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Related Manuals for Bruker M4 TORNADO
Summary of Contents for Bruker M4 TORNADO
- Page 1 TORNADO High performance Micro-XRF spectrometer...
- Page 2 Suggestions for improvement are welcome. Order no. DOC-M81-EXX012 V1. Issue: 04/12/13. © 2013, Bruker Nano GmbH, Berlin, Germany. All trademarks and registered trademarks are the sole property of their respective owners. Printed in the Federal Republic of Germany.
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Page 3: Table Of Contents
3.4 Spectroscopic Resolution ....................22 3.5 Composition of a Spectrum .................... 23 3.6 Evaluation of X-ray Fluorescence Spectra ..............23 4 The M4 TORNADO system ......................27 4.1 Product Description ......................27 4.1.1 Product features ..................... 27 4.1.2 Product versions ..................... 27 4.2 Hardware System Components .................. - Page 4 6.9.5 The Line scan tab ..................111 6.9.6 The Phases tab .................... 112 6.9.7 Quantification of area distributions ............... 116 6.10 Using the M4 TORNADO Report Editor ............... 116 6.10.1 Handling objects ................... 118 6.10.2 Add drawings and text .................. 119 6.10.3 Using placeholders and auto text ..............
- Page 5 10 Transportation ......................... 154 11 Disposal ............................ 155 A Quantification with M-Quant ....................156 B Standard extent of delivery for the M4 TORNADO ............... 159 C General safety precautions of the M4 TORNADO ..............160 D Biological effects of X-ray radiation ..................161 Index ...............................
- Page 7 Table of Figures Table of Figures Fig. 1 Safety equipment on the front panel of the M4 TORNADO ........18 Fig. 2 Emergence of X-ray fluorescence radiation ..............19 Fig. 3 Emergence of a digital X-ray spectrum ...............21 Fig. 4 Definition of FWHM .....................22 Fig.
- Page 8 Table of Figures Fig. 59 The panel X-ray tube ....................129 Fig. 60 Selection of a calibration file ..................130 Fig. 61 Selection of the camera ports ................... 130 Fig. 62 Settings for stage speed and joystick sensitivity ............131 Fig.
- Page 9 Warning labels and name plates of the electronic units ..........18 Table 3 Steps of spectrum evaluation ..................24 Table 4 Connections of the M4 TORNADO system components ..........28 Table 5 Technical parameters of the M4 TORNADO ..............30 Table 6 Electrical connections ....................33 Table 7 External requirements ....................34...
- Page 10 List of Tables Table 59 List of the components included in the standard delivery ........159 User Manual...
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Page 11: Introduction
These operating instructions are intended to familiarize the user with the operation of Bruker’s M4 TORNADO. The instructions allow the user to get started quickly and include all information necessary to operate the device in a safe and competent way. -
Page 12: Intended Usage
Analysis of aggressive chemical or radioactive substances 1.4 Warranty and Liability The general conditions of sale and supply as passed to the operator of the M4 TORNADO X-ray analysis device by Bruker Nano GmbH strictly apply. Warranty and liability claims for personal and material damage are excluded if they are a result of one or more of the following reasons: ... -
Page 13: Safety Instructions
2 Safety Instructions 2.1 General Information X-ray energy levels (up to 50 keV) in the excitation beam as used in the M4 TORNADO cause damage to tissue and bone as a result of high levels of radiation. Poorly healing wounds and, in extreme cases, loss of individual limbs (e.g. -
Page 14: Safety Instructions For Handling Beryllium
Observing the safety rules can prevent a risk of X-ray radiation for the operator due to the measures taken by the manufacturer and the technical installations. According to the Röntgenverordnung (RöV) – the German X-ray Ordinance - the M4 TORNADO complies with a full protection system regarding its radiation protection data and the radiation exposure of the operating staff. -
Page 15: Protection Against Electric Current
Switching on the system voltage is only possible by means of a key switch. Switching on the high voltage is only possible using the controlling software "M4 TORNADO" included in delivery. The following basic safety rules must be observed at all times: ... -
Page 16: Protection Against Mechanical Movements
40 W (refer also to the datasheet of the X-ray tube). All possible constructive measures have been implemented to avoid X-ray radiation hazards for the personnel. The safety equipment of the M4 TORNADO is listed in Table 1 and illustrated in Fig. 1. User Manual... -
Page 17: Table 1 Safety Equipment Of The M4 Tornado
Safety Instructions Table 1 Safety equipment of the M4 TORNADO Pos. Safety equipment Function Key switch, on the left side Implies an operation by authorized persons only board Green warning light “Power” Indicates that the mains voltage is switched on and the... -
Page 18: Warning Labels And Name Plates
Safety Instructions Fig. 1 Safety equipment on the front panel of the M4 TORNADO 2.10 Warning Labels and Name Plates Table 2 Warning labels and name plates of the electronic units Element Place Function Front panel Company logo Front panel... -
Page 19: Functional Principles
Functional principles 3 Functional principles This section offers a short general description of the functional principles of the M4 TORNADO. For a more comprehensive description, please refer to the reference manual for Physical Principles of Micro-XRF. 3.1 X-ray Fluorescence The basis of X-ray fluorescence analysis is an excitation and relaxation process within the atomic electron shell. -
Page 20: Detection Of X-Ray Quanta
This continuous radiation is emitted by the tube. The tube radiation, both characteristic radiation of the tube material (for the M4 TORNADO typically Rhodium) and the bremsstrahlung, excites the sample to emit only characteristic radiation. This reduces the spectral background of the excited spectrum. -
Page 21: Fig. 3 Emergence Of A Digital X-Ray Spectrum
It cannot be compared with a current measurement of a voltage or a current as known from electrical engineering. The quality of the spectrum and therefore the analytical results strongly depend on the fluorescence intensity and the time of measurement. Measurement times between 10 s and 180 s are common. M4 TORNADO... -
Page 22: Spectroscopic Resolution
Functional principles An X-ray spectrum usually does not just contain the fluorescence lines of the sample material but also excitation radiation, which has been scattered by the sample material. 3.4 Spectroscopic Resolution The natural width of fluorescence lines is normally < 10 eV and variations depending on the type of line series (K, L, M) and the chemical bond type of the atom are negligible. -
Page 23: Composition Of A Spectrum
Upon completion of the measurement, the spectrum itself is just a data set and not yet a result. It is an iterative process of spectrum correction and evaluation that leads to the solution of an analytical task. The different steps of a spectrum evaluation will be briefly described in Table 3. M4 TORNADO... -
Page 24: Table 3 Steps Of Spectrum Evaluation
Functional principles Table 3 Steps of spectrum evaluation Procedure Spectrum Spectra correction Correction of certain detector artifacts such as shelf background, escae peak, and sum peaks. Element identification The X-ray fluorescence lines of the individual elements are stored in an atomic data library. The identification of the elements is normally done by an interactive comparison of the measured... - Page 25 The value for the fit quality should preferably be smaller than 10. High values (>10) are an indicator for misidentified or non-identified elements or for an inaccurate gain χ − δ − correction. M4 TORNADO...
