User Manual
X-MET3000TX
Series handheld XRF analyzers
X-MET3000TX / TXS / TXR
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P.O. Box 85 (Nihtisillankuja 5) FI-02631 ESPOO, Finland Tel: 09 329 411
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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.
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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
5.3.1. Set Measurement Time...37
5.3.2. Output Settings...37
5.3.3. Test Measurement ...37
5.3.4. Method Type Parameters...38
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
5.4.1. Set Measurement Time...43
5.4.2. Output Settings...43
5.4.3. Test Measurement ...43
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
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 X-MET3000TX 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.
Principal components of the X-MET 3000TX
2.1. Principal parts
Analyzer Battery (*2) Battery charger
Standard shipping case
Instrument stand
for bench top use AC adapter PDA computer
Stylus
Included accessories:
USB Synchronisation cable
PDA AC adapter
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Remote extension cable for PDA
Safety shield for
small samples Kapton window filmkit Shoulder strap
PDA display shield set
Protection cover
User Manual
Optional accessories: (depending on analyzer type)
Sample bag holder Background plate Sample cup holder Sample cups
Sample bags Sample pressing
tool
Remote trigger cable
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.
Figure 2.2.1
Figure 2.2.2
Figure 2.2.3
Figure 2.2.4
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.
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. To turn on the instrument, turn the X-MET3000TX interlock key to the “ON” position.
The second lock is for removing the palmtop computer from the instrument.
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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 320×240 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.
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.
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 HumidityContinuous 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.
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
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.
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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 (non-blinking) 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.
Turn on the instrument.
WARNING: To measure small sized samples, which don’t 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.
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.
22 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.
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. Figure 4.3. Measurement screen, Main menu.
Figure 4.4. Measurement in progress.
Figure 4.5.
Measurement results screen.
24 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.
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 ¼ 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.
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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 cursor’s position in channels. Count gives the number of counts at the cursor’s 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”.
Select “XRF Line Display” to place markers on the spectrum identifying the α and β 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.
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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
30 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.
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 measurement’s 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.
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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.
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).
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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.
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
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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
5.3. Empirical assay method Settings
Figure 5.18. Settings menu of empirical assay method
5.3.1. 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.
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 approximately two (2) second intervals (Figure 5.19). The final result is calculated after releasing the trigger.
Figure 5.19. Updating screen during measurement
5.3.2. Output Settings See Section 5.2.2. 5.3.3. Test Measurement See Section 5.2.3.
38 5.3.4. Method Type Parameters
This screen allows the changing of various parameters related to the selected measurement 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.
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.
40 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”.
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.
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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 calibration´s 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.
5.4. Identification method Settings
Figure 5.28.
5.4.1. Set Measurement Time
The measurement time can be changed by activating “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.
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 approximately 2 second intervals (see Figure 5.19.) The final result is calculated after releasing the trigger.
5.4.2. Output Settings See Section 5.2.2.
5.4.3. Test Measurement See Section 5.2.3.
5.4.4. Method Type Parameters
This screen allows the changing of various parameters related to the selected measurement method.
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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 measurement’s 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
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
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.
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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.
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
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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.
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 –
Yellow, High voltage on, failsafe warning light –
Operator trigger interlock – When the trigger is pulled, X-rays are generated if the following
conditions are met:
Infrared beam safety sensor –
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.
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.
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.
52 Dual red X-ray on failsafe warning light –
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 doesn’t 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.
When the trigger is pulled and the infrared sensor is engaged, the red lights will be activated indicating the generation of X-rays. If one or both of the red LED’s are burned out, X-rays will not be generated.
Protective safety shield for small sample
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, 2µA).
Aluminium sheet Relative intensity Iron sheet Relative intensity
0 mm 100 0.0 mm 100 1 mm 55 0.1 mm 31 2 mm 36 0.2 mm 15 3 mm 26 0.3 mm 8 4 mm 19 0.4 mm 5 5 mm 15 0.5 mm 3 10 mm 5 1.0 mm 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 DONT
Read and understand the safety information (Section 7)
Override the safety features
Follow any instructions given Point the analyzer at any person or animal Store the key away from the analyzer when
not in operation to prevent unauthorized use.
Leave the key with the analyzer when not in use
Store the analyzer in a safe location when not in use.
Leave the analyzer unattended if not safely stored away.
Keep control over who is authorized to use the device.
Allow people into the beam path and train users in managing this risk.
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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 1300 h 26 h 50 344 h 6 h 53 min 25 96 h 1 h 55 min 10 20 h 25 min 5 7 h 9 min 0 1 h 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.
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 3.1µA. (1µSv = 100µrem).
56 Position µSv/hr Position µSv/hr 1 0.07 8 0.07 2 0.07 9 0.06 3 0.04 10 0.05 4 0.05 11 0.05 5 0.05 12 0.06 6 0.06 13 0.05 7 0.07
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.
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 isn’t 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.
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.
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9.2 Radiation safety
Please read thoroughly the “radiation safety” section in the XMET3000TX User’s 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 9.3 Safety shield for 9.4 Background plate
for sample bag sample cup
measurements measurements (option)
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).
