and clock adjustment

3.4. Charging the batteries

3.4.2 Charging the PDA internal battery

Turn the instrument off (Section 3.7.).

3.5. Bench top operation

Turn on the instrument.

3.6 To turn off the instrument

3.7. Sample preparation

Figure 4.1. Start menu

Figure 4.2. Getting connected

4.2. Making measurements

Via this menu the user can:

WARNING: When the X-MET3000TX is operating, ensure that the sample

Figure 4.4. Measurement

4.2.2. Name Sample

Figure 4.6. Name sample.

4.2.3. Select Method

Figure 4.7. Selecting a method.

4.2.3.1. Empirical Assay method type

Figure 4.8. Result of an empirical assay method measurement

Figure 4.9. Result of positive identification of 2 Cr 1Mo

Figure 4.10. Result of negative identification.

4.2.3.3. Fundamental Parameters method type

4.2.4. Display spectra

Figure 4.11. Spectral display.

4.12. Selection of element for line identification

4.13. Spectral display XRF line markers

4.2.5. Configuration Backup

4.14. Configuration Backup Settings

5.2. FP method Settings

Figure 5.1. Settings menu of a FP method