- Page 26 Functional principles Procedure Spectrum Result calculation The net peak areas are transferred to the quantification method. Different methods can be used in dependence of the knowledge about the sample (homogeneous, layer system), on the availability of references and the requirements for accuracy.
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Page 27: The M4 Tornado System
Fully radiation protected instrument according to German X-ray ordinance 4.1.2 Product versions The M4 TORNADO is available in a basic version with several features that can be optionally used to adapt the instrument to the analytical task. These options are: ... -
Page 28: Hardware System Components
PC with peripheral components like monitor, keyboard, mouse Vacuum pump Fig. 6 Components of the M4 TORNADO system The connections of the M4 TORNADO system components are listed in Table 4. Table 4 Connections of the M4 TORNADO system components Pos. Component... -
Page 29: Spectrometer
The M4 TORNADO system 4.2.1 Spectrometer The spectrometer consists of several components. The sample chamber is a large rectangular box that allows the analysis of large samples. The sample chamber can be vacuum closed. The door is motor driven and has sensors to stop the door movement for protection of the user. -
Page 30: Instrument Control Pc
(detector, X-ray optics). The pump is also maintenance free. 4.2.4 Technical parameters The most important technical parameters of the M4 TORNADO are displayed in Table 5. Table 5 Technical parameters of the M4 TORNADO... - Page 31 The M4 TORNADO system Parameter M4 TORNADO Connections 3 prong grounded plug P + N + PE, according to DIN 49441 Components X-ray tube Manufacturer Rtw Dr.Warrikhoff Röntgentechnik GmbH Type Ceramic side window fine focus or line focus tube with Be-window MCBM-50-0.6BRh, MCB-50-0.7q W Max.
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Page 32: Hardware Installation
The M4 TORNADO system Parameter M4 TORNADO Sample positioning Stage motorized X-Y-Z-stage Traversing range 200 mm x 160 mm x 120 mm Mapping range 190 mm x 160 mm Max. speed 100 mm/s Sample view Camera 1, 2 coloured camera system with microscope Magnification 10x and 100x sample view of approx. -
Page 33: Electrical Connection
The M4 TORNADO system Fig. 7 Room planning for the installation of the M4 TORNADO 4.3.2 Electrical connection The electrical connections required for the M4 TORNADO are specified in Table 6. Table 6 Electrical connections Electrical connection Dimensions Spectrometer 100 V…240 V 50 Hz…60 Hz... -
Page 34: External Requirements
The vacuum pump has to be adapted to the line voltage system; all other components are prepared for wide range power supply. 4.3.3 External requirements The installation of the M4 TORNADO requires several external prerequisites. They are listed in Table 7. Table 7... -
Page 35: The M4 Tornado Software
With multiple client installations a user can log in from any client workstation and access his private data and user profile on the M4 TORNADO server. With multiple M4 TORNADO servers in the network, the server to connect to is selected during log in procedure. -
Page 36: Fig. 8 Structure Of The M4 Tornado Software
The M4 TORNADO Software Fig. 8 Structure of the M4 TORNADO software Point contains the functionality for accumulation of spectra from single points. Multi-Point contains the functionalities of Point combined with the possibility of analyzing a large number per set point. Points are fixed with respect to the image frame of the video image where the points were placed. -
Page 37: Main Screen Areas
5.1.3 Main screen areas Title bar. The title bar at the top of the M4 TORNADO program window contains the general ® control buttons common to Windows applications for controlling the display. - Page 38 The M4 TORNADO Software A list of spectra displayed below the spectrum window provides control over display, data exchange, and spectrum analysis. Result window. Calculated results, result diagrams or other presentations of evaluated data are displayed in the right part of the screen.
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Page 39: Analysis Options
Standard-based analysis. Standard-based analysis is provided allowing to improve the precision of bulk quantitative sample analysis using a set of available reference materials. Automatic and interactive spectrum analysis. M4 TORNADO performs automatic spectrum analysis during or after spectrum acquisition and supports batch processing for multiple spectra. -
Page 40: Volumes, Files And Folders
M4 TORNADO software. 5.1.6 Volumes, files and folders Volumes and folders. Each user logged in to M4 TORNADO can access private and public volumes on the server. The private data is not visible to other users, in public volumes all users have the same rights so that any user can access, change, and delete any file or folder stored here. -
Page 41: Table 8 Steps For Program Installation
The first step of program installation informs about the start of installation. Select the type of device you would like to operate (M4 TORNADO or M6 JETSTREAM). The third step informs about the path for the installation. This path can be changed according the PC requirements. -
Page 42: Installation Of The Usb Camera Driver
The installation procedure has to be finished. After finishing the setup assistant, the M4 TORNADO program is available. M4 TORNADO can be started with the entry in the Start menu or the Desktop Icon 5.2.2 Installation of the USB camera driver If the instrument is connected to the USB-port, the driver has to be installed separately. -
Page 43: Connection Of Pc And Instrument
The M4 TORNADO Software Table 9 Steps for USB camera driver installation Dialog Description Installation should be performed with drivers that are on the hard-disk. The path of the drivers will be searched automatically. This procedure has to be repeated 6 times, since there are 3 cameras and each of them has 2 drivers. -
Page 44: Table 10 Generation Of Connection Between Instrument And Instrument Pc (Windows ® Xp)
The M4 TORNADO Software ® Table 10 Generation of connection between instrument and instrument PC (Windows Dialog Description Selection of Network connections on the Select Local Area connections Select the Internet Protocol (TCP/IP) Use the following addresses: IP address: 192.168.10.1 sub net mask: 255.255.255.0... -
Page 45: Table 11 Generation Of Connection Between Instrument And Instrument Pc (Windows ® 7)
The M4 TORNADO Software ® Table 11 Generation of connection between instrument and instrument PC (Windows Dialog Description Selection of Network connections on the Select Local Area connections Select properties Select the Internet Protocol Version 4 (TCP/IPv4) Use the following addresses: IP address: 192.168.10.1... -
Page 46: Installation Of A New Software Version
New software versions are delivered as an Install CD. Here the Install.exe file has to be executed. Before doing that, the path of the existing program should be changed. The path is C:\programs\Bruker\M4 Tornado. This can be renamed to, for example, M4 TornadoX. Then the update can be started. -
Page 47: Registration
For safety reasons, opening the console of the communication server requires Windows administrator rights. 5.3.2 Assigning new users New users are to be assigned via the communication server. Double clicking the Bruker icon ® in the Windows task bar opens the console of the communication server. -
Page 48: Altering User Name And Password
The M4 TORNADO Software Each new user is automatically assigned a folder structure in a private volume of the server. Default methods, a predefined user profile, and demo data are copied to the user folders. Open the dialog for creating a new user with New. - Page 49 (seconds). Standby mode is also provided for the spectrometer electronics. Standby mode can be entered via command from the M4 TORNADO program window (see section 6.2.2.1) or by confirming the corresponding option when terminating a work session.
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Page 50: Starting The Operation
Recovering from errors. In cases of program lockup due to improper operation or unexpected circumstances a restart of M4 TORNADO is normally sufficient. In more severe cases a restart of the personal computer and/or the QUANTAX server may be required. More severe system breakdowns - if any - should be handled by trained service personnel. -
Page 51: Running The Program Without Measurement
The M4 TORNADO Software Step Procedure Figure Start the measuring software Start with the corresponding icon on the desktop or via Start >> Programs >> Bruker>> M4 TORNADO. Password protection The access to the software is authorized after entering the username and the password. -
Page 52: Fig. 11 Switching Off The Instrument
The M4 TORNADO Software Reduce the tube parameters Move the stage to the park position Shut down the X-ray tube Vent the sample chamber Fig. 11 Switching off the instrument User Manual... -
Page 53: Using The M4 Tornado Software
Using the M4 TORNADO Software 6 Using the M4 TORNADO Software 6.1 Getting started Fig. 12 Start-up screen of the program M4 TORNADO Table 15 Functions and settings of the start-up screen Object Description Hints Username Every user can have its own account... -
Page 54: Main Program Window And Settings
Image capturing Fig. 13 Main program window of M4 TORNADO The title bar at the top of the M4 TORNADO main program window contains the general control ® buttons common to Windows applications for the program window. Available functions for the display of the captured images, measurement data and results are compiled in Table 16 . - Page 55 Using the M4 TORNADO Software Object Description Hints Image window Zoom function Image settings Brightness, contrast (intensification), colour correction Edits display settings Measurement data window Open interactive element Clickable periodic table of elements and peak identification tool finder Searches volumes for similar...
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Page 56: Hardware Area
Using the M4 TORNADO Software 6.2.1 Hardware Area The hardware area contains several icons. They allow settings of hardware functions and their display. The following icons are available: Table 17 Icons of the hardware area Icon Description of function Switching on and off the vacuum pump and displaying of the pump status. While pumping, a blue light flashes. -
Page 57: Device Area
Using the M4 TORNADO Software Icon Description of function The vacuum status bar displays the pressure and the pumping status. During pumping the vacuum bar becomes shorter and goes from red to green. The green colour shows that the system is ready for measurement. -
Page 58: Fig. 16 Tube Line And Tube Settings Dialog
Using the M4 TORNADO Software The following information about the spectrometer settings can be found: Optimum pulse throughput (factory setting) Maximum energy of the spectrum (i.e. channel width is 2.5 eV, 5 eV, 10 eV or 20 eV) ... -
Page 59: Fig. 17 Stage Line
Using the M4 TORNADO Software Table 18 Options for tube settings Object Description Hints Display of working hours, anode These values are only declared X-ray tube material and max. tube power Setting of the current tube voltage Tube voltage and current are... -
Page 60: Table 19 Options For Stage Settings
The joystick sensitivity can be set for all axes. The M4 TORNADO is designed to work at high speed. For a better handling of sensitive samples it is possible to reduce the speed if considered necessary. The same is valid for the acceleration. -
Page 61: Project Area
This allows the combination of different data types (spectra, images, element distributions, results, element lists, etc.) in one file. Some of the M4 TORNADO objects can only be saved by embedding them in project files. Fig. 18 shows an example of a M4 TORNADO project area. - Page 62 Using the M4 TORNADO Software Option Description Save / Save as … Save the marked project. If no project name is displayed on the title bar, the new project exists only in the working memory as current project. It has to be saved to a project file.
- Page 63 Using the M4 TORNADO Software 6.2.3.2 Loading and saving project files Loading files. To load a file into the memory, open the Import/Export menu ( icon in line with the word “Project”) and click Open. The same browser options apply as for other files. The selected file will become the current project displayed in the Project screen area.
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Page 64: Acquiring Spectra
Using the M4 TORNADO Software 6.2.3.5 Information field and preview For every project item and node a quick information field is displayed next to the item name with analytically relevant information as well as time and date stamps. Clicking the... -
Page 65: Spectrum Display And Manipulation
Using the M4 TORNADO Software Preset for measurement time It can be set to automatic or manual, in real or live time. In case of stop of measurement by number of counts, the energy region has to be set separately. -
Page 66: Fig. 21 Spectra Workspace With Spectrum Display
Using the M4 TORNADO Software During a running acquisition, it is not possible to change the workspace, alter device settings, ® highlight objects, etc. (a warning will be issued). However, Windows multitasking is not influenced. Saving spectra. Acquired or loaded spectra are temporarily stored in the spectrum list (spectrum clipboard) of the corresponding workspace. -
Page 67: Table 21 Options For Spectrum Display
Using the M4 TORNADO Software Table 21 Options for spectrum display Object Description Hints Function bar above spectrum display Activates high speed spectra preview Spectrum will be continuously refreshed Configures spectra preview Allows settings for refresh time Acquires a spectrum... - Page 68 Using the M4 TORNADO Software Object Description Hints Spectrum matching - Searches See section 6.3.3 volumes for similar spectra Spectrum arithmetic Adds, substracts and multiplies spectra Auto-scales spectrum window Scales the displayed spectrum in according to foreground spectrum the foreground for full intensity...
- Page 69 Using the M4 TORNADO Software Object Description Hints Selects the displayed value of A pull-down menu opened by quantification clicking the right-facing arrow left Results shows various types for data presentation. The following information will be given: The displayed result data can be...
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Page 70: Spectra Matching
Using the M4 TORNADO Software 6.3.3 Spectra matching This function can be used to find and display spectra similar to the one currently selected. The similarity is defined with respect to channel content. In order to find similar spectra, all spectra are scaled to the same energy axis (X-axis) and compared in a cross correlation process channel by channel. -
Page 71: Table 22 Steps For The Spectra Matching Procedure
Using the M4 TORNADO Software Table 22 Steps for the Spectra matching procedure Object Description Left side of the dialog Setting of the matching conditions. The search requires 3 steps. Defines the sources for the search of matching spectra. This is possible: ... -
Page 72: Qualitative And Quantitative Analysis
Using the M4 TORNADO Software 6.4 Qualitative and quantitative Analysis 6.4.1 Element identification 6.4.1.1 Interactive element identification The interactive element identification can be performed directly from the spectrum window or be requested as the first step of an interactive quantitative spectrum analysis, executed e.g. after clicking the button. - Page 73 Using the M4 TORNADO Software Method Description Direct element entry. Elements can be added to the identification list directly by using the dialog in the bottom line of the identification tool labelled element. New elements can be specified by the international element symbols (‘Na’) or the atomic...
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Page 74: Table 24 Automatic Peak Identification
Using the M4 TORNADO Software 6.4.1.2 Automatic element identification The M4 TORNADO software also offers automatic procedures for the element identification. In particular in Micro-XRF spectra there are several spectrum artefacts – deriving from the detector like Escape, Tail and Shelf, and sum peak which can be calculated and considered. Others as diffraction peaks deriving from the sample cannot be calculated, so automatic peak identification should be only the first step. -
Page 75: Quantitative Analysis With M4 Tornado
Using the M4 TORNADO Software 6.4.2 Quantitative analysis with M4 TORNADO For the quantification with the M4 TORNADO different methods are available: standardless analysis for bulk materials (Fundamental Parameter based analysis, FP) standard-based analysis for bulk materials ... -
Page 76: Standardless Analysis For Bulk Materials
Using the M4 TORNADO Software 6.4.3 Standardless analysis for bulk materials The standdardless quantification is a Fundamental Parameter- based analysis and very useful for the analysis of non-homogeneous bulk samples, which are mostly analyzed with Micro-XRF methods. 6.4.3.1 Selection of a quantification method Table 25 summarizes the options for the selection and definition of quantification methods. -
Page 77: Fig. 25 Method Editor
Using the M4 TORNADO Software 6.4.3.2 Definition of a quantification method The definition of a quantification method can be performed by opening the method editor with the rightward-facing arrow below the button. The method editor dialog allows settings for every element. The different options offered by this dialog are described in the table below. - Page 78 Using the M4 TORNADO Software Option Description Only the elements defined in the spectrum with the periodic table are used. This can be the periodic table in the spectrum display of the measured spectrum or the periodic table in the spectrum display of quantification.
- Page 79 Using the M4 TORNADO Software Option Description Fixed concentration. If the concentration of certain elements is known, it is possible to use this information for the quantification. The concentration can be written into the box. These elements are displayed with a green background and concentration is shown in the special property of the element.
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Page 80: Fig. 26 Result Presentation For Interactive Quantification
Using the M4 TORNADO Software 6.4.3.3 Quantification procedure The standardless quantification always follows the procedure: Element (Peak) identification and Result calculation and display. The quantification has to be started with the button. The quantification of a spectrum analysis is executed without any user interaction if the automatic mode (“A”) is selected or includes interactive steps if the interactive mode (“i”) is chosen. -
Page 81: Table 27 Result Presentation For Interactive Quantification
Using the M4 TORNADO Software This dialog offers the following options. Table 27 Result presentation for interactive quantification Option Description For a description of the options for the method editor, please refer to Table 26. Result: Display of the quantification result... -
Page 82: Table 28 Quantification Results Display
Using the M4 TORNADO Software After the identification has been completed, click the button to go back to the original spectrum display and to see the quantification results on the right hand side of the dialog and below the spectrum display. There are two tabs:... -
Page 83: Fig. 27 Results Tab
Using the M4 TORNADO Software Result tab displays the same result data as the result presentation. The icon allows defining the displayed results parameters for the current spectrum (see Fig. 27). Fig. 27 Results tab Parameter tab presents measurement data of the current spectrum, such as ... -
Page 84: Fig. 29 Spectrum Tab
Using the M4 TORNADO Software Fig. 29 Spectrum tab Table 29 Energy calibration of the current spectrum Option Description Spectrum display The spectrum displays the current spectrum with all identified X-ray lines. Peaks that are selected for energy calibration are colored in blue. -
Page 85: Standard-Based Analysis For Bulk Materials
Using the M4 TORNADO Software 6.4.4 Standard-based analysis for bulk materials The analysis of bulk samples can also be performed using standard-based quantification methods. Note that a standard-based quantification requires a wide variation of different sets of standards. For the standard-based quantification the use of a data file with the ending XADF is necessary. -
Page 86: Definition Of Measurement Conditions
Using the M4 TORNADO Software 6.5.1 Definition of measurement conditions 6.5.1.1 Sample positioning Three camera systems and various modes for stage movement are available to guarantee the exact positioning of the sample required by the small spot of the excitation radiation. Two camera images with different options can be displayed simultaneously on the left hand side of the screen (see Fig. - Page 87 Using the M4 TORNADO Software Object Description Hints Autofocus Moves the sample upwards and calculates the contrast value of the current image. Final positioning for the point with highest contrast. Start the mosaic imaging See Table 31 Enlarge the image Enlarge the image view for original size.
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Page 88: Table 31 Options For Mosaic Imaging
Using the M4 TORNADO Software Table 31 Options for mosaic imaging Dialog Description The mosaic imaging feature allows combining single images of the sample to a complete image. The region of the mosaic image can be limited to reduce the time for image capture. -
Page 89: Measurement And Data Evaluation
Using the M4 TORNADO Software Automatic stop of the measurement according to the required accuracy Finishing of the measurement with given measurement time or preset counts in a defined energy region Settings for quantification Fig. 31 Definition of acquisition parameters 6.5.2 Measurement and data evaluation... -
Page 90: Definition Of Measurement Conditions
Using the M4 TORNADO Software Fig. 33 The Multi-Point workspace 6.6.1 Definition of measurement conditions The sample positioning has to be performed according to the description in section 6.5.1.1. The available functions for setting the measurement points (see Fig. 33) are described in the next table. - Page 91 Using the M4 TORNADO Software Object Description Hints Selects all objects Deletes selected objects Performs an autofocus before every measurement Defines automatically a grid with Automatic needs a preset number of points and a given number of points over type of distribution (regular grid or randomly the complete image chosen).
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Page 92: Measurement And Data Evaluation
Using the M4 TORNADO Software Automatic stop of the measurement according to the required accuracy Finishing of the measurement with given measurement time or preset counts in a defined energy region Settings for quantification Fig. 34 Definition of acquisition parameters 6.6.2 Measurement and data evaluation... -
Page 93: Auto-Point Analysis
Using the M4 TORNADO Software 6.7 Auto-Point Analysis Auto-Point workspace allows the measurement of point patterns (distributed single points, lines and matrices) under the same measurement conditions and saving the spectrum for every point separately. The measurement point patterns are related to the stage coordinates. - Page 94 Using the M4 TORNADO Software Object Description Hints The coordinates of these points are displayed in blue. Also Z-coordinates are saved and used. Maximum 3 reference points can be saved. Reference points can also be measurement points. Setting of single points...
- Page 95 Using the M4 TORNADO Software Object Description Hints Import/Export menu for acquired data, positions and results. Opens a saved complete data set. Data sets are saved in a ZIP-file with sample image, coordinates of Saves the acquired data, positions measurement points, spectra and quant or results.
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Page 96: Measurement And Data Evaluation
Using the M4 TORNADO Software Object Description Hints Moves the stage to the start point of the highlighted object. Deletes the highlighted object(s). The same function is also possible with Delete button. Opens a legend for the running Auto-Point measurement Different settings for the measurement time and mode are possible for the spectrum acquisition. -
Page 97: Quantification
Using the M4 TORNADO Software The measured spectra are displayed in the spectra field. Fig. 38 Spectrum field for Auto-Point measurement Files saved in the Auto-Point workspace in the *.spl format can be opened both in the Point and in the Multi-Point workspace. -
Page 98: Line Scan Analysis
Using the M4 TORNADO Software 6.8 Line Scan Analysis Line workspace allows the element distribution analysis along a line. Fig. 40 The Line workspace 6.8.1 Definition of measurement conditions The measurement conditions can be set on the right side of the dialog. The display of the sample... -
Page 99: Fig. 41 Settings For Line Scan Acquisition
Using the M4 TORNADO Software Object Description Hints Filter for line scan Number of points to be used for average or median filter Fast line scan with qualitative Absolute scaling would distribution normalize all elements to the maximum intensity on the line. -
Page 100: Measurement And Data Evaluation
Using the M4 TORNADO Software 6.8.2 Measurement and data evaluation Fig. 42 shows the display of the profiles along the line for selected elements. The presentation of element profiles can be changed by clicking on the legend. The elements results can be displayed in absolute or relative scaling. -
Page 101: Quantification Of Line Distributions
Using the M4 TORNADO Software Object Description Hints Definition of the presentation of line Open with double click on the scans legend It is possible to change the color, width and type of the lines (downward-facing arrow) and to toggle between dots and... -
Page 102: Area Analysis - Mapping
Using the M4 TORNADO Software 6.9 Area Analysis - Mapping Area workspace allows the determination of the element distribution in an area. Fig. 43 The Area workspace 6.9.1 Definition of measurement conditions The mapping area can be set on the sample image in every presentation mode by moving the edges with the mouse. - Page 103 Using the M4 TORNADO Software Object Description Hints Number of pixels in X and Y-direction Only one of the three and pixel distance parameters can be set, the others will be calculated to guarantee the same pixel distance in both directions.
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Page 104: Measurement And Data Evaluation
Using the M4 TORNADO Software Pre-setting of measurement time Measurement time per pixel Mode of stage movement (It is recommended to use several cycles with shorter measurement time than one map with long pixel time) Total duration of measurement Map denomination by ... -
Page 105: The Map Result Tab
Using the M4 TORNADO Software Fig. 45 Map data on the Area workspace The presentation of the data set can be done as Element distribution map – Map result tab Spectra from different objects – Spectrum tab Element distribution along any line in the map – Line scan tab ... -
Page 106: Table 37 Options For The Map Result Display In The Area Workspace
Using the M4 TORNADO Software Table 37 Options for the map result display in the Area workspace Object Description Hints Import/Export menu Export/Import of complete database, element maps, element selections and result tables Element identification Use to select elements for mapping, see section 6.3.3... -
Page 107: Fig. 47 Display Of Mapping Information
Using the M4 TORNADO Software Object Description Hints Element / phase contribution Controls color intensity of element/phase, control for every element switches on/off (check box) contribution to map or phase image, or changes the associated color by clicking on the color field 6.9.3.1 Display of mapping information... -
Page 108: Fig. 49 Map Paint Tool
Using the M4 TORNADO Software 6.9.3.3 Map paint tool This tool allows to measure the length of an object or determines the angle to the horizontal. Additionally, it allows to make inscriptions into the map, like marking some areas, special points or writing a text. -
Page 109: Table 38 False Color Display
Using the M4 TORNADO Software 6.9.3.5 False color display This option allows the display of element maps in false color presentation for the selected elements. The false color will be calculated from the sum intensities of the selected elements. The sensitivity of color selection can be adjusted. -
Page 110: The Spectrum Tab
Using the M4 TORNADO Software Table 39 Element chart Type of evaluation Description The intensity histogram shows the probability of element intensities in the different pixels. The considered element can be changed with the pull down menu. The colouring can be changed with help of the scroll bars. -
Page 111: The Line Scan Tab
Using the M4 TORNADO Software Another important spectrum is the maximum pixel spectrum (see Table 37). This spectrum is artificial and will be calculated from the highest content of every channel independent of the pixel. This spectrum allows the identification of elements that are concentrated only in hotspots. With this knowledge, the calculation of the distribution of these elements is possible. -
Page 112: The Phases Tab
Using the M4 TORNADO Software There is one additional function to improve the statistics of a line scan. With the definition of the line scan it is possible to enlarge the “thickness” of the line with the + key and reduce it with the –... -
Page 113: Fig. 53 The Phases Tab
Using the M4 TORNADO Software Fig. 53 The Phases tab The clipboard at the bottom of the phase display contains the original image and, for each individual phase (P1 to Pn), a colored image showing the area it occupies. The list below the phase image displays for each individual phase (P1 to Pn) values for the occupied area (in pixels, µm... - Page 114 Using the M4 TORNADO Software Object Description Hints Activation of automatic update of The automatic update can be phase analysis activated with the downward- facing arrow next to the AutoPhase button Slide bars The slide bars for Sensitivity, Area Edges...
- Page 115 Using the M4 TORNADO Software 6.9.6.2 Different methods for the determination of phases Histogram method basically operates within a virtual n-dimensional ‘element space’. The intensity of every mapped element spans one axis of this space. The chemical composition of each pixel in the map is virtually plotted as a single point into the space. That means pixels containing the same or similar chemical composition are within the same region of this space –...
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Page 116: Quantification Of Area Distributions
The quantification can be started with the button. The quantification runs over the complete mapped area and generates concentration images. 6.10 Using the M4 TORNADO Report Editor Report workspace permits the generation of graphical documentations of the measured data and analysis results. These reports also serve as containers for relevant measurement data of spectra, images, mapping etc. -
Page 117: Fig. 54 Workspace Report
Both applications can run simultaneously allowing the report to be built up during the course of work. Transferring data to third party applications with the M4 TORNADO software works with a few mouse clicks. Internal Reports. The M4 TORNADO software includes a WYSIWYG editor (report editor) very ®... -
Page 118: Handling Objects
Using the M4 TORNADO Software Report templates. Report templates are of the same data type as M4 TORNADO reports, i.e. they are as easy to design as a normal report. Existing reports can serve as or easily be converted into templates. -
Page 119: Add Drawings And Text
Using the M4 TORNADO Software Object Description Fixing. To fix an object, highlight it by clicking into it and check the option Fixed in the Properties section. A fixed object cannot be moved until unfixed. When a fixed object is highlighted an anchor is shown. -
Page 120: Using Placeholders And Auto Text
Using the M4 TORNADO Software Line width and arrow tips. Line width can be assigned to lines, arrows, and borderlines of shapes and text boxes. The tip of an arrow can be reshaped or resized. Lines can be converted to arrows and vice versa by using the tip selection dialog. -
Page 121: Using The Clipboard
Save... from the subsection Marked object ® Export to WORD. To export a complete designed M4 TORNADO report to Microsoft WORD (if installed), click the option Export to WORD in the subsection Report Deleting a report. -
Page 122: System Functions
Using the M4 TORNADO Software Print preview will remove the grid, the border lines, the limiters of text fields and placeholders, etc. at one click, providing a display of the page just like it is printed. Undo. Clicking the icon undoes the last action. Click it immediately after an unwanted action. -
Page 123: General Display Settings
Using the M4 TORNADO Software Object Description Hints Show the product licence Displays the actual product licence Update licence Allows the update of the licence. Required, if additional options have been purchased Screen “Select licence file” will be opened and the licence can be... -
Page 124: Table 43 Functions In The User Interface Panel
Using the M4 TORNADO Software Table 43 Functions in the User interface panel Object Description Hints Section Languages Use of the language of the interface The languages will be changed on line. The selection must be confirmed by clicking on... -
Page 125: Spectrometer Calibration
Using the M4 TORNADO Software Object Description Hints Elements Allows settings for every element Clickable periodic table of elements for quantification for editing element settings Selection of element colour Element name and lines Selection of the displayed lines... -
Page 126: Table 44 Functions In The Spectrometer Panel
Using the M4 TORNADO Software Table 44 Functions in the spectrometer panel Object Description Hints Select the pulse processor for For M4 TORNADO the pulse calibration throughput is usually prepared for 130 kcps Select the energy range for Available are 10 keV, 20 keV, 40 keV... -
Page 127: Image Settings
Using the M4 TORNADO Software 6.11.4 Image settings The panel Imaging allows the setting and adjustment of the camera systems. It has two parts – on the left the display of the camera image and on the right hand side the options for adjustment. - Page 128 Using the M4 TORNADO Software Object Description Hints Right hand section Adjustment of the white Position a white paper in the balance for the image sample chamber and press the button. Definition of image geometry Select the camera, position a...
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Page 129: X-Ray Tube Settings
Using the M4 TORNADO Software Object Description Hints Setting of ranges for an improved The limits are displayed in the shadow free mosaic image image by a green rectangle. Optimize the size to to reduce Set the image size by limits from shadow effects on the mosaic. -
Page 130: Adjustment Of The Instrument
Using the M4 TORNADO Software Fig. 60 Selection of a calibration file 6.12 Adjustment of the Instrument The instrument must be carefully adjusted so that the full functionality is guaranteed. For the adjustment the tabs in the workspace System can be used. The following adjustment procedures are necessary. -
Page 131: Settings For Stage And Joystick
Using the M4 TORNADO Software 6.12.2 Settings for stage and joystick The settings of the stage speed and joystick sensitivity can be performed with the help of the control software in the device area, stages settings. This adjustment needs not to be controlled and repeated. -
Page 132: Adjustment Of The Image Size
Using the M4 TORNADO Software Fig. 63 Taking a white standard 6.12.4 Adjustment of the image size The image size for both low and high magnification can be set in the workspace System>>Imaging. These settings are stable and do not need repeated adjustments. -
Page 133: Settings Of Image Parameters
Using the M4 TORNADO Software Position a sample with scale on the stage and adjust it in the focal plane of high mag camera. The green line in the image can be positioned to the scale by Click&Drag with the ends of the line. The corresponding distance has to be set in the data box. -
Page 134: Settings For The X-Ray Spot Calibration
Using the M4 TORNADO Software 6.12.6 Settings for the X-ray spot calibration A fine adjustment of the X-ray spot position to the sample image is possible by digital tuning of the cross hair position in the working space System>>Imaging. The X-ray foil on the blue reference sample should be positioned in the chamber and focused to the correct height. -
Page 135: Settings In The Area For Mosaic Image
Using the M4 TORNADO Software All settings have to be saved with Fig. 66 Setting in the area for autofocus 6.12.8 Settings in the area for mosaic image The sample illumination is not completely homogeneous. This is the reason that mosaic images show the edges of every image. -
Page 136: Fig. 67 Setting Of Reduced Area For Mosaic Image
Using the M4 TORNADO Software Fig. 67 Setting of reduced area for mosaic image 6.12.8.2 Correction of the illumination For the correction of the shadowing a matt white paper can be positioned in the focal plane and its image can be captured and saved. The shadowing is then used to correct the other images. -
Page 137: Often Used Analytical Procedures
7 Often Used Analytical Procedures This section intends to give the analyst a quick overview of the most important tools and analytical procedures, so permitting an instant start into analyses with the M4 TORNADO system. 7.1 Recommended Measurement Parameters The measurement parameters like tube HV, current and measurement time depend strongly on the sample itself and also on the analytical task. -
Page 138: Point
Often Used Analytical Procedures 7.2 Point Fig. 69 Point analysis User Manual... -
Page 139: Table 49 Steps For Point Analysis
Preview. Dead time should be less than 60 % Set the final tube parameters in the device area X- ray tube Set the measurement time with the downward- facing arrow next to Acquire Start the measurement with Acquire M4 TORNADO... -
Page 140: Multi-Point
Often Used Analytical Procedures 7.3 Multi-Point Fig. 70 Multi-Point analysis User Manual... -
Page 141: Table 50 Steps For Multi-Point Analysis
Preview. Dead time should be less than 60 % Set the measurement time with the downward- facing arrow next to Acquire Start the measurement with Acquire M4 TORNADO... -
Page 142: Auto-Point
Often Used Analytical Procedures 7.4 Auto-Point Fig. 71 Auto-Point analysis User Manual... -
Page 143: Table 51 Steps For Auto-Point Analysis
Preview. Dead time should be less than 50 % Set the measurement time with the downward- facing arrow next to Acquire Start the measurement with Acquire M4 TORNADO... -
Page 144: Line Scan
Often Used Analytical Procedures 7.5 Line scan Fig. 72 Line scan analysis User Manual... -
Page 145: Table 52 Steps For Line Distribution Analysis
Preview. Dead time should be less than 50 % Set the measurement time stage mode with the downward-facing arrow next to Acquire Start the measurement with Acquire M4 TORNADO... -
Page 146: Area Analysis
Often Used Analytical Procedures 7.6 Area Analysis Fig. 73 Area analysis - Mapping User Manual... -
Page 147: Table 53 Steps For Area Analysis
Acquire It is recommended to use short measurement times per pixel and measure in several cycles to accumulate distributions with high spatial resolution Start the measurement with Acquire M4 TORNADO... -
Page 148: Quantification
Often Used Analytical Procedures 7.7 Quantification Quantification is possible for every spectrum measured with the M4 TORNADO. Point spectra can be measured directly with Point, Multi-Point Auto-Point or by batches of them. Quantification is possible for spectra calculated from distribution analysis... -
Page 149: Quantification Of Distribution Measurements
(see 7.7.1). Due to the very short measurement time per pixel as well as the large number of pixels, in particular for mappings which would require a long calculation time, the mapping pixels can be binned for quantification. M4 TORNADO... -
Page 150: Table 55 Steps For The Quantification Of Distribution Measurements
Often Used Analytical Procedures Table 55 Steps for the quantification of distribution measurements Step Examples/hints Select the element distribution measurement (Area scan) that should be quantified Select the quantification method via the downward- facing arrow next to the Quantify button Define the special conditions for the quantification with the right-facing arrow below the Quantify... -
Page 151: Shutdown
If the instrument is only used during the day, it is sufficient to switch off the tube overnight. If the M4 TORNADO is turned off completely overnight, it must be waited approx. 30 min for the thermal equilibration of the X-ray tube to be finished. -
Page 152: Maintenance Of The M4 Tornado
Before replacing a fuse, the instrument must be disconnected from the mains supply. For overload protection, the M4 TORNADO is equipped with two safety fuses 2,5 A T/H which are located in the mains socket on the rear panel of the instrument. -
Page 153: Cleaning Of The Turntable
Maintenance of the M4 TORNADO If the fuses blow again upon replacement, the instrument must be disconnected from the mains supply and the service of Bruker Nano GmbH should be informed. 9.2 Cleaning of the Turntable The sample chamber should always be kept clean because contamination can influence the analytical result. -
Page 154: Transportation
Transportation 10 Transportation Danger! Risk of injury by dropping or lifting the spectrometer. The M4 TORNADO weighs ~ 130 kg. Whether it is packed or not, the device should be lifted and carried with the help of lifting tools. Caution! Danger of instrument damage due to impacts, coldness and moisture. -
Page 155: Disposal
The X-ray tube and the detector contain the toxic substance Beryllium. The disposal of these components must be executed by the manufacturer. All components of the M4 TORNADO, excepting the X-ray tube and the detector, are disposed as hazardous waste. The components X-ray tube and detector contain the toxic substance Beryllium and, thus, are taken back by the manufacturer. -
Page 156: A Quantification With M-Quant
Quantification with M-Quant A Quantification with M-Quant Quantitative analysis is performed by calculation of a theoretical spectrum with the Sherman relation. This calculated spectrum is compared with the measured one and then the quantification result is iteratively improved. The flow chart of this calculation is shown in Table 57 together with the description of the steps of calculation. - Page 157 Further uncertainties are calculated by consideration of Counting statistics Fundamental parameters uncertainty Peak overlap and shape uncertainty The quantification result than can be presented with uncertainties. 1) Horst Ebel, X-ray Tube Spectra, X-ray Spectrometry, 28, 255-266 (1999) M4 TORNADO...
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Page 158: Table 58 Calculation Of Correction Factors
Quantification with M-Quant The calculation of the correction factors uses the following procedures. Table 58 Calculation of correction factors Calibration type Description Optic calibration The X-ray optic has an influence on the excitation spectrum. The tube spectrum can be calculated by theory. However, there is no possibility for a calculation of the optic influence. -
Page 159: B Standard Extent Of Delivery For The M4 Tornado
M4 TORNADO, PC, monitor, vacuum pump USB signal connection between M4 TORNADO and PC Ethernet signal connection between M4 TORNADO and PC... -
Page 160: C General Safety Precautions Of The M4 Tornado
If you suspect that the safety system does not work correctly or that radiation protection is impaired for any reason, immediately switch off the system and contact your local Bruker Service Representative. Manipulations and modifications of the safety systems are strictly forbidden! -
Page 161: D Biological Effects Of X-Ray Radiation
Prompt effects: after large doses of radiation delivered over short periods of time. effects such as cancer induction that may appear months or years after a Delayed effects: radiation exposure M4 TORNADO... - Page 162 Biological effects of X-ray radiation Delayed effects of radiation exposure Cancer Studies of people exposed to high doses of radiation have shown that there is a risk of cancer induction associated with high doses. The specific types of cancers associated with radiation exposure include leukemia, multiple myeloma, breast cancer, lung cancer, and skin cancer.
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Page 163: Index
External requirements ......... 34 Program finishing ........51 False colour display ........109 Program installation ........40 Fit quality ............. 25 Program M4 TORNADO ......53 Functional description ......... 19 Program start ..........50 Fuse replacement ........152 Project area ..........61 General safety precautions ....... - Page 164 Index Quantification, single element spectrum ... 148 Start-up ............53 Recommended measurement parameters 137 Statistical error Sigma ......... 25 Reconstructed spectrum ......156 System Assignments ......... 122 Resolution, spectroscopic ......22 Tab Imaging ..........127 Result calculation ........26 Tab Spectrometer ........125 Result display ...........
